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1

EKC451

PROCESS DESIGN & ANALYSIS

TASK 3

Group members : ELAINE OOI CHIN WEN (117883)

NURUL EZATI MAT SIDEK (117903)

SOON KAH AIK (115884)

SYAFIQAH BINTI MAD ZIN (117909)

SYED ZULFADLI BIN SYED PUTRA

(115886)

Lecturer’s name : PROF MADYA DR. NORASYID AZIZ

Date of

submission

: 15th

December 2015

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Table of Contents List of Figure........................................................................................................................................... 6

List of Tables .......................................................................................................................................... 7

Chapter 1 Problem Statement ................................................................................................................. 9

1.1 Letter of Transmittal ......................................................................................................................... 9

1.2 Methyl Tertiary Butyl Alcohol (TBA) Industry from Malaysia Chemical Industry Point of

View 11

1.2.1 Introduction to MTBE .............................................................................................................. 11

1.2.2 Application of MTBE: ............................................................................................................. 11

1.2.3 Benefits of MTBE in Gasoline................................................................................................. 12

1.2.4 History of the global perspectives on the usage of MTBE in Gasoline ................................... 13

1.2.5 The Advantages of MTBE over Ethanol .................................................................................. 15

1.2.6 Importance of MTBE to Malaysia Chemical Industry: ............................................................ 15

Chapter 2: Process Alternatives ............................................................................................................ 16

2.1 Three Process Alternatives for MTBE Production ......................................................................... 16

2.1.1 MTBE Production from Dehydrogenation of Isobutane .......................................................... 16

2.1.2 MTBE Production by Isobutylene from Refineries ................................................................. 21

2.1.3 MTBE Production by Isobutylene from TBA:......................................................................... 25

2.2 Comparison between Alternatives .................................................................................................. 22

2.3 Choice of Process ............................................................................................................................ 31

2.3.1 Safety and Health Issues: ......................................................................................................... 31

2.3.2 Environmental Issues: .............................................................................................................. 32

2.3.3 Public Issues: ........................................................................................................................... 33

2.3.4 Flexibility and Controllability:................................................................................................. 34

2.3.5 Economic Indicators and Market Background Analysis: ......................................................... 35

2.3.6 Current related problem of the plant to the environment and society: ..................................... 37

Chapter 3: Critical Assessment of the Process Chosen ......................................................................... 39

3.1 Capacity of Plant ............................................................................................................................. 39

3.2 Plant Location [51] [52] .................................................................................................................. 42

3.3 Complete Description of Process Chosen ....................................................................................... 44

3.4 Similar Plant in Malaysia [75] ........................................................................................................ 49

3.5 Environment, Safety and Health Concerns ..................................................................................... 50

3.5.1 Environmental Concerns .......................................................................................................... 50

3.5.2 Safety Concerns ....................................................................................................................... 51

3.5.3 Health Concern ........................................................................................................................ 52

3.6 Projected Demands/Supply for Next 10 years ................................................................................ 53

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Chapter 4 Process Synthesis Structure and Analysis ............................................................................ 56

4.1 Input-Output Structure .................................................................................................................... 56

4.2 Feed and Product Specifications: .................................................................................................... 57

4.3 Price of all Product, By-Product and Raw Materials ...................................................................... 60

4.4 Destination Codes and Component Classification .......................................................................... 61

4.5 Utilities of the Process .................................................................................................................... 62

Chapter 5 Process Flow Diagram.......................................................................................................... 63

5.1 Block flow diagram for MTBE synthesis from isobutylene and methanol: ................................... 63

5.2 Process Flow Diagram .................................................................................................................... 65

5.3 Innovative Approach in Process Design ......................................................................................... 66

Chapter 6 Process Analysis ................................................................................................................... 67

6.1 Justification of Equipment .............................................................................................................. 69

6.2 Separation Operations Used in Production of MTBE ..................................................................... 72

Chapter 7: Mass Balance and Energy Balance of the Process Plant ..................................................... 74

7.1 Mixing Point ................................................................................................................................... 74

7.2 Feed Pump (P-101) ......................................................................................................................... 75

7.3Heat Exchanger (E-101) .................................................................................................................. 75

7.4 MTBE Reactor (R-101) .................................................................................................................. 76

7.5 MTBE Tower (T-101) ..................................................................................................................... 77

7.6 Condenser (E-102) .......................................................................................................................... 78

7.7 Reflux Pump (P-102) ...................................................................................................................... 79

7.8 Heater (E-104) ................................................................................................................................ 80

7.9 Bottom Reboiler (E-103) ................................................................................................................ 81

7.10 Methanol Absorber Column (T-102) ............................................................................................ 82

7.11 Methanol Recovery Tower (T-103) .............................................................................................. 83

7.12 Distillate Condenser (E-105) ........................................................................................................ 84

7.13 Reflux Pump (P-103) .................................................................................................................... 85

7.14 Methanol Recycle Pump ........................................................................................................... 86

7.15 Bottom Reboiler (E-106) .............................................................................................................. 87

7.16 Water Recycle Pump (P-105) ................................................................................................... 88

7.17 Water Mixing Point ................................................................................................................... 90

7.18 Comparison Aspen and Excel Calculation ................................................................................ 91

7.18.1 Mass Balance Justification between Manual Calculation and Aspen Simulation.............. 99

7.18.2 Energy Balance Justification between Manual Calculation and Aspen Simulation ........ 102

Chapter 8 Utilities and Other Issues ................................................................................................... 103

8.1 Utilities .......................................................................................................................................... 103

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8.2 Amount of Waste Generated ......................................................................................................... 105

8.2.1 Liquid Waste .......................................................................................................................... 105

8.2.2 Vapor waste ........................................................................................................................... 105

8.2.3 Mode of liquid waste and vapour waste disposal................................................................... 106

Chapter 9 ............................................................................................................................................. 107

9.1 Mass transfer Equipment Design .................................................................................................. 107

9.1.1 Distillation Column, T-101 .................................................................................................... 107

9.1.2 METHANOL ABSORBER/SCRUBBER (T-102) ................................................................ 110

9.1.3Distillation Column, T-103 ..................................................................................................... 113

9.2 Heat Transfer Equipment .............................................................................................................. 116

9.2.1 Feed Heater, E-101 ................................................................................................................ 116

9.2.2 Condenser, E-102 ....................................................................................................................... 119

9.2.3 Reboiler, E-103 .......................................................................................................................... 122

9.2.4 Heater, E-104 ............................................................................................................................. 125

9.2.5 Condenser, E-105 ....................................................................................................................... 128

9.2.6 Reboiler, E-106 ...................................................................................................................... 131

9.3 Reactor Design .............................................................................................................................. 134

9.3.1 MTBE REACTOR (R-101) DESIGN .................................................................................... 134

9.4 Auxiliary Equipment Design ........................................................................................................ 137

9.4.1 Pump ...................................................................................................................................... 137

9.4.1.1 Feed Pump, P-101 ........................................................................................................... 138

9.4.1.2 Reflux Pump, P-102 ........................................................................................................ 139

9.4.1.3 Reflux Pump, P-103 ........................................................................................................ 140

9.4.1.4 Methanol Recycle Pump, P-104 ...................................................................................... 141

9.4.1.5 Water Recycle Pump, P-105 ........................................................................................... 142

9.5 Comparison between Aspen and Excel Calculation ..................................................................... 143

9.5.1 Mass Transfer Equipment ...................................................................................................... 143

9.5.1.1 Distillation Column, T-101 ............................................................................................. 143

9.5.1.2 Distillation Column, T-103 ............................................................................................. 144

9.5.2 Heat Transfer Equipment ....................................................................................................... 145

9.5.2.1 Feed Heater, E-101 ......................................................................................................... 145

9.5.2.2 Heater, E-104 .................................................................................................................. 146

9.5.3 Reactor Design ....................................................................................................................... 146

9.5.3.1 MTBE Reactor, R-101 .................................................................................................... 146

References ........................................................................................................................................... 147

Appendix A ......................................................................................................................................... 155

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Thermodynamic Data of Reactants and Product ............................................................................. 155

Physical Data .................................................................................................................................. 157

MSDS of All Chemical Components in Process ............................................................................ 159

Appendix B ......................................................................................................................................... 216

Economic Potential ......................................................................................................................... 216

Appendix C ......................................................................................................................................... 221

Mass Transfer Equipment Design ................................................................................................... 221

Heat Transfer Equipment Design .................................................................................................... 283

Reactor Design ................................................................................................................................ 346

Auxiliary Equipment Design .......................................................................................................... 371

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List of Figure Figure 1: MTBE Production Facility .................................................................................................... 17

Figure 2: Schematic Diagram of the Oleflex Isobutane Dehydrogenation Process .............................. 18

Figure 3: A simplified flow diagram of the Ethermax process ............................................................. 20

Figure 4: Typical Layout of MTBE Plant ............................................................................................. 21

Figure 5: Etherification Process in Packed Bed Reactor ...................................................................... 23

Figure 6: Liquid-liquid Extraction Column .......................................................................................... 24

Figure 7: Reaction Pathway for Indiect Conversion of TBA to MTBE (ARCO process)[23] ............. 25

Figure 8: Block Flow Diagram for Indirect Conversion of TBA to MTBE (ARCO process) .............. 26

Figure 9: Reaction Pathway for Direct Conversion of TBA to MTBE (formerly the Texaco Process,

now the Huntsman Process) [27] .......................................................................................................... 26

Figure 10: Mechanism of TBA to MTBE catalysed by sulfonic acid resin .......................................... 27

Figure 11: Block flow diagram for direct conversion of TBA to MTBE (formerly the Texaco process;

now the Huntsman process) .................................................................................................................. 27

Figure 12: History and projections of global MTBE supply and demand from 2010 to 2020 ............. 37

Figure 13: Fuel ether demand in Asia from 1992 to 2011 .................................................................... 40

Figure 14: The amount of new vehicles registered in Malaysia [55] .................................................... 40

Figure 15: Malaysia motor gasoline consumption per year [56] ......................................................... 41

Figure 16: Structure of the global production of MTBE by country, 2013 .......................................... 41

Figure 17: The Location of Plant at Teluk Kalong, Terengganu, Malaysia.......................................... 42

Figure 18: Etherification Process in Packed Bed Reactor .................................................................... 44

Figure 19: Distillation Column Process for MTBE .............................................................................. 46

Figure 20: Vapor-liquid equilibrium and chemical equilibrium of the ternary system MTBE, methanol

and isobutene [105] ............................................................................................................................... 47

Figure 21: Liquid- liquid Extraction Column ....................................................................................... 47

Figure 22: Recovery of Methanol using Distillation Column ............................................................... 48

Figure 23: History and projections of global MTBE supply and demand from 2010 to 2020 ............. 54

Figure 24: Projections of global MTBE supply and demand from 2015 to 2024 ................................ 55

Figure 25: Block Diagram for the Production of MTBE ...................................................................... 63

Figure 26: Block Diagram for the Production of MTBE with Temperature and Pressure ................... 64

Figure 27: Process Flow Diagram (After modification) ....................................................................... 65

Figure 28: Block Diagram of Initial/ Existing MTBE Production Plant .............................................. 66

Figure 29: Aspen Flowsheet .................................................................................................................. 91

Figure 30: Aspen Result for Distillation Column, T-101 ................................................................... 143

Figure 31: Aspen Result for Distillation Column, T-103 ................................................................... 144

Figure 32: Aspen Result for Feed Heater, E-101 ................................................................................ 145

Figure 33: Aspen Result for Heater, E-104 ......................................................................................... 146

Figure 34: Input-output structure for MTBE production from isobutylene and methanol ................. 217

Figure 35: Recycle structure for MTBE production from isobutylene and methanol......................... 218

Figure 36: Graph of economics potential vs recycle ratio .................................................................. 219

Figure 37: Reactor structure for MTBE production from isobutylene and methanol ......................... 219

Figure 38: Graph of economics potential vs isobutylene conversion ................................................. 220

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List of Tables Table 1: Comparison between Alternatives .......................................................................................... 22

Table 2: Advantages and Disadvantages of Direct Synthesis of MTBE from Isobutylene and Methanol

.............................................................................................................................................................. 49

Table 3: Similar Plant in Malaysia ........................................................................................................ 49

Table 4: Block Diagram about above Description Text ........................................................................ 57

Table 5: Feed and Product Specification of Methanol .......................................................................... 57

Table 6: Feed and Product Specification of Isobutylene ...................................................................... 58

Table 7: Feed and Product Specification of MTBE .............................................................................. 59

Table 8: Price of Raw Materials and Product ....................................................................................... 60

Table 9: Price of By-product ................................................................................................................. 60

Table 10: Destination Codes and Component Classification ................................................................ 61

Table 11: Justification of Equipment .................................................................................................... 69

Table 12: Separation Operation Used in Methyl Tert-Butyl Ether (MTBE) MTBE Production .......... 73

Table 13: Stream Table from Aspen ...................................................................................................... 92

Table 14: Mass Balance Comparison .................................................................................................... 93

Table 15: Energy Balance Comparison ................................................................................................ 96

Table 16: Utilities for Heater, Cooling Jacket, Condenser and Reboiler ............................................ 103

Table 17: Total Electrical Energy Consumption per Year .................................................................. 104

Table 18: Total Power Requirement ................................................................................................... 104

Table 19: Specification sheet for distillation column T-101 ............................................................... 108

Table 20: Specification sheet for methanol absorber, T-102 .............................................................. 111

Table 21: Specification sheet for distillation column T-103 ............................................................... 114

Table 22: Specification Sheet for Feed Heater, E-101 ........................................................................ 117

Table 23: Specification Sheet for Condenser, E-102 .......................................................................... 120

Table 24: Specification Sheet for Reboiler, E-103 ............................................................................. 123

Table 25: Specification Sheet for Heater, E-104 ................................................................................ 126

Table 26: Specification Sheet for Condenser, E-105 .......................................................................... 129

Table 27: Specification Sheet for Reboiler, E-106 ............................................................................. 132

Table 28: Specification sheet for MTBE reactor, R-101 .................................................................... 135

Table 29: Specification Sheet of Feed Pump, P-101........................................................................... 138

Table 30: Specification Sheet of Reflux Pump, P-102 ....................................................................... 139

Table 31: Specification Sheet of Reflux Pump, P-103 ....................................................................... 140

Table 32: Specification Sheet of Methanol Recycle Pump, P-104 ..................................................... 141

Table 33: Specification Sheet of Water Recycle Pump, P-105 ........................................................... 142

Table 34: Comparison between Aspen and Excel Calculation Value for T-101 ................................ 143

Table 35: Comparison between Aspen and Excel Calculation Value for T-103 ................................ 144

Table 36: Comparison between Aspen and Excel Calculation Value for E-101 .................................. 145

Table 37: Comparison between Aspen and Excel Calculation Value for E-104 .................................. 146

Table 38:: Thermodynamic Data of Isobutene, Methanol and MTBE ............................................... 155

Table 39: Thermodynamic Data of Di-isobutylene, Dimethyl ether, TBA and Water ....................... 156

Table 40: Physical Data of Isobutene, Methanol and MTBE ............................................................. 157

Table 41: Physical Data of Di-isobutylene, Dimethyl ether, TBA and Water .................................... 158

Table 42: MSDS of Methyl Tert-Butyl Ether ..................................................................................... 159

Table 43: MSDS of Methanol ............................................................................................................. 165

Table 44: MSDS of Isobutylene ......................................................................................................... 175

Table 45: MSDS of Diisobutylene ...................................................................................................... 186

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Table 46: MSDS of Dimethyl Ether ................................................................................................... 193

Table 47: MSDS of Tert-Butyl Alcohol ............................................................................................. 202

Table 48: MSDS of Water .................................................................................................................. 210

Table 49: Economics potential of MTBE production with varying methanol recycle ratio ............... 218

Table 50: Economics potential of methanol production with varying isobutylene conversion .......... 220

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Chapter 1 Problem Statement

1.1 Letter of Transmittal Process Design Team,

Process Design and Analysis Department,

MTBE Corporation SDN BHD,

Tanjung Langsat Industrial Park,

81707 Johor.

Date: 14 September 2015

Prof.Madya Dr. Norashid Aziz,

Plant Manager,

MTBE Corporation SDN BHD,

Teluk Kalong Industrial Estate,

24000 Terengganu.

Dear Sir,

Plant Design for the Production of Methyl-Tert-Butyl-Ether (MTBE)

Refer to the above title; the detail primary stage plant design for the production of MTBE is

enclosed. The expected production capacity for this design will be around 300,000 tonnes per

year of MTBE. This would be the second MTBE manufacturing company in Malaysia after

MTBE Sdn. Bhd in Kuantan. World demand of MTBE in Asia has been growing at much

more rapid than elsewhere in the world. It is because MTBE is relatively cheap and abundant

supply.

2. The location of our MTBE plant production will be placed at Teluk Kalong Industrial

Estate, Terengganu. The reason we want to locate our plant at Teluk Kalong is because this

industrial estate is only 9.6 km away from Kemaman, where Tipco Asphalt Public Company

Limited (one of the largest oil refineries in Malaysia) is located. The transportation facilities

at Teluk Kalong can be divided into two main types which are airport (Kuantan Airport,

Kerteh Airport, and Kuala Terengganu Airport) and port (Kemaman Port, Kerteh Port and

Kuantan Port) facilities. Due to the availability of these facilities, raw material such as

isobutene, methanol can be easily imported from overseas and the finished product can be

distributed to the other states in Malaysia.

3. We choose to produce MTBE directly from isobutylene (by-product from fluid catalytic

cracking operations in refineries) and methanol. This is because the reaction only involved

packed bed reactor, distillation column and raffinate stripper which are quite simple process

compared to other alternative process. Besides, the etherification reaction is an exothermic

process. Thus, low temperature is favorable to the formation of MTBE. In addition, low

pressure is needed in this reaction to ensure the reaction occurs in liquid state.

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4. The main concern is that although there is another MTBE supplier in Malaysia, and

the amount of MTBE produced by that company is sufficient to cope with the demand in

Malaysia, our design team wish to be the second team to propose a production design on

MTBE. Consequently, if there is a second MTBE manufacturing plant in our country, the

price of MTBE would not be solely controlled by the first company in Malaysia. Moreover,

the consumption is still very high in the world especially Asia. Thus, we are targeting an

export-based MMA production plant too in order to increase our revenue annually.

5. Our detailed plant design included process flow diagram, process and equipment

optimization, reactor sizing, market analysis, operating condition, mass and energy balance,

cost, safety and health issue. We also design our plant with considering the impact to the

environment.

6. If there is any doubt, for further inquiry and information about this project, do not

hesitate to contact us. We hope that this design of producing MTBE can meet your

expectation. Thank you for your cooperation and we hope we will hear good news from you

soon.

Thank You.

Yours Faithfully,

_______________________ ______________________ _____________________

(Syed Zulfadli Syed Putra) (SOON KAH AIK) (ELAINE OOI CHIN WEN)

013-9766379 012-5548418 012-3740879

[email protected] [email protected] [email protected]

Project manager Member of plant design Member of plant design

_____________________________ _____________________________

(NURUL EZATI BT MAT SIDEK) (SYAFIQAH BINTI MAD ZIN)

019-9660312 011-24373876

[email protected] [email protected]

Member of plant design Member of plant design

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1.2 Methyl Tertiary Butyl Alcohol (TBA) Industry from Malaysia

Chemical Industry Point of View

1.2.1 Introduction to MTBE MTBE (methyl tertiary-butyl ether) is an organic compound with the formula

C5H12O.In MTBE, one carbon atom is that of a methyl group, -CH3 and the other is the

central atom of a tertiary butyl group, -C(CH3). It is a chemical compound that is produced by

the chemical reaction of methanol and isobutene. MTBE is a flammable, colorless liquid at

normal temperature and pressure with freezing point of -109oC (-164

oF) and boiling point of

55oC (131

oF).MTBE is used only with good ventilation and avoid all ignition sources as it is

extremely flammable with a high vapor pressure. Its flashpoint is -10oC (14

oF) and self-

ignition temperature of 374oC (705

oF) [1]. In addition, MTBE exhibits advantages such as

low water solubility and good materials compatibility [2]. Besides, it is very soluble in some

organic solvents such as alcohol and ether [3].

1.2.2 Application of MTBE: Methyl tertiary butyl ether (MTBE) is one of the most popular oxygenated

compounds for gasoline. Oxygenated compounds are used in gasoline blending to improve

fuel specifications such as octane quality. Owing to its high oxygen content raising property,

it can helps in complete combustion of fuel and reducing knocking within the engine which

in turn improves the life span of the machine. Besides, the use of MTBE in fuel also helps in

reduce pollutant emissions. Adding oxygenates to gasoline can improve combustion and

decrease carbon monoxide (CO) and hydrocarbon (HC) emissions to the environment. Thus,

MTBE had been used in U.S. gasoline since 1979 to replace tetraethyl lead as the use of

tetraethyl lead will cause the pollution of air. [2]

Besides, MTBE is also used as a chemical intermediate to produce high purity

isobutylene. By reversing MTBE formation reaction, pure isobutylene is obtained.

Isobutylene is used to manufacture butyl rubber, polyisobutylene and methyl methacrylate

(MMA), which are used in numerous end-use industries such as automotive, industrial

manufacturing and electronics. [4]

In addition, MTBE is a good solvent and extract ant. High purity MTBE is being used

as a process reaction solvent in the pharmaceuticals industry. Besides, MTBE is a non-

chlorinated process solvent. It is also used as a solvent for chromatographic techniques.

Furthermore, it is used as a solvent in Grignard synthesis and other organometallic reactions.

It is also used as an anionic and cationic polymerization solvent. [5]

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1.2.3 Benefits of MTBE in Gasoline Technical Benefits:

MTBE is the most widely used fuel oxygenate, due to its combination of technical

advantages and supply availability. MTBE delivers high octane value at relatively low cost.

In addition, MTBE offers low water solubility (compared to e.g. alcohols), low reactivity and

relatively low volatility. These characteristics allow refiners to overcome handling problems

in the fuel distribution system posed by alcohol oxygenates.

Another important reason for the widespread use of MTBE is feedstock flexibility.

MTBE can either be made inside the refinery, using petroleum-derived raw materials, or it

can be produced externally, using natural gas feedstocks, thereby ensuring ready availability

and reducing dependence on crude oil for the production of automotive fuels.

Furthermore some quite recent studies have shown that the octane appetite of modern

cars seem to differ from that of previous populations. It appears that the conventional

measures of anti-knock quality (RON and MON) are no longer appropriate for modern

engines. The modern Japanese and European cars equipped with knock sensors prefer fuels of

high sensitivity and high RON. Adding MTBE in the gasoline is a way to improve these

properties in the fuel.

Air quality benefits:

MTBE provides considerable air quality benefits, which can be divided into two main

categories. There are the direct effects, largely due to more complete fuel combustion, and

the indirect effects, arising from the dilution of other, less desirable, gasoline pool

components.

Direct effects include the reduction of specific pollutants limited by law, such as

carbon monoxide (CO) and unburned hydrocarbons (HCs), as well as other serious pollutants

such as particulate matter (PM) and ground-level ozone (O3).

Indirect effects include the reduction of sulphur, olefins, aromatics and benzene levels,

regardless of whether the fuel is used in current or older technology vehicles.

The extent of MTBE’s air quality benefits depends on various parameters, such as the

percentage of blended MTBE, the presence of catalyst devices, the type and age of engine

and the driving cycle. Nevertheless, there is general agreement in the industrial and scientific

communities on broad values.

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Carbon monoxide: CO emission is reduced on average by at least the same percentage

as MTBE content in gasoline.

Unburned hydrocarbons: For each 1 or 2% of MTBE, there is a 1% reduction in total

HC emissions.

Particulate matter: It is estimated that each 1% of MTBE results in a 2 to 3% PM

emission reduction.

Ozone: MTBE generates about half the ozone compared with iso/alkylates and one-

tenth that of aromatics.

Benzene: It is estimated that, for each 1% of MTBE, there is an equivalent percentage

reduction in benzene emissions, both evaporative and exhaust.

Olefins: MTBE displays low vapour pressure and low volatility compared to olefins.

Converting olefins to MTBE in the refinery removes some of the most reactive and

volatile components from the gasoline pool.

Lead: MTBE is an effective substitute for lead, a toxic compound that has been

phased out in most parts of the world.[9]

1.2.4 History of the global perspectives on the usage of MTBE in

Gasoline As mentioned previously, addition of MTBE into gasoline which acts as octane

booster will reduce ozone-forming smog, hazardous carbon monoxide pollution, and other

toxic air pollutants. The passage of the U.S. 1990 Clean Air Act (CAA) resulted in increased

use of MTBE in order to reduce carbon monoxide and hydrocarbon emissions (till now).

MTBE also reduces air toxics emissions and pollutants that form ground-level ozone. MTBE

has been the additive most commonly used by gasoline suppliers throughout most of the

country. It has been used because it is very cost-effective in meeting air quality and gasoline

performance goals.

Unfortunately, MTBE is more soluble in water, has a smaller molecular size, and is

less biodegradable than other components of gasoline. Consequently, MTBE is more mobile

in groundwater than other gasoline constituents, and may often be detected when other

components are not. In the United States, a debate is raging over the environmental

consequences of the increased use of methyl tertiary-butyl ether (MTBE).The controversy

started with a report submitted in November 1998 by the University of California (UC Davis),

on Health and Environmental Assessment of MTBE to the State of California. This study was

authorized by the California Senate to assess a variety of issues and public concerns

14

associated with the use of MTBE in gasoline. In early 2000’s, the U.S. Environmental

Protection Agency (EPA) has taken actions to significantly reduce or eliminate MTBE. At the

same time, Governor Gray Davis’s decree that MTBE be phased out from California gasoline

by 2003 was based largely on two projections that have proven to be erroneous: that MTBE is

a pervasive groundwater contaminant throughout the state, and that MTBE poses a health

threat to Californians. Ethanol is then became the primary alternative of oxygenate to replace

the MTBE.

However, The European MTBE market appears to be relaxed in the face of EPA’s

proposed ban on the MTBE. This is because the result of the EU risk assessment carried out

in Finland was presented in January 2001. It concluded that MTBE was not a toxic threat to

health, but can leave a bad taste in drinking water. As a result, in the draft directive for new

fuel quality laws called Auto Oil II, published May 11, 2001, the EU set no limitations on the

use of MTBE in fuel after2005. Using a similar approach as the official EU Risk Assessment

process, the European Centre for Eco-toxicology and Toxicology of Chemicals(ECETOC)

recently concluded, ‘‘the risk characterization for MTBE does not indicate concern for

human health with regard to current occupations and consumer exposures.’’ Also, the

German Federal Environmental Agency (UBA) has concluded their study into MTBE, which

was initiated after the situation in California. They have advised the Ministry for the

Environment that MTBE does not constitute a threat for the German environment at this time,

as the general condition of the underground storage tanks is considered to be very good and

the potential health risks from MTBE are negligible.

Similarly, due to the relative ease in blending of MTBE into gasoline, easy

transportation and storage, as well as relatively cheap and abundant supply, MTBE is the

most widely used oxygenate in Asia. With respect to California’s MTBE situation

(contamination of water due to leakage of MTBE), Asian trading sources have said there is

little possibility of MTBE being phased out in Asia. It has been observed that economics

rather than politics were the determining factor for MTBE survival in Asia. There are a lot of

issues that Asian governments need to address if they want to get rid of MTBE, such as the

cost effectiveness to build new infrastructure such as new processing plants and additional

road network, ensuring adequate supply of MTBE alternatives, and how much would

gasoline cost in the end. [6]

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1.2.5 The Advantages of MTBE over Ethanol In USA, MTBE is banned from use in gasoline due to studies that revealed it causes

groundwater contamination and cancer, primarily due to leakage from underground storage

tank. When ethanol issued to replace MTBE as the octane enhancer, unlike MTBE, ethanol

has a greater ability to attract and absorb large amounts of water and moisture into the fuel.

(MTBE is also soluble in water, but less so than ethanol). This property of ethanol has then

dramatically changed the shelf life of fuel. Fuel that did not contain ethanol had a shelf life of

several years. Unlike ethanol-blend fuels which remain stable for a maximum of only 90-100

days. In terms of performance, the heating value (energy) of MTBE is always higher than

ethanol. Also, the auto ignition temperature of MTBE is higher than ethanol, thus MTBE will

give higher octane rating compared to ethanol. [7]

Next, ethanol blends evaporate more readily than MTBE blends. Therefore, using

ethanol increases refiner production costs and reduces operating flexibility. In addition,

ethanol contributes about one half the blending volume provided by MTBE, and the

maximum amount of ethanol that can be blended into gasoline is capped at 10% (versus 15%

for MTBE). As a result, ethanol is unable to dilute many, less desirable, gasoline components.

Besides, the cost of ethanol is more expansive than the MTBE, so ethanol’s use is

uneconomic without a large government subsidy. From the environmental standpoint, ethanol

emits more harmful smog-forming emissions in the summertime than MTBE due to its high

tendency to evaporate. Because ethanol is used in lower volumes, it provides less reduction in

toxic air emissions than MTBE. Ethanol also can contribute to increased NOx emissions. [8]

1.2.6 Importance of MTBE to Malaysia Chemical Industry: Malaysia is the second largest oil and gas producer in the Association of Southeast

Asian Nations (ASEAN) and one of the world’s top LNG producers.[10] There are over 3500

oil and gas (O&G) business in Malaysia comprising international oil companies,

independents, services and manufacturing companies that support the needs of the O&G

value chain both domestically and regionally. Many major global machinery and equipment

(M&E) manufacturers have set up bases in Malaysia to complement home-grown M&E

companies, while other Malaysian oil and gas companies are focused on key strategic

segments such as marine, drilling, engineering, fabrication, offshore installation and

operations and maintenance (O&M).

In recent years, Malaysia has also created a vibrant market for merger-and-acquisition

activities to acquire key resources such as technology, capabilities, physical space as well as

16

key personnel. As a result, Malaysian services companies today offer competitive rates and

skilled manpower to support the growth of the upstream and downstream sectors while

remaining competitive compared to other countries in the region. [11]

There are a few local and international operators involved in the upstream exploration

and production activities in Malaysia. PETRONAS Carigali Sdn. Bhd remains the main local

operator in Malaysia. The international oil and gas companies such as Exxon, Shell, Hess and

Talisman also play a significant role in the exploration and production of oil and gas in

Malaysia together with PETRONAS Carigali Sdn. Bhd.

The Government of Malaysia has contributed significantly towards policy and macro-

economic planning to secure a sustainable and long-term success of the oil and gas industry.

The Government’s main objective is to increase aggregate production capacity by five

percent (5%) every year up to the year 2020 to meet domestic demand growth while

sustaining crude oil and LNG exports to overseas markets. In the Asia Pacific region,

Malaysia aims to be the number one oil and gas hub by 2017, taking advantages of its

strategic location at key shipping lanes as well as strong economic fundamentals in China,

India and within Southeast Asia. [12]

Chapter 2: Process Alternatives

2.1 Three Process Alternatives for MTBE Production Methyl tert-butyl ether (MTBE) is produced through the reaction of isobutylene with

methanol. There are different sources of the isobutylene feedstock, often depending on the

type of MTBE producer. Unlike methanol, isobutylene is generally not available

commercially and thus must be either obtained from process streams available in-house or

manufactured separately, generally starting from butane. There are three primary MTBE

processes and the brief descriptions of the different sources of isobutylene and of each

process are shown below.

2.1.1 MTBE Production from Dehydrogenation of Isobutane A typical etherification complex configuration is shown in figure 1 for the production of

methyl tertiary butyl ether (MTBE) from butanes and methanol. Three primary catalytic

processes are used in an MTBE complex:

1. Paraffin isomerization to convert normal butane into isobutane

2. Dehydrogenation to convert isobutane into isobutylene

17

3. Etherification to react isobutylene with methanol to make MTBE

Figure 1: MTBE Production Facility

Isomerization of n-butane:

Field butanes, a mixture of normal butane and isobutane obtained from natural gas

condensate, are fed to a deisobutanizer (DIB) column. The DIB column prepares an isobutane

overhead product, rejects any pentane or heavier material in the DIB bottoms, and makes a

normal butane side cut for feed to the paraffin isomerization unit. The DIB overhead is

directed to the Oleflex unit. The once-through conversion of isobutane is approximately 50%.

About 91% of the isobutane conversion reactions are selective to isobutylene and hydrogen.

On a mass basis, the isobutylene selectivity is 88 wt%. [13]

The remaining normal butane is combined with dry makeup hydrogen will channel to

the paraffin isomerisation unit at the temperature between 230 – 340oF (110 to 170

oC) and

200 to 300 psig (1480 to 2170 kPa). The function of hydrogen is to suppress polymerization

of the olefin that is formed as intermediates. A small amount of promoter which is organic

chloride is added to maintain the stability of the catalyst activity and it will convert

completely as hydrochloric acid in the reactors.

The efficiency of stream will be increased when there are two reactors used instead

only one reactor. The reactor product which is isomerate will flow to a stabilizer while

18

hydrochloric acid will flow to the scrubber and the scrubber will remove the hydrochloric

acid from the light gases. The stabilized liquid product contains almost same amount of

composition mixture of n-butane and isboutane. The unconverted n-butane will be recycled

back to isomerization unit to convert it to isobutane in order to achieve nearly total

conversion of n-butane to isobutane. [14]

Dehydrogenation of Isobutane: [15]

Isobutane undergoes dehydrogenation to produce isobutylene. Dehydrogenation step

is carry out in the presence of catalyst which is platinum supported on alumina. The Oleflex

dehydrogenation process consists of three moving bed radial flow reactors in series that feed

stream is preheated in a furnace and send to the first reactor. Since the temperature of outlet

product drops due to endothermic reactions, the inter-stage furnaces are placed between

reactors to increase temperature. The outlet product from the first reactor is heated in the

second stage inter-stage furnace and fed to the second reactor. Due to coke formation on the

catalyst surface, the outlet catalyst from the third reactor is sent to the regeneration section. In

the regeneration reactor, the formed coke is burnt and regenerated catalyst is recycled to the

first reactor and turns along the process. Figure 2 shows the schematic diagram of the Oleflex

process.

Figure 2: Schematic Diagram of the Oleflex Isobutane Dehydrogenation Process

High temperature and low pressure will shift to isobutene dehydrogenation, but also

promote side reaction and catalyst deactivation. Thus, inter-stage furnaces function to

19

maintain the desired temperature required for dehydrogenation reaction. The equation below

shows the dehydrogenation of isobutane.

iC4H10 ↔ iC4H8 + H2

Isobutane ↔ Isobutene + Hydrogen

Besides, there are 3 possible side reactions that might occur during dehydrogenation of

isobutane.

1. Isobutane Cracking:

iC4H10+H2↔ C3H8 + CH4

Isobutane + Hydrogen ↔ Propane + Methane

2. Propane Dehydrogenation:

C3H8 ↔ H2 + C3H6

Propane ↔ Hydrogen + Propene

3. Coke Formation

iC4H8↔ 4C + 4H2

Isobutene ↔ Carbon + Hydrogen

Etherification Process:

The Ethermax process can be used to produce methyl tert- butyl ether (MTBE). This

process combines the Hüls fixed-bed etherification process with advanced RWD catalytic

distillation technology from Koch-Glitsch, Inc. The combined technology overcomes reaction

equilibrium limitations inherent in a conventional fixed-bed etherification process. The

Ethermax process reacts isobutylene over an acid resin in the presence of methanol to form

MTBE. The reaction chemistry and unit operating conditions are essentially the same as those

of a conventional ether process, such as the Hüls MTBE process, except that KataMax

packing has been added to increase the overall conversion. KataMax packing represents a

unique and proprietary approach to exposing a solid catalyst to a liquid stream inside a

distillation column. The reactive distillation zone of the RWD column uses KataMax packing

to overcome reaction equilibrium constraints by continuously fractionating the ether product

from unreacted feed components. As the ether product is distilled away, the reacting mixture

is no longer at equilibrium. Thus, fractionation in the presence of the catalyst promotes

20

additional conversion of the reactants. Isobutylene conversion of 99 for MTBE can be

achieved in this process. [16]

Figure 3 is a simplified flow diagram of the Ethermax process. Isobutylene and small

excess stoichiometric amount of methanol join a controlled quantity of recycle from the

reactor effluent and are cooled prior to entering the top of the primary reactor. The combined

feeds and recycle are all liquids. The resin catalyst in the primary reactor is a fixed bed of

small beads. The reactants flow down through the catalyst bed and exit the bottom of the

reactor. Effluent from the primary reactor contains MTBE, methanol and unreacted C4 olefins

and usually some C4paraffins, which were in the feed.

A significant amount of the effluent is cooled and recycled to control the reactor

temperature. The net effluent feeds a fractionator with a section containing catalyst. This is

Koch’s proprietary reaction with distillation (RWD) column. The catalyst section, located

above the feed entry, is simply structured packing with conventional MTBE resin catalyst

between the corrugated mesh plates. MTBE is withdrawn as the bottom product, and

unreacted methanol vapor and isobutylene vapor flow up into the catalyst reaction to be

converted to MTBE.

The advantages of an RWD column include essentially complete isoolefin

conversions. The excess methanol and unreacted hydrocarbons are withdrawn from the RWD

column reflux accumulator and fed to a methanol recovery tower. In this tower, the excess

methanol is extracted by contact with water. The resultant methanol-water mixture is distilled

to recover the methanol, which is then recycled to the primary reaction. [17]

Figure 3: A simplified flow diagram of the Ethermax process

21

2.1.2 MTBE Production by Isobutylene from Refineries Isobutylene is produced as a byproduct of fluid catalytic cracking (FCC) operations in

refineries. There are trace amounts of other inert isomers found in the refineries such as n-

butane, isobutane and etc. Isobutylene from FCC can directly use to react with methanol

because the other inert isomers will not react with methanol.

The etherification of isobutylene from refinery and methanol is carried out according

to the following equilibrium reaction:

(CH3)2C=CH2 + CH3OH ↔ (CH3)3C-O-CH3 ∆Ho

298 ≈ -37kJ/mol

This exothermic reaction takes place in the liquid phase between 50 and 90oC at 0.7 to

1.5x 106 Pa. [19] MTBE is produced via direct addition of methanol to isobutylene using ion

exchange resin as catalysts. Reaction takes place in the liquid phase at mild process condition

in the presence of acidic solid catalyst. Typical catalyst is sulphonic-ionic rubber.

Temperature of the reaction is kept low, and it can be adjusted to wide range of values. High

temperatures are not recommended due to possibility of catalyst deactivation, which becomes

unstable at temperature of 130oC. Operation of the unit at lower temperature enables safe

operation and long lasting catalyst. [20]Another typical catalyst used is Amberlyst-15.

Amberlyst-15 shows selectivity toward MTBE ranging from 92 to 98%. MTBE selectivity is

directly related to the ratio of methanol and isobutylene. Its selectivity increases when

methanol is in slight excess. However, the resin is not heat resistant and must be used at

temperatures lower than 120oC. [18]

Figure 4: Typical Layout of MTBE Plant

22

Figure 3 above shows a typical layout of a MTBE plant. Firstly, fresh and recycled

methanol is mixed with the C4 stream. The combined stream is first fed to a packed bed

reactor which is usually operated close to isothermal conditions. Uniform temperature avoids

hot spots leading to fast catalyst decay. Thus, temperature control is a significant concern in

this first reactor. The reaction stream from the isothermal reactor is directed to a second

reactor, packed bed type, to complete the MTBE synthesis. The reaction takes place in this

second stage adiabatically. The following step in the process is the separation of MTBE from

the remaining C4, methanol and byproducts. Following this operation, unconverted methanol

is separated from the C4 stream and recirculated to the first reactor. The purity of MTBE

reaches 99.1%.

However, there are 3 main side reactions occur during the synthesis of MTBE. The main

by-products from the side reactions are di-isobutylene, dimethyl ether (DME) and tertiary

butyl alcohol (TBA). The equation for side reactions are shown below: [6]

1. (CH3)2C(CH2) + (CH3)2C(CH2) ↔ (CH3)3C(CH)C(CH3)2

Isobutylene + Isobutylene ↔ Di-isobutylene

2. (CH3)OH + (CH3)OH ↔ (CH3)O(CH3) + H2O

Methanol + Methanol ↔ Dimethyl ether + Water

3. (CH3)2C(CH2)+ H2O ↔ (CH3)3C(OH)

Isobutylene + Water ↔ Tertiary butyl alcohol

The production of di-isobutylene and TBA is limited by controlling the temperature

level for the first and the water content of the reaction medium for the second. Catalyst life is

usually one year. [19]Besides, the presence of excess amounts of methanol in the

etherification reactors can help to control the side reaction. If the methanol/isobutylene ratio

drops to less than stoichiometric level, di-isobutylene formation increases rapidly and

simultaneously isobutylene trimers and tetramers are also formed. [6]

The isobutene conversion (XIB), yield IB (at equilibrium) to MTBE (YMTBE) and

selectivity to MTBE (SMTBE) using Amberlyst 15 catalyst with ratio of methanol/isobutylene

of 1.1 is 92, 94.7 and 96.5% respectively [103].

23

MTBE is recovered as the bottoms product of a distillation unit. The methanol-rich

C4 distillate is sent to the methanol-recovery section. Water is used to extract excess

methanol and recycle it back to process. The isobutylene-depleted C4 stream may be sent to a

raffinate stripper or to a moiseive-based unit to remove other oxygenates such as DME,

MTBE, methanol and tert-butanol. [21]

Etherification process:

Figure 5: Etherification Process in Packed Bed Reactor

The etherification process of methanol and isobutylene is an exothermic reaction. This

exothermic reaction takes place in the liquid phase at 90oC and 1000kPa. High temperatures

are not recommended due to possibility of catalyst deactivation, which becomes unstable at

temperature of 130oC. Operation of the unit at lower temperature enables safe operation and

long lasting catalyst.[20] The reaction occur inside the packed bed reactor is shown below:

(CH3)2C=CH2 + CH3OH ↔ (CH3)3C-O-CH3 ∆Ho298 ≈ -37kJ/mol

The isobutene conversion (XIB), yield IB (at equilibrium) to MTBE (YMTBE) and

selectivity to MTBE (SMTBE) using Amberlyst 15 catalyst with ratio of methanol/isobutylene

of 1.1 is 92, 94.7 and 96.5% respectively [103].

However, there are 3 main side reactions occur during the synthesis of MTBE. The main

by-products from the side reactions are di-isobutylene, dimethyl ether (DME) and tertiary

butyl alcohol (TBA). The equation for side reactions are shown below: [6]

1. (CH3)2C(CH2) + (CH3)2C(CH2) ↔ (CH3)3C(CH)C(CH3)2

Isobutylene + Isobutylene ↔ Di-isobutylene

2. (CH3)OH + (CH3)OH ↔ (CH3)O(CH3) + H2O

Methanol + Methanol ↔ Dimethyl ether + Water

24

3. (CH3)2C(CH2)+ H2O ↔ (CH3)3C(OH)

Isobutylene + Water ↔ Tertiary butyl alcohol

However, there are no reported works on the selectivity of the side reaction during the

synthesis of MTBE from isobutylene and methanol. Several strategies have been used to

reduce the production of these undesirable by-products. First, the ratio of methanol and

isobutylene is kept above one to suppress the dimerization of butane. Reaction temperatures

below 100oC can diminish the formation of dimethyl ether. Finally, the pretreatment of the

feed stream which is removal of water can prevents the formation of TBA [104].

Liquid-liquid extraction process:

Figure 6: Liquid-liquid Extraction Column

The mixture of by-products, mixed C4 and methanol is further separate using liquid-

liquid extraction process. In order to recycle back the unreacted methanol, we have to

separate it from C4 stream and by-products using a liquid-liquid extraction column. Water is

used during the removal of methanol from a C4 stream. This is because methanol is highly

soluble in water but evolves back out of the water if recycled. [60] The pressure used in

liquid-liquid extraction column must be greater than the bubble point pressure of two liquid

phases at all trays. Most extractors operate around ambient temperature and the pressure of

column is 200kPa which will ensure that all the components are in the liquid phase around

the ambient temperature (20-60oC).

25

2.1.3 MTBE Production by Isobutylene from TBA: In this process, TBA is used to produce MTBE. TBA is produced in large quantities

from processes for producing propylene oxide from propylene. Propylene oxide is an organic

compound that is produced on a large scale industrially with its major application being its

use for the production of polyether for use in making polyurethane plastics and propylene

glycol. Tertiary butyl alcohol (TBA), a co-product of propylene oxide (PO), is produced by

PO manufacturers. Although it can be used directly as an oxygenate, it can also be used as a

raw material in the production of MTBE. Some of the PO manufacturers will also produce

MTBE starting from the co-product, TBA. They start with isobutane as a feedstock to

produce TBA and then, ultimately, MTBE, as part of the “PO/MTBE” manufacturing process

[22].

In order to produce MTBE for TBA, TBA must first be dehydrated to isobutylene in

the first reactor according to the first equation below, followed by reaction of IB with

methanol to produce MTBE in the second reactor according to the next equation.

Figure 7: Reaction Pathway for Indiect Conversion of TBA to MTBE (ARCO process)[23]

The dehydration of tertiary butyl alcohol, TBA, to form isobutylene is well known.

The reaction is a relatively simple one to promote; high temperature alone will convert

tertiary butyl alcohol to isobutylene, though it is usually preferred to use a catalyst. With the

presence of solid acid catalysis, the dehydration temperature in the range of 72oC to 90

oC is

preferred. The isobutylene produced is then extracted/separated from the water and is send

the second reactor together with excess methanol to yield MTBE. According to John F.

Knifton and friends, the first reaction (dehydration) and the removal of water can be

completed in a reactive distillation unit [24].

26

By using this unit, high dehydration rates of the TBA can be maintained over a long

period of time as the presence of water in the reactor which cause detrimental effect on the

reaction rate is removed continuously from the reactor [25].In this unit, the isobutylene

formed (more volatile compared to water) flows upward through the upper distillation section

a reflux splitter and then to a reflux condenser, where it is cooled by room temperature water.

Meanwhile the higher boiling aqueous distillation reaction product (mainly water) flows

downwards through the lower distillation section. The isobutylene is then fed into a second

reactor together with methanol where etherification occurs. The block flow diagram of the

two reactions is shown in figure below.

Figure 8: Block Flow Diagram for Indirect Conversion of TBA to MTBE (ARCO process)

However, the route that is proposed here is the direct method. In the direct method

(formerly the Texaco process; now the Huntsman process), MTBE can be produced by

reacting TBA directly with methanol in one reactor in the presence of an acid catalyst

(hydrogen ion-exchange acid resins, such as Amberley’s 15[26] in which water is also

formed as a by-product:

Figure 9: Reaction Pathway for Direct Conversion of TBA to MTBE (formerly the Texaco Process,

now the Huntsman Process) [27]

The reaction above is catalysed by sulfonic acid resin catalyst. Sulfonic acid is the

active component of the catalyst. The catalyst donates a hydrogen ion to the tert-butyl alcohol.

Once the alcohol is protonated, it forms a good leaving group (water) which will leave the

alcohol and form a carbocation. Rearrangement within the carbocation does not occur

because it is already in its most stable form (tertiary carbocation). This cation is then trapped

27

by the methanol to form tert-butyl methyl ether. The mechanism is shown in the figure below

[28]:

Figure 10: Mechanism of TBA to MTBE catalysed by sulfonic acid resin

Similarly, a reactive distillation column can be used for the synthesis of MTBE from

TBA and methanol using ion exchange resin. TBA and methanol are fed continuously into a

catalytic packed column. The MTBE produced can be separated as a top product. The water

produced can be obtained as a bottom product. As proposed by Mohammed Matouq et al, [29]

the reactive distillation column is separated into 2 zones: reaction zone and separation zone.

The reactants are mixed in the presence of catalyst bed and the products formed are boiled

and separated in fractional distillation column. Water and TBA with higher boiling points,

existed in the reaction. MTBE with lower boiling point existed in the separation zone.

Meanwhile, methanol with its middle boiling point existed in both reaction and separation

zone.

Zhang Ziyang et al [30] carried out the experiment and identified that the purity of

MTBE in the product formed is quite low, which is0.7611. To increase the purity of MTBE,

azeotropic separation can be performed but additional expenditures have to be allocated such

as capital cost and maintenance cost. The flow of the direct synthesis of MTBE from TBA

and methanol is illustrated in the block flow diagram below.

Figure 11: Block flow diagram for direct conversion of TBA to MTBE (formerly the Texaco process;

now the Huntsman process)

22

2.2 Comparison between Alternatives Table 1: Comparison between Alternatives

Green Chemistry and Sustainability

Method Production of MTBE from butane

(UOP-Oleflex)

Production of MTBE from

isobutylene

Production of MTBE from Tert-Butyl

Alcohol (TBA)

Raw Material Isobutylene and methanol Isobutylene and methanol Tertiary butyl alcohol (TBA) and methanol

Nature of the Raw

Material

Non renewable Non renewable Non renewable

Reaction a) Isomerization:

Butane Isobutane

b) Dehydrogenation:

i) Desired reaction:

Isobutene Isobutylene +

Hydrogen

ii) Side Reaction:

1.Isobutane + hydrogen

Propane + Methane

2. Propane Propene +

Hydrogen

3. Isobutene Carbon +

Hydrogen

d) Etherification (Ethermax):

Desired Reaction:

Etherification:

a) Desired Reaction:

Isobutylene + MeOH MTBE

b) Side reaction:

1. Isobutylene + Isobutylene

Di-isobutylene

2. MeOH + MeOH Dimethyl

Ether + H2O

3. Isobutylene + H2O TBA

a) Desired Reaction:

TBA + MeOH MTBE + H2O

b) Side reaction:

MeOH + MeOH Dimethyl ether +H2O

23

Isobutylene + MeOH MTbe

Purity of MTBE N/A 0.991 0.7332

Yield of MTBE N/A N/A 0.7611

Conversion of

MTBE

0.99 0.95 0.8524

Catalyst

Catalyst Used a) Isomerization step: Platinum

supported on alumina with HCl as

promoter

b) Dehydrogenation step:

Platinum supported on alumina

c) Etherification (Ethermax):

Acid resin

a) Acidic ion exchange resin

b) Acidic solid catalyst such as

sulphonic ionic rubber

OR

Amberlyst-15

Sulfonic acid resin catalyst [31]

Catalyst Recovery Dehydrogenation step: Catalyst

will remove from the last reactor

and regenerated separately

Catalyst life is usually one year N/A

Environment Impact

Effect of product

to environment and

health

Breathing large amounts of MTBE for short periods of time adversely affects the nervous system of animals. Effect

range from hyperactivity and incoordination to convulsions and unconsciousness. MTBE by itself is not likely to

cause environmental harm at levels normally found in the environment. MTBE can contribute to the formation of

photochemical smog when it reacts with other volatile organic carbon substances in air. [32]

By product Propane, Methane, Propene,

Hydrogen, Carbon

Diisobutylene, Dimethyl ether,

Water, Tertiary Butyl

Dimethyl ether, Water

24

alcohol,Untreated Methanol

Effect of by-

product to

environment

Methane able to absorb infrared

radiation at a rate 21 times greater

than greenhouse gas CO2. [33]

1. Diisobutylene: very toxic to

aquatic life with long lasting

effects. [34]

2. t-butyl alcohol:

3. dimethyl ether: not expected to

be persistent in the environment

and is not bio accumulative [35]

Dimethyl ether: not expected to be

persistent in the environment and is not bio

accumulative.

Energy Consumption

Energy Consumed a) Isomerization: energy

consumption is intermediate.

Isomerization is exothermic

reaction. Low temperature is

favorable for the process.

However from kinetic point of

view, activity of catalyst increase

with temperature. Thus, optimum

temp is used in this step.

b) Dehydrogenation step: energy

consumption is high as

dehydrogenation is endothermic

reaction. High temperature is

favorable. Inter-stages furnace are

used.

Energy consumption is low as the

reaction of isobutene and

methanol is exothermic process.

Low temperature is favorable for

the formation of MTBE.

The reaction between TBA and MeOH is

endothermic, the application of external

heat to the distillation column is desirable

in maintaining the temperature profile of

the column and the rate of the reaction.

[36]

Way to control Heat exchanger to control the Heat exchanger to control the Heat exchanger to control the temperature

25

energy

consumption

temperature of isomerization unit temperature of packed bed reactor of column.

Flexibility of Operation

Temperature a) Isomerization:

110~ 170 oC

b) Dehydrogenation step:

600~610 oC

50-85 oC

<250oC

Pressure a) Isomerization:

1470~2180kPa

b) Dehydrogenation step:

40 to 140kPa

700 to 1500 kPa Atmospheric pressure

Reactor Type a)Isomerization:

Deisobutanizer (DIB) column,

2 reactors

b) Dehydrogenation step:

3 radial-flow reactors, inter-stage

furnaces and regeneration system

Packed bed reactor, Distillation

unit, Raffinate stripper or

moiseive-based unit

Reactive distillation column which carry

out chemical reaction and separation

simultaneously

Safety Factor

Safety precaution Temperature and pressure of

Oleflex unit should be maintained

at desired range to prevent

runaway reaction occurs as it

involves high temp and pressure.

Temperature of reactor should

maintained at desired temperature

as the reactants and product

formed are flammable. The

reactant are both flammable.

Temperature of the reactor should be

maintained at desired temperature as the

reactants and product formed are

flammable. Suitable respiratory equipment

must be worn in case of insufficient

26

Methanol is flammable. Thus,

should keep away from heat, open

flames and sparks.

Thus, should keep away from

heat, open flames and sparks.

ventilation or confined space

Health concern 1) Butane: vapors are not

irritating. However contact with

liquid or cold vapor may cause

frostbite, freeze burns and

permanent eye damage. Same

condition happen when direct

contact to skin and through

ingestion. Inhalation of

concentration of about 10,000ppm

may cause central nervous system

depression such as dizziness,

drowsiness, headache and similar

narcotic symptoms, but no long

term effect.

2. Methanol: flammable liquid and

vapor. Harmful if inhaled. Maybe

fatal or cause blindness if

swallowed. May cause central

nervous system depression. May

cause digestive tract irritation with

nausea, vomiting and diarrhea.

Causes respiratory tract irritation.

May cause liver, kidney and heart

damage.

1.Isobutylene: Inhalation of

moderate concentrations causes

dizziness, drowsiness and

unconsciousness. Contact with

eyes or skin may cause irritation;

the liquid may cause frostbite

[37]

2.Methanol: flammable liquid

and vapor. Harmful if inhaled.

Maybe fatal or cause blindness if

swallowed. May cause central

nervous system depression. May

cause digestive tract irritation

with nausea, vomiting and

diarrhea. Causes respiratory tract

irritation. May cause liver, kidney

and heart damage

1. TBA: flammable liquid. May cause

central nervous system depression. Maybe

adsorbed through the skin. May cause eye

and skin irritation. May cause respiratory

and digestive tract irritation

2.Methanol: flammable liquid and vapor.

Harmful if inhaled. Maybe fatal or cause

blindness if swallowed. May cause central

nervous system depression. May cause

digestive tract irritation with nausea,

vomiting and diarrhea. Causes respiratory

tract irritation. May cause liver, kidney and

heart damage

Potential of cause Reactants and product are

flammable in the presence of open

Reactants and product are

flammable in the presence of fire,

The product formed is flammable in the

presence of open flames and sparks.

27

accident flames and sparks. High temp and

pressure in Oleflex unit might

cause run away reaction or

explosion occur. Excessive

breathing in of methanol and

MTBE may cause fatal.

open flames and sparks.

Excessive breathing in of

methanol and MTBE may cause

fatal

Excessive breathing in of tert-butanol,

methanol and MTBE may cause fatal.

Waste Management

Waste Pentane and other heavier material

from deisobutanizer (DIB)

column. By products such as

propane, methane, propene,

hydrogen and carbon.

Waste such as inert butane,

isobutane and etc from refinery.

By products such as di-

isobutylene, dimethyl ether,

water, TBA. Unreacted methanol.

Water, unreacted methanol, unreacted tert-

butanol and insignificant amount of

dimethyl ether and isopropyl tert-butyl

ether

Handling of waste Unreacted methanol recycled back

to reactor. Pentane, propane,

methane, propene and hydrogen

can used as fuel.

Unreacted methanol recycled

back to reactor. Water can used

for extraction of unreacted

methanol.

Unreacted methanol and tert-butanol can

be separated from the product stream and

recycled but this involve addition

installation of separation unit which

increase the capital and maintenance cost.

31

2.3 Choice of Process As shown in table above, the three alternative ways to produce MTBE have been

discussed in terms of green chemistry and sustainability, environmental impact, energy

consumption, flexibility of operation and safety factors and waste management. In order to

choose the most suitable and feasible process alternative for our plant design, the advantages

and disadvantages of each aspect have been taken into account and thorough considerations.

There are 3 alternative ways to produce MTBE which has shown as below:

Method 1: MTBE production from n-butane

Method 2: MTBE production from isobutylene

Method 3: MTBE production from tertiary butyl alcohol (TBA)

Among the alternatives of the process suggested, the direct synthesis of MTBE from

isobutylene and methanol is the most applicable route path since it has the several advantages

among other routes. It will further discuss on several aspects as shown below.

2.3.1 Safety and Health Issues: Safety and health issues are the most crucial issues that must be considered when

selecting the material that being used in the plants. This is because the safety and health

issues not only covered the workers but also to the surrounding residential areas.

Firstly, we analyze the safety and health issues from the aspect of temperature of the

process. Desired temperature should be maintained throughout the process to prevent run

away reaction occurred. For method 1, there are 3 basic steps (isomerization,

dehydrogenation and etherification) involved in order to produce MTBE. Isomerization and

etherification (Ethermax) process are exothermic process. Thus, low temperature is favorable

in these two processes. In isomerization process, the desired temperature is 110 to 170oC.

While for etherification process, the desired temperature is 50 to 85oC. However, high

temperature is required for dehydrogenation process which is 600 to 610oC. This is because

dehydrogenation process is endothermic reaction. High temperature is favorable for the

formation of product.

For method 2, it only involve exothermic reaction. The desired temperature is 50 to

85oC. On the other hands, for method 3, it involved both exothermic and endothermic

reaction (dehydration and etherification). TBA dehydration to isobutylene is an endothermic

32

reaction. Thus, high temperature (<250oC) is favorable for the process. Whereas

etherification is exothermic reaction, low temperature of 50 to 85oC is required.

Next, we will analyze the safety and health issues from the aspect of pressure of the

process. Same as temperature, pressure is needed to maintain within the desired range. High

pressure might cause rupture of reactor or even explosion occur. In method 1, high pressure is

involved in isomerization step which is 1470 to 2180kPa. Besides, moderate pressure is used

in both dehydrogenation and etherification process. On the other hands, moderate pressure

which is 700 to 1500kPa is required for the etherification process. Lastly, atmospheric

pressure is required in method 3 which is the lowest pressure required compared to the others

two methods.

From the aspect of raw material, three methods use different raw materials which are

butane, isobutylene and TBA in order to produce MTBE. From the aspect of fire hazard, all

the raw materials are highly flammable. Hence, they must keep away from heat, sparks, open

flames or hot surfaces. From the aspect of health hazard, high exposure to butane will causes

drowsiness but no other evidence of systemic effect. On the other hands, inhalation of

moderate concentration of isobutylene will cause dizziness, drowsiness and unconsciousness.

Besides, contact with eyes or skin may cause irritation; the liquid may cause frostbite. While

for TBA, its vapor is narcotic in action and irritating to respiratory passages and its liquid is

irritating to skin and eyes. [37] In addition, among the three raw materials, TBA has been

classified as hazardous under Global Harmonized System of Classification and Labeling of

Chemicals (GHS) for its health effects.[38] Thus, extra careful is needed when handle with

TBA compared to isobutylene and butane.

Thus, we can conclude that method 2 is more applicable route path from the aspect of

safety and health issues. This is because reaction path in method 2 require low temperature

and moderate pressure. Besides, the raw material used in method 2 is not the most hazardous

compared to TBA used in method 3.

2.3.2 Environmental Issues: Generally, all of raw materials used are non-renewable sources. Besides, the product

itself which is MTBE will bring some environmental issues. Breathing large amounts of

MTBE for short periods of time adversely affects the nervous system of animals. Its effect

range from hyperactivity and incoordination to convulsions and unconsciousness. MTBE can

contribute to the formation of photochemical smog when it reacts with other volatile organic

33

carbon substances in air. [32]Thus, comparison between the by-products from the three

alternative route paths is our main focus.

For method 1, there are several by-products produced. Most of the by-products come

from the dehydrogenation process. One of the by-products is methane. Methane able to

absorb infrared radiation at a rate of 21 times greater than greenhouse gas, CO2. Thus, if the

by-product is not handle carefully and release to the atmosphere, it will lead to greenhouse

phenomena. Same as method 1, there are also several by-products formed through method 2.

One of the by-products which is di-isobutylene is very toxic to aquatic life with long lasting

effects. Thus, it has to handle carefully before it discharges from the reactor. Lastly, for

method 3, only two type of by-products produced which is water and dimethyl ether. Water

basically is not harmful to the environment. On the other hands, dimethyl ether is extremely

flammable and may form potentially explosive mixtures with air. Thus, we should not release

it to surrounding environment to prevent soil and water pollution.

All these route paths will produce by-product that might causes environmental issues

if mishandling them. However, method 3 only produces two kinds of by-products which is

water and dimethyl ether. Thus, the probability of mishandling of by-product is lower

compared to others two methods as method 1 and 2 have more by-products to handle with. In

conclusion, method 3 is more applicable route path in the aspect of environmental issues.

2.3.3 Public Issues: In August 1995, the City of Santa Monica discovered MTBE in drinking water supply

wells at its Charnock Wellfield. By 1996, persistent and increasing levels of MTBE at

concentrations as high as 600μg/L caused all of the Charnock Wellfield supply wells to be

shut down. Several public supply wells in South Lake Tahoe were found to be impacted by

MTBE. In 2001, the South Tahoe Public Utility District took 12 of the District’s 34 drinking

water wells off-line due to the detection or nearby presence of MTBE. In Glennville,

California, MTBE was detected in drinking water at some of the highest levels of MTBE ever

recorded. One well tested at 20,000 parts per billion. As of November 2009, MTBE had been

detected in 27 of approximately 4800 active and standby public groundwater sources at

concentrations greater than the SMCL (secondary maximum contaminant level) of 5.0μg/L.

MTBE was detected above the MCL (maximum contaminant level) of 13μg/L in 9 of those

active and standby public groundwater sources, and has also been detected in significant

concentrations in domestic and in small water system wells in many parts of the state. [39]

34

From the history of occurrence stated above, it shows that contamination of water

sources by MTBE is one of the serious public issues caused by MTBE plant. Fairly small

amounts of MTBE in water can give it an unpleasant taste and odor, making the water

undrinkable. MTBE also does not break down (biodegrade) easily. As a result, it is harder to

clean up once contamination occurs. [40]

For method 1, it involves 3 basic steps to produce MTBE. The plant for production of

MTBE can considered quite large compared to method 2 which only required one basic step.

More piping system and reactors involved in method 1 compared to method 2. Extra by

products and reactions have to take care compared to method 2. Thus, it will increase the

probability of leakage of MTBE to environment. For method 3, it involved the dehydration of

TBA and water is produced together with MTBE. Separation process is required to segregate

MTBE from water. Besides, necessary treatment is required for water before it discharge to

the environment in order to ensure water is free of MTBE. Thus, method 3 has the highest

probability to cause contamination of water sources if treatment of by-product which is water

is not carry out well.

In conclusion, method 2 is more applicable route path in the aspect of public issues.

This is because it only involved one basic step. Thus, it is easier to handle compared to

method 1 and 3.

2.3.4 Flexibility and Controllability:

In terms of the availability of the feedstock, Method 1 that use butane as their raw

material are abundant in many parts of the world. Similarly, the feedstock (C4 olefins mixture)

of the Method 2 is highly abundant in all around the world as well. There are a lot of

Refinery/Petrochemical Plants in the world for example Saudi Arabia, Venezuela and China

that can supply the demand of the feedstock to our plant. Thus, if the supply of the feedstock

is less in Malaysia, it is not a problem for us to get the feedstock from other countries.

However, tert-butyl alcohol (TBA) that is obtained as a side product from the propylene

oxide (PO) manufacturing plant. Hence, its source is highly dependent on the production of

PO. Also, the price of TBA is also slightly higher than isobutylene. [41] Hence, Method 2 is

more attractive compared to other alternatives for the production of MTBE in terms of

flexibility of feedstock.

35

For Method 1, there are 2 reactions that require two difference temperature and

pressure range for the reactions to occur. The desired temperature that is required to yield

MTBE in the second reaction is between 600oC and 610

oC, which is the highest compared to

the other methods. In addition, this narrow 10oC range and presence of two desired

temperature range for two different reactions have actually increased the difficulty and

complexity in controlling the reaction. Similarly, the pressure that required to promote the

isomerization in Method 1 is as high as 2180kPa. Meanwhile, Method 2 has the lowest

temperature (50oC-85

oC) condition and wider range for production of MTBE. The required

pressure is intermediate which is about 700kPa to 1500kPa.For method 3, the optimum

temperature for the reaction to occur can reach as high as 250oC and the reaction can occur

under atmospheric pressure. When comparing these three methods, Method 2 is still the best

choice temperature-wise, and when it is studied from the point of pressure, it is placed as

second after Method 3.

For controllability, Method 2 is the best as alternative and technology. Method 2 is

well established and is less complex compared to the other MTBE production plants, so the

process can be easily controlled. Other methods are more complicated such as Method 1

which requires dehydrogenation process before the MTBE can be formed by etherification

process. In other words, less unit operation is used compared to other alternatives routes, so

much easy to control. When the number of unit operations is less, the amount of energy

needed to operate the plant also will remain low. Based on the analysis, Method 2 is the

alternatives that give the most desired condition in terms of flexibility and controllability.

Thus, Method 2 is chosen as the route to produce MTBE.

2.3.5 Economic Indicators and Market Background Analysis: One of the raw materials used in three of the methods are same. Methanol is the

common feedstock that is required to produce MTBE no matter which route is chosen. In all

the three routes, pure methanol is obtained from refinery.

Butane comes from natural gas. It is derived from fossil fuel, created over the course

of millions of years by a complex process deep inside the earth from the remains of plants,

animals, and numerous microorganisms. [42]The butane that is used in Method 1 is obtained

from refineries. The raw material that is required for Method 2 is C4 olefin mixture, which

contains isobutylene is obtained from the petrochemical refineries. Malaysia is the second-

largest oil producer in Southeast Asia [43], and has the fifth largest oil reserves in the Asia

36

Pacific region. [44] Thus, there are a lot of oil refineries all around the Malaysia that make

Malaysia able to produce 642,700 barrel of oil per day in 2012[45]. Even all the oil refineries

in Malaysia do not want to supply their C4 stream product to our plant, we still can buy

isobutylene from overseas (i.e. China). According to Honeywell’s UOP base in China, there

are currently five C4 Oleflex units in operation, producing nearly 2 million metric tons of

isobutylene annually [46]. This is a large production rate so it would not be a problem in

getting the raw material we wanted for Method 2. For Method 3, the raw material TBA which

is obtained from propylene oxide producer is not feasible because there is no propylene oxide

plant in Malaysia.

In term of raw material price, butane is the cheapest compared to isobutylene and

TBA. However, Method 1 which is highly intensive because it consists of more unit

operation compared with Method 2 and Method 3. According to the official webpage of the

world's largest petrochemical market information provider, ICIS, the price of TBA is higher

than isobutylene, thus it is preferable to buy isobutylene instead of TBA. In addition, if

Method 3 is chosen, in order to get a sufficient amount of TBA, we probably have to buy it

from the largest producer of propylene oxide which is situated at United States. [47] Due to

the longer distance compared to China, this will subsequently increase the transportation cost

of raw material.

In terms of global demand, Argus DeWitt claimed that MTBE demand has increased

in the past few years driven by cleaner fuel requirements in China and increased gasoline

consumption in Asia, Americas, and the Middle East.Argus is a leading provider of data on

prices and fundamentals, news, analysis, consultancy services and conferences for the global

crude, oil products, LPG, natural gas, electricity, coal, emissions, bioenergy, fertilizer,

petrochemical, metals and transportation industries. According to Argus DeWitt 2015 Fuels

and Oxygenates Annual report [48], MTBE demand is expected to increase steadily in the

years to come but global operating rates will weaken as China overbuilds MTBE capacity.

Figure below shows the history and projections of global MTBE supply and demand from

2010 to 2020.

37

Figure 12: History and projections of global MTBE supply and demand from 2010 to 2020

Based on the figure above, it is clear that the global demand of MTBE in the next few

year is expected to increase. In this 2015 annual report, Argus DeWitt also pointed out that

Europe which initially switched most of their oxygenates to ETBE, but in the last few years

have toggled back several of their swing plants to MTBE, primarily due to cost and enough

bio-fuel credits. Also, gasoline demand in the Middle/East has been increasing in the past few

years along with the usage of MTBE. Argus DeWitt expects MTBE exports out of the Middle

East to decline as internal usage increases. All these have contributed to the increment of the

MTBE global demand in the next few years. Also, a report on Methyl Tertiary Butyl Ether

(MTBE) Market Analysis published by Grand View Research last year, claimed that there

will be a significant growth over the next six years on account of its increasing consumption

as a fuel additive in gasoline engines. [48]Therefore, we can conclude that MTBE production

plant will be a profit making plant for the next few years. Not to forget, by supplying the

surplus MTBE to global market will not only glorify Malaysia, but also spur the growth of

Malaysian economy.

2.3.6 Current related problem of the plant to the environment and

society: Contamination of Water Source:

As mentioned previously, the leaking of MTBE to underground is one of the problems

of the plant to the environment. This is because MTBE is soluble in water and will lead to

contamination of water when leakage occurs. It might cause environmental pollution when it

38

leak to river or lake. Besides, it will cause problems to society as it contaminates the drinking

water source. The recent case of contamination of water source occurred in South Lake

Tahoe. Several public supply wells were found to be impacted by MTBE. In 2001, the South

Tahoe Public Utility District took 12 of the District’s 34 drinking water wells off-line due to

the detection or nearby presence of MTBE. In Glennville, California, MTBE was detected in

drinking water at some of the highest levels of MTBE ever recorded. One well tested at

20,000 parts per billion. As of November 2009, MTBE had been detected in 27 of

approximately 4800 active and standby public groundwater sources at concentrations greater

than the SMCL (secondary maximum contaminant level) of 5.0μg/L. MTBE was detected

above the MCL (maximum contaminant level) of 13μg/L in 9 of those active and standby

public groundwater sources, and has also been detected in significant concentrations in

domestic and in small water system wells in many parts of the state. [39]

Fire Incident:

As we know, MTBE is extremely flammable with a high vapor pressure. It is use only

with good ventilation and avoids all ignition sources. [1] The recent explosion and fire

incident occurred at a Huntsman Petrochemical Corp. plant in Port Neches, Tex., near the

Louisiana border. According to board investigators, the fire occurred as works prepared a

process pipe for scheduled maintenance within 27 000 b/d that produces MTBE. The plant

personnel did not know at the time that the pipe contained residual feedstock chemicals said

by CBS officials. Workers directed steam through the pipe and inadvertently caused the

residual chemical inside to overheat and decompose as part of the shutdown. According to

investors, the pipe was ruptured due to accumulating of pressure and releasing a flammable

vapour cloud then ignited. Two workers were sent to the hospital with second degree burns

and caused minor injuries to several others. The explosion and fire apparently occurred

during a maintenance shutdown operation in the plant the produces propylene oxide and

methyl tertiary butyl ether (MTBE). [50] Flammable vapour cloud will cause environmental

pollution. The released toxic gas during explosion will also affect nearby residential areas as

it might cause health problem in society

39

Chapter 3: Critical Assessment of the Process Chosen

3.1 Capacity of Plant After researching and discussing among our group members for several times, the

production capacities of our designed plant are fixed at 300,000 tonnes of methyl tert-butyl

ether (MTBE) per year. The capacities are decided based on the following factors:

1. MTBE world market outlook in terms of it demand

2. Production and profit sharing of the plant

3. The size of the plant as well as the equipment used

The main reason that we set the capacity that high is due to its high demand for the next

five year. According to research report on Global Methyl Tertiary Butyl Ether (MTBE)

Market Analysis, Market Size, Application Analysis, Regional Outlook, Competitive

Strategies And Forecasts, 2014 To 2020 published by Grand View Research, Inc., Methyl

tertiary butyl ether (MTBE) market is expected to witness significant growth over the next

five years on account of its increasing consumption as a fuel additive in gasoline engines. In

addition, the growing automobile industry in Asia Pacific mainly Japan, China and India is

expected to drive demand for MTBE over the next five years.[49] Thus, by producing at this

capacity, we are expecting our plant to become one of the largest productions of MTBE to

fulfil the demand requirement in Asia Pacific.

The figure below shows the fuel ethers demand in Asia from 1992-2011. It is obvious that

the demand of ethers (i.e. MTBE) in Asia is increasing drastically from year to year. The high

demand of MTBE as the oxygenate in fuel is mainly due to the phase out of lead. Also,

SIBUR, a Russian gas processing and petrochemicals company has expanded its methyl

tertiary butyl ether (MTBE) designed capacity in Tchaikovsky, Perm Territory, from 200,000

to 220,000 tonnes per year.[53]This has further convince us to have such high production rate

as the MTBE demand in Asia is the highest in the world. [54]

40

Figure 13: Fuel ether demand in Asia from 1992 to 2011

Figure 14: The amount of new vehicles registered in Malaysia [55]

Also, the no. of cars that sold in Malaysia is increasing since 10 years ago. As

depicted in the graph above, the number of new vehicles registered in Malaysia, there is a

drop in number of vehicle registered for the past few months, and it is probably due to the

depreciation of our country currency, Ringgit Malaysia. However, a lot of economists and

government minister such as central bank governor Dr Zeti Aktar Aziz believed the

weakening currency to be a short term problem. And, most of them are confident the ringgit

will eventually bounce back. So, the no. of cars on the road will increase as well. Generally,

the graph below shows that the number of vehicles registered in Malaysia is increasing

annually. Thus, the amount of MTBE required will raise as the petrol consumption is

increased as well (shown in the figure below).

41

Figure 15: Malaysia motor gasoline consumption per year [56]

Figure 16: Structure of the global production of MTBE by country, 2013

Figure above shows that Asia is the largest producer of MTBE in the world as the

demand of MTBE in Asia is also the highest. Based on an article published by Merchant

Research & Consulting, Ltd., the global demand for MTBE was over 15.3 million tonnes in

2013. [57] Comparing to the production capacity of out plant (300k tonnes), our targeted

capacity is just 0.02% of the total production in world. Thus, it is still acceptable to have this

production rate of 300 000 metric tonnes per annum.

Furthermore, based on the only MTBE plant capacity that currently available in

Malaysia, MTBE Sdn. Bhd and the annual production rate is found to be 300,000 tonnes per

year as well. It used to be exporter but became medium-sized importer in the last few years.

[58] Therefore, we believe this capacity would be sufficient for all supplies in Malaysia and if

more than sufficient, then it will be exported.

42

3.2 Plant Location [51] [52]

Figure 17: The Location of Plant at Teluk Kalong, Terengganu, Malaysia

The location of the plant can have a crucial effect on the profitability of a project and

for future expansion of company. Many factors must be considered when selecting a suitable

site to enhancing the production. The proposed plant must be acceptable to the local

community. Full consideration must be given to the safe location of the plant so that it does

not impose a significant additional risk to the community. After deep discussion, we decided

to choose Teluk Kalong, Terengganu, Malaysia.

Teluk Kalong is an Industrial Estate located 9.6 km from Kemaman district. Teluk

Kalong consists of 1429.00 hectares as total developed area and total area available is 125.10

hectares which sufficient for the production of MTBE. Next, Terengganu’s industrial land is

one of the cheapest in Malaysia. We can get the land at RM0.18 to RM 5.60 (US$0.06 to

$1.75) per square foot compared to other states where land sells from lows of RM2.00 to

RM4.50 to highs RM18.00 to RM22.00 per square foot. The land also flat, well drained and

suitable for load-bearing characteristic. Terengganu also provided ready-built factories with

pre-installed facilities which premium RM45.00 to RM60.00 per 𝑚2 . Moreover, Teluk

Kalong is proposed for petrochemical and heavy industry petrochemical which is very

strategic for production of MTBE.

Teluk Kalong is a matured Industrial zone with good access to electric supply, water

supply and gas supply. Electrical power will be needed for the plant as most of the plant

43

facilities need electricity to operate. For example compressor and pump used in the plant

need electric power to operate. Thus, the electricity is generated at the Tenaga Nasional

Berhad and total generation capacity is 900 MW. There is no major breakdown and low

frequency of interruption had occur before. There also special industrial tariff of electricity

for industrial consumer which is minimum monthly charge is RM600.00. Water is used as

cooling medium in the plant due to its high heat capacity, lower cost, available in abundance

and it is renewable. Water is used as cooling medium in the plant due to its high heat capacity,

lower cost, available in abundance and it is renewable. Chemical processes require large

quantities of water for cooling and general process used and the plant must be located near a

source of quality. Therefore, water is supply by Terengganu Water Company (SATU) located

in Bukit Shah. SATU also give minimum charge RM50.00 to industrial plant with RM1.15

water rate per 𝑚3. Gas is supplied by Gas Malaysia or Petronas Gas with negotiable rates

based on the quantity demanded.

The transport of materials and products to and from the plant will also be

consideration in site selection. The site that we are considered is close to at least two major

forms of transport: road, rail, airport or a sea port. Road transport is suitable for local

distribution from central warehouse. Air transport is convenient and efficient for the

movement of personnel and essential equipment. The road, sea port and airport facilities are

easily accessible from the Teluk Kalong industrial area. The ports located around Terengganu

are Kemaman Port, Kerteh Port and Kuantan Port while airport nearby are Kuala Terengganu

Airport and Kerteh Airport.

The availability and price of suitable raw materials is one of factors to determine the

site location. Plant producing bulk chemicals are best located close to the source of the major

raw material. This meant our plant of MTBE also close to the marketing area. The raw

materials supplier of Isobutylene is available from MTBE Gebeng Plant, Pahang and

Methanol is available from Petronas Chemical Group Berhad.

All industrial processes produce waste products and full consideration must be given

to their disposal. The disposal of toxic and harmful effluents of production of MTBE must be

covered by local regulations. Therefore, Terengganu employs an integrated environmentally

friendly waste management system for industrial wastes. The monthly charges vary for

disposal of toxic waste carried out by Kualiti Alam according to the type and quantity of

waste. There are solid and liquid waste form for packaged waste and bulk wastes. The

scheduled waste disposal also is provided by Aldwich-Enviro Management and sewerage

44

services are carried out by Indah Water Consortium with charges are based at RM2.50 per

employee per month.

3.3 Complete Description of Process Chosen There are numerous variations on MTBE plant designs. In general, an MTBE plant is

comprised of the following sections:

Reactor section

MTBE recovery section

Methanol recovery section

MTBE is produced from isobutylene and methanol which is liquid phase in a packed bed

reactor. Isobutylene is comes from fluid catalytic cracking (FCC) operations in refineries as a

by-product. Since others inert isomers present in the C4 stream from FCC will not react with

methanol, we assume that the feed stream from FCC only consists of isobutylene. On the

other hands, methanol is the common feedstock that can obtain from refinery. Our project

scope included the following steps:

1. Etherification process

2. Distillation process for MTBE

3. Liquid-liquid extraction process

4. Recovery of methanol

Etherification process:

Figure 18: Etherification Process in Packed Bed Reactor

45

The etherification process of methanol and isobutylene is an exothermic reaction. This

exothermic reaction takes place in the liquid phase at 80oC and 1000kPa. High temperatures

are not recommended due to possibility of catalyst deactivation, which becomes unstable at

temperature of 130oC. Operation of the unit at lower temperature enables safe operation and

long lasting catalyst.[20] The reaction occur inside the packed bed reactor is shown below:

(CH3)2C=CH2 + CH3OH ↔ (CH3)3C-O-CH3 ∆Ho298 ≈ -37kJ/mol

The isobutene conversion (XIB), yield IB to MTBE (YMTBE) and selectivity to MTBE

(SMTBE) using Amberlyst 15 catalyst is 90, 87 and 97% respectively [103].

However, there are 3 main side reactions occur during the synthesis of MTBE. The main

by-products from the side reactions are di-isobutylene, dimethyl ether (DME) and tertiary

butyl alcohol (TBA). The equation for side reactions are shown below: [6]

3 (CH3)2C(CH2) + (CH3)2C(CH2) ↔ (CH3)3C(CH)C(CH3)2

Isobutylene + Isobutylene ↔ Di-isobutylene

4 (CH3)OH + (CH3)OH ↔ (CH3)O(CH3) + H2O

Methanol + Methanol ↔ Dimethyl ether + Water

5 (CH3)2C(CH2)+ H2O ↔ (CH3)3C(OH)

Isobutylene + Water ↔ Tertiary butyl alcohol

However, there are no reported works on the selectivity of the side reaction during the

synthesis of MTBE from isobutylene and methanol. Several strategies have been used to

reduce the production of these undesirable by-products. First, the ratio of methanol and

isobutylene is kept above one to suppress the dimerization of butane. Reaction temperatures

below 100oC can diminish the formation of dimethyl ether. Finally, the pretreatment of the

feed stream which is removal of water can prevents the formation of TBA [104].

46

Distillation Process for MTBE:

Figure 19: Distillation Column Process for MTBE

The product MTBE, by-products and unreacted feeds from the etherification process

will sent to MTBE tower which is a distillation column to separate the product from the

others component. It is complicated due to the presence of minimum boiling azeotropes

between MTBE and methanol and isobutylene and methanol. [59]

The vapor-liquid equilibrium and the chemical equilibrium of the ternary system

MTBE/ methanol/ isobutene are illustrated in the figure below. There are two minimum

azeotropes in this mixture, one between the higher boiler MTBE and the intermediate boiler

methanol and the second between methanol and the low boiler isobutene. The pressure used

for distillation process is 500kPa. According to Andreas Beckmann et.al, at a pressure of

500kPa, the equilibrium curve does not intersect either of the two locus curves of reactive

azeotropes anywhere in the entire concentration space. Accordingly, no reactive azeotrope

exists in the system under these conditions. Thus, separation of MTBE from isobutylene and

methanol is easier.

47

Figure 20: Vapor-liquid equilibrium and chemical equilibrium of the ternary system MTBE, methanol

and isobutene [105]

Liquid-liquid extraction process:

Figure 21: Liquid- liquid Extraction Column

The mixture of by-products, mixed C4 and methanol is further separate using liquid-

liquid extraction process. In order to recycle back the unreacted methanol, we have to

separate it from C4 stream and by-products using a liquid-liquid extraction column. Water is

48

used during the removal of methanol from a C4 stream. This is because methanol is highly

soluble in water but evolves back out of the water if recycled. [60]

Recovery of Methanol:

Figure 22: Recovery of Methanol using Distillation Column

The mixture of methanol and water is further separate using distillation column where

the distillation process is carried out at 1 atm. Methanol is distilled off as the top product

while the water is collected as the bottom product. 99.5% purity of methanol can obtained

through distillation process. [61] The methanol and water is further recycled back to the

etherification process and liquid-liquid extraction column respectively.

Reaction Kinetic of Process:

The reaction rate expression for the MTBE is shown as following:[62]

𝑟𝑠 = 𝑘𝑠𝐾𝑎

[ 𝐶𝐴𝐶𝐵

0.5 −𝐶𝐶

1.5

𝐾𝑒𝑞

(1 + 𝐾𝐴𝐶𝐴 + 𝐾𝐵𝐶𝐵)1.5

]

49

Where:

𝑘𝑠 = 𝑠𝑢𝑟𝑓𝑎𝑐𝑒 𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛 𝑟𝑎𝑡𝑒 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 = 1.2 × 1013 exp(−87900

𝑅𝑇) ,

(𝑔𝑚𝑜𝑙𝑒

𝑔 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡)1.5

ℎ𝑟

𝐾𝐴 = 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑢𝑚 𝑎𝑑𝑠𝑜𝑟𝑝𝑡𝑖𝑜𝑛 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 = 5.1 × 1013 exp(97500

𝑅𝑇),

𝑔 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡

𝑔𝑚𝑜𝑙𝑒

𝐾𝐶 = 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑎𝑑𝑠𝑜𝑟𝑝𝑡𝑖𝑜𝑛 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 = 1.6 × 10−16 exp(119000

𝑅𝑇),

𝑔 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡

𝑔𝑚𝑜𝑙𝑒

𝐾𝑒𝑞 = 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

𝐶𝐴 = 𝐼𝑠𝑜𝑏𝑢𝑡𝑦𝑙𝑒𝑛𝑒 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛,𝑚𝑜𝑙𝑒/𝑙

𝐶𝐵 = 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛,𝑚𝑜𝑙𝑒/𝑙

𝐶𝐶 = 𝑀𝑇𝐵𝐸 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛,𝑚𝑜𝑙𝑒/𝑙

Table 2: Advantages and Disadvantages of Direct Synthesis of MTBE from Isobutylene and Methanol

Advantages Disadvantages

Low temperature and pressure

Long catalyst life (usually one year)

Small area required for plant site

(only involve one basic step)

High selectivity

Desired conditions have to

maintained to prevent formation of

by-products

3.4 Similar Plant in Malaysia [75] Table 3: Similar Plant in Malaysia

Plant Methyl Tertiary Butyl Ether (MTBE)

Capacity 300,000 tpa MTBE, 80,000 tpa Propylene

Company MTBE Malaysia Sdn Bhd

Commissioning December 1992

50

Uses MTBE is a high quality additive for increasing the octane

level in unleaded gasoline.

Polypropylene is one of the fastest growing base polymers for

the manufacture of woven bags, plastics, films, ropes, chairs

and other industrial products.

This plant supplies propylene as feedstock to the

PETRONAS/BASF acrylic acid/acrylic esters plant and oxo-

alcohols complex.

3.5 Environment, Safety and Health Concerns

3.5.1 Environmental Concerns For each plant, environmental issue must be taken into consideration. Proper waste

disposal is needed to ensure the by product or effluent from the plant production do not cause

any impact to environment. We must well understand the environment effect of each by-

product before we can manage it in appropriate way.

It can be released into the environment via 3 ways which are air, water and soil. As

mentioned before, MTBE is volatile and may be emitted to the atmosphere through

evaporation during the distribution and use of gasoline containing MTBE. Long period and

high exposure to MTBE may be experienced by workers during the production, storage and

distribution of MTBE itself, and also of gasoline containing MTBE. Typical occupational

exposures are 4 to 45 mg/m³ during MTBE handling [76].

Most amounts of MTBE released into the environment will be distributed in the

atmosphere. Due to the solubility of MTBE in water, some of this atmospheric MTBE will

tend to be washed out by rain and enter surface water and shallow groundwater. Other than

that, if MTBE is spilled on the ground, rain water can dissolve MTBE and carry it through

the soil and into groundwater [77]. According to American Cancer Society, when MTBE gets

in the ground, it can travel faster and farther through groundwater than other gasoline

components due to its solubility in water. It makes it more likely to contaminate public water

systems and private drinking water wells if gasoline is spilled on the ground or leaks out of

underground storage tanks. Even fairly small amounts of MTBE in water can give it an

unpleasant taste and odour, making the water undrinkable. MTBE also does not break down

(biodegrade) easily. As a result, it is harder to clean up once contamination occurs [78].

51

Although there are occasion that MTBE or gasoline contained MTBE spilled directly

into the soil, MTBE can be effectively remediated by two soil treatment technologies,

typically without any costs beyond those needed for remediating other petroleum constituents.

This is because MTBE has a very high vapour pressure and a low affinity for sorption to soil.

Soil vapour extraction (SVE) is an in-situ soil treatment technology that removes volatile

contaminants from soil in the unsaturated zone above groundwater by extracting the

contaminant vapours with a vacuum that is applied to the subsurface. Low-temperature

thermal desorption (LTTD) is an ex-situ soil treatment technology that uses temperatures

below ignition levels to separate volatile contaminants from soil. However, SVE and LTTD

must be used soon after a release, before most of the MBTE moves from the soil into the

groundwater [79].

Anyway, according to the latest scientific information, there is no indication that

MTBE can persist long enough in the air at a level which would cause harm to environment

as it will be destroyed in atmosphere within days by photo-oxidation reactions [76].

3.5.2 Safety Concerns Safety is the main criteria in any plant operation. Since the production of MTBE

involves a number of chemicals, standard operating procedures (SOP) should be employed to

assist with working safely. Disobeying the SOP may cause runaway reaction. Anyway,

proper control system is needed to regulate the system parameter such as the reactor

temperature, to ensure the process operating condition is maintained at appropriate value,

thus minimize the occurrence of accident. Lastly, personal protection equipment should be

worn all the time to avoid or at least minimize the injury whenever we are working in the

plant. Now, let’s focus on the main raw material and the main product formed in the plant.

As we all know, MTBE is very volatile. MTBE will quickly evaporate from open

containers. In the open air, it will quickly break down into other chemical compounds, with

half of it disappearing in about 4 hours [77]. However, MTBE is highly flammable, so all the

appropriate safety precautions should be strictly observed during handling. It is considered as

explosive if its concentration in air is between 1.3 and 8% by volume.[76] Hence, fire source

such as spark should be prohibited in the production plant as the fuel (MTBE vapor) and the

oxygen (from air) is abundant in the factory. Also, air ventilation ca be introduced to

dilute/disperse the evaporated MTBE around the production site.

52

There are no specific exposure limits for isobutylene. However, fires impinging

(direct flame) on the outside surface of unprotected pressure storage vessels of isobutylene

can be very dangerous. Direct flame exposure on the cylinder wall can cause an explosion

either by BLEVE (Boiling Liquid Expanding Vapor Explosion), or by exothermic

decomposition. When isobutylene is on fire, it can be extinguished by shutting off the source

of the gas. Then use water spray or a foam agent to cool fire-exposed containers, structures,

and equipment [80].

As required by OSHA, the highest limit of methanol in working environment is 200

ppm TWA or 260 mg/m3 TWA. Since methanol is alcohol, it is considered as flammable as

well. To extinguish the fire burn on the methanol, water spray is recommended. Although

other side reaction can be avoided by operating the reaction at specified temperature range,

similar cares should be taken as well since all the product and side products are hydrocarbon

which have increased the fire hazard. Rubber gloves, face shield, chemical splash goggles

and appropriate attires (chemical resistant pants, jackets and shoes) should be worn when

handling with all types of chemical.

3.5.3 Health Concern MTBE enters the body through breathing and swallowing water contaminated with

MTBE. EPA has determined that MTBE has a potential to cause hazardous effects in humans.

Some people have complained of symptoms such as nausea, dizziness, and light-headedness,

headaches, and nose and throat irritation after breathing vapours from gas containing MTBE.

But it’s not clear if these symptoms are caused by MTBE or other components of gasoline

[81].

Although there is no scientific evidence to indicate MTBE is a human carcinogen or a

serious health threat, a number of laboratory studies of animals exposed to high doses of

MTBE have showed stomach irritation, liver and kidney damage, and nervous system effects.

Some of the studies also indicate an increase in liver and kidney cancer in rats and mice that

breathed high levels of MTBE or consumed high concentrations of the chemical [82].

Several national and international agencies study substances in the environment to

determine if they can cause cancer. These agencies include National Toxicology Program

(NTP), International Agency for Research on Cancer (IARC) and Environmental Protection

Agency (EPA). The EPA maintains the Integrated Risk Information System (IRIS), an

electronic database that contains information on human health effects from exposure to

53

various substances in the environment. EPA’s Office of Water has concluded that there isn’t

enough evidence to estimate potential health risks of MTBE at low exposure levels in

drinking water, but that the evidence supports the conclusion that MTBE is a potential human

carcinogen at high doses. Thus, excessive intake of MTBE should be avoided for the sake of

human health [82].

Similarly, Chronic inhalation or oral exposure to methanol may result in headache,

dizziness, giddiness, insomnia, nausea, gastric disturbances, conjunctivitis, visual

disturbances (blurred vision), and blindness in humans. The large quantity of methanol

ingestion can be toxic but this is not considered possible under normal process operation.

3.6 Projected Demands/Supply for Next 10 years As stated earlier, MTBE is widely used in gasoline as an octane booster and

oxygenate. It can also be used to make high purity isobutylene for butyl rubber and

polyisobutylene production. The product with high purity can also be used in pharmaceutical

intermediates production [83]. However, the main application of MTBE is still as a gasoline

additive; this end use accounts for about 92% of global product demand [84].

According to a report (Methyl Tertiary Butyl Ether (MTBE): 2015 World Market

Outlook and Forecast up to 2019) published by Merchant Research & Consulting Ltd on June

2015, they believe that the next few years consumption of MTBE in developed countries will

decrease, but developing ones will show stable growth. Undeniably, the consumption of

MTBE in Western countries have been decreasing for the last few decades. MTBE used to be

popular until it was found out to be dangerous to the environment. USA, Canada, Japan and

Western Europe countries have shifted to ETBE, ethanol and other alternatives.

However, MTBE is still produced in North America but all amounts are exported. At

the same time Asia Pacific region increases MTBE capacity. As stated previously, China is

the largest country that is dominating the global MTBE demand [85]. According to another

Market Outlook report on MTBE published by Research and Market, China's demand for

Methyl Tert-Butyl Ether (MTBE) has grown at a fast pace in the past decade. In the next

decade, both production and demand will continue to grow [86]. Also, a market research

report on Methyl Tert-Butyl Ether (MTBE) Markets in China published on August this year

has also claimed that both the production and demand of MTBE in China will continue to

grow in the next decade [87].

54

Besides, another report published by Grand View Research, Inc. last year also stated

that the methyl tertiary butyl ether (MTBE) market is expected to witness significant growth

over the next six years on account of its increasing consumption as a fuel additive in gasoline

engines. In addition, the demand for MTBE is expected to grow as it improves the octane

number of fuel, reduces harmful emissions and provides good anti-knocking properties to the

engine. One of the reason is due to the rising demand for gasoline and its additives in oil &

gas and marine sectors is expected to propel market growth over the forecast period [88].

Where there is demand, there will be supply which explained that there is always a

supply for every demand. Since the demand of MTBE is expected to be increased in the next

few years, more suppliers/manufacturers will tend to increase their production rate in order to

meet the market demand. Thus, to act as one of the supplier to cope with the increasing

demand of the MTBE, I think it is reasonable to establish one MTBE production plant in

Malaysia. As predicted by Argus Dewitt in their report on Fuels and Oxygenates Annual

2015, they are expecting that the supply of MTBE to the market will increase together with

the demand till 2020. The graph below shows the supply and demand of MTBE extracted

from Fuels and Oxygenates Annual 2015. The global supply and demand was increasing

rapidly since 2010.

Figure 23: History and projections of global MTBE supply and demand from 2010 to 2020

Similarly, the demand and supply of the MTBE in the next 4 years after 2020 is

expected to increase at the same rate as well. To the best of our knowledge, China will still

remain as a developing country by 2024. In 2015, China’s CDP is still a fraction of that in

advanced countries and its market reforms are incomplete. Also, 98.99 million people still

lived below the national poverty line of RMB 2,300 per year. With the second largest number

of poor in the world after India, poverty reduction remains a fundamental challenge [89]. We

55

could not say that China cannot transform into a developed country in the next 10 years, but

based on the current data, it is very hard or almost impossible for China to do so within this

short period. Hence, as long as China is still a developing country, the MTBE will have a

market. Figure below shows the forecast of global MTBE demand and supply from 2015-

2024 based on the increment in amount from the last few years.

Figure 24: Projections of global MTBE supply and demand from 2015 to 2024

56

Chapter 4 Process Synthesis Structure and Analysis

4.1 Input-Output Structure Figure below shows all input and output streams that are involved in the process of

production of MTBE.

The input streams are:

1. Isobutylene uses as raw material from fluid catalytic cracking (FCC) operation in

refinery which is also known as isobutylene in C4’s stream since it consists of others

inert isomers besides isobutylene.

2. Pure methanol from refinery uses as raw material for the production of MTBE

3. Water uses for liquid-liquid extraction to remove methanol from mixed C4 stream and

by-products.

The output streams are:

1. MTBE which is the desired product in this process

2. Mixed C4’s stream which is waste product in this process.

3. A trace amount of by-products which are TBA and Di-isobutylene in the

etherification process.

The recycled streams are:

1. Recycle stream of methanol from distillation tower

2. Recycle stream of water from distillation tower

57

Table 4: Block Diagram about above Description Text

Input Operation Output

Isobutylene

in C4’s

stream

Methanol

4.2 Feed and Product Specifications: 1. Methanol [90]

Table 5: Feed and Product Specification of Methanol

Test Method Specification

Appearance IMPCA 003-98 Clear & free of suspended

matter

Purity on dry basis, %wt. IMPCA 001-02 Min 99.85

Packed Bed Reactor (MTBE Reactor)

MTBE, TBA, Di-isobutylene,

Mixed C4 & Methanol

Distillation Column (MTBE Tower)

MTBE

TBA, Di-isobutylene,

Mixed C4 & Methanol

Liquid-liquid Extraction Column (Methanol Absorber)

Water Mixed C4 TBA Di-isobutylene

Distillation Column (Methanol Recovery Tower)

Methanol & Water

Recycled

water

Recycled methanol

58

Acetone content, mg/kg IMPCA 001-02 Max 30

Ethanol, mg/kg IMPCA 001-02 Max 50

Color Pt-Co ASTM D 1209 Max 5

Water, %wt. ASTM E 1064 Max 0.1

Initial boiling point, oC ASTM D 1078 Max range 1.0

oC including

64.6±0.1oC

Dry point, oC

Range, oC -

Specific gravity @20o/20

o

22020/20oC

ASTM D 4052 0.791-0.793

PTT at 15oC, minutes ASTM D 1363 Min 60

Chloride as Cl, mg/kg IMPCA 002-08 Max 0.5

Hydrocarbons ASTM D 1722 Pass test

Carbon sable substances ASTM E 346 Max 30

Acidity as acetic acid, mg/kg ASTM D 1613 Max 30

Total iron, mg/kg ASTM E 394 Max 0.1

Nonvolatile matter,

mg/1000ml

ASTM D 1353 Max 0.8

Odor ASTM D 1296 *

(*) Characteristic & Non-Residual Odor

2. Isobutylene [91]

Table 6: Feed and Product Specification of Isobutylene

Test Method Specification

Isobutylene, %wt. HOC 0573

Min 99.8

Butadiene, %wt., Max 0.01

59

Butene-1, %wt. Max 0.1

Butene-2, Total, %wt. Max 0.1

Isobutane, %wt. Max 0.2

n-Butane, %wt. Max 0.2

Propane, %wt. Max 0.05

Propylene, %wt. Max 0.05

t-Butyl Alcohol, ppm Max 50

Water, ppm HOC 0438 Max 50

Acetylene as vinyl acetylene,

ppm

D4424 Max 10

Carbonyls as acetaldehyde,

ppm

HOC 0429 Max 50

Sulfur, ppm HOC 0229 Max 1

3. MTBE [92]

Table 7: Feed and Product Specification of MTBE

Test Method Specification

MTBE, %wt. ASTM D 5441 Min. 92

Water, %wt. ASTM D 1744 Max. 0.2

TC4, %wt. ASTM D 5441 To be reported

Methanol, ppm Max. 100

TBA, %wt. Max. 2.0

TAME, %wt. To be reported

DIB, %wt. To be reported

C5 contents, %wt. Max. 5

60

4.3 Price of all Product, By-Product and Raw Materials 1. Raw Materials and Product

Table 8: Price of Raw Materials and Product

Material Availability Average Price

Raw

Material

Isobutylene

[93]

By-product of refinery Fluid Catalytic

Cracking Unit (FCCU)

Dehydrogenation of butanes

RM 2963/tonne

Methanol

[94] Produced from natural gas resources RM 1323/tonne

Product MTBE

[95] Reaction between isobutylene and

methanol RM 4663/tonne

2. By-product

Table 9: Price of By-product

Material Availability Average Price

By-

Product

Diisobutylene (DIB)

[96]

Dehydrating tertiary butyl

alcohol

Catalytic dehydrogenation

of isobutane

RM 463.99/kg

Dimethyl ether (DME)

[97]

Methanol dehydration

Gasification of coal or

biomass

Through natural gas

reforming

RM 4410/tonne

Tert-Butyl Alcohol

(TBA) [98] Side-product of Propylene

Oxide (PO) production RM 5040/tonne

Water [99] Purchased from Syarikat

Air Terengganu Sdn. Bhd. RM 1.15/m

3

61

4.4 Destination Codes and Component Classification

Table 10: Destination Codes and Component Classification

NO COMPONENTS COMPONENTS

CLASSIFICATION

DESTINATION DESTINATION

CODES

1 Methanol Raw material MTBE Reactor R-101

MTBE Tower T-101

Methanol Absorber T-102

Methanol Recovery

Tower

T-103

2 Isobutylene Raw material MTBE Reactor R-101

MTBE Tower T-101

Methanol Absorber T-102

3 Mert-Tert-Butyl-

Ether (MTBE)

Product MTBE Tower T-101

4 Tert-Butyl

Alcohol (TBA)

By-Product MTBE Tower T-101

5 Di-Isobutylene By-Product MTBE Tower T-101

6 Di-Methyl Ether By-Product MTBE Tower T-101

62

4.5 Utilities of the Process

In MTBE production plants, utilities such as electricity, water and steam are important

for them.

Electricity

Electricity is needed for the plant operation as most of the plant facilities need

electricity to function. This is because electric motor is the most common used motor as it is

more efficient and very reliable in a wide range of wattage. Electrical component such as

pumps, control system, mixer and compressors. There are many electrical generation plants

which is able to supply required amount of electricity for example Tenaga Nasional Berhad

(TNB).

Water

Water is used to cool down the reactor by heat exchanger. Water is used as cooling

medium in the production of MTBE plant due to its high heat capacity, low cost, low

viscosity, non-hazardous, available in abundance and it is renewable. Water also can be used

in the jacketed system since this plant involved exothermic reaction. This reaction required

jacketed system in the reactor to control the temperature release from the reactor. The water

from heat exchanger and jacketed system can be recycling back without need to be treated

caused it cause no harm. Sources of water that supply to the plant are from Kemaman Port

and Kertih Port. Kemaman Port is Malaysian Deepwater general purpose Industrial Port. This

port is deepest in the region and can handle vessels up to 150,000dwt. Kertih Port is a marine

port and is managed by Petronas subsidiary company. It is a dedicated port for liquid

petrochemical products.

Steam

Steam is used as heating medium in heat. Steam is used to heat up or supply energy to

the plant that required to increase the temperature of the steams like reboiler and heat

exchanger.

63

Chapter 5 Process Flow Diagram

5.1 Block flow diagram for MTBE synthesis from isobutylene and

methanol:

Figure 25: Block Diagram for the Production of MTBE

64

Figure 26: Block Diagram for the Production of MTBE with Temperature and Pressure

65

5.2 Process Flow Diagram

Figure 27: Process Flow Diagram (After modification)

66

5.3 Innovative Approach in Process Design

Figure 28: Block Diagram of Initial/ Existing MTBE Production Plant

67

Figure 28 shows the initial/existing plant design of the direct synthesis of MTBE from

isobutylene and methanol and the plant design after modification is made. The followings are

the modification that has been introduced into the plant.

1. In order to ensure the complete reaction between isobutylene and methanol, the

amount of methanol added into the reactor is always 10% more than the

stoichiometric factor.

2. A centrifugal mixing pump is installed before both of the reactants are feed into the

reactor to promote mixing so that the reactants mix well with each other when

contacting with catalyst.

3. The water released from the second distillation column (Methanol Recovery Tower)

is recycled to liquid-liquid extraction column (Methanol Absorber) instead of draining

it away. By recycling the water, the usage of water can be reduced greatly. Anyway,

only 50% of the water released from the methanol recovery tower is recycled back

into methanol absorber, and the other 50% is still from water source. This is to make

sure that the water which acts as solvent will remain effective while reducing the cost

of water tariff.

Chapter 6 Process Analysis Figure 27 above shows the updated Process Flow Diagram (PFD) of the MTBE

production plant designed by Group 10. The whole process is started off by pumping the raw

materials, which are methanol and C4s (mainly isobutylene) into the reactor, R-101. This

reactor, R-101 is a packed bed reactor, which is filled with solid catalyst named Amberlyst-

15 resin catalyst. Inside this reactor, etherification has occurred to produce MTBE and other

undesired products that include tertiary butyl alcohol (TBA) and di-isobutylene (DIB).

Besides, impurities present in C4 stream such as butane, butene, 1,3-butadiene and unreacted

isobutylene and methanol also present in the effluent of the reactor. The operating condition

for this packed bed reactor (MTBE reactor) is maintained at 75 oC and 1000 kPa. The first

feed to the reactor, C4s (mainly constituted of isobutylene), is obtained from fluid catalytic

cracking (FCC) operations in refineries as a by-product, while the methanol, which derived

from natural gas is the ordered from petrochemical refinery. Both of the feeds are channeled

into a pipe and passed through a pre-heater, E-101 to increase the temperature of the feed to

75 oC as the reaction is favorable to occur at 75

oC. Then, a centrifugal mixing pump pumps

the heated methanol and isobutylene into the MTBE reactor. This pump will also promote

further mixing of both raw materials and enhance the reaction later in the reactor.

68

As mentioned above, etherification reaction will occur in the reactor, R-101 packed

with Amberlyst-15 Polymeric catalyst. The formation of MTBE from methanol and

isobutylene is an exothermic reaction. So, heat will generate as this reaction occur. On the

other hands, at 75 oC, the selectivity of the formation of MTBE is as high as 96.5%. Heat

produced during etherification reaction will cause temperature increase. From the literature, if

the reactor temperature more than 100 oC, it will promote the formation of by-product which

is dimethyl ether (DME). In order to maintain the temperature in the reactor at 75 oC

throughout the whole process, the reactor is jacketed so that a coolant can withdraw the heat

energy generated by this exothermic reaction. The flow rate of coolant in the cooling jacket is

controlled so that the desired temperature in reactor can be maintained.

Next, the outlet of the reactor is then fed into a distillation column, T-101 (MTBE

tower) where MTBE is collected as bottom product together with trace amount of by-

products. The operating pressure of this distillation column is maintained 750 kPa. A reboiler

is installed at the bottom of the distillation column to increase the purity of the MTBE

collected. Meanwhile, other undesired products are collected as distillate. A condenser is

installed at exit of distillate to enable reflux to occur.

The upper product from MTBE tower is then sent to a water scrubbber, T-102

(Methanol Absorber) to extract the unreacted methanol. Water is added into column to extract

methanol out from the C4 mixture. Methanol will dissolve in water to form water-methanol

mixture as the solubility of methanol in water is very high. This water-methanol mixture is

collected from the bottom of the absorber and send as feed into a second distillation column,

T-103. The top product of the absorber, mainly consist of other C4’s, is then combusted in a

furnace as they are all hydrocarbon. The pressure in the absorber is maintained at 100 kPa.

The second distillation column, T-103 (methanol recovery tower) is a unit operation that

used to separate the methanol and water so that they can be recycled to the feed of reactor R-

101 and the water is partially recycled back into the water scrubber, T-102 respectively. 50%

of the water collected from the methanol recovery tower is drained, and the other half is

mixed with fresh feed water to extract methanol again in water scrubber. The distillation

process is carried out at 100 kPa.

69

6.1 Justification of Equipment Table 11: Justification of Equipment

Code

Equipment

Material of

Construction

Operating Conditions

Purpose/Usage

Continuous/

Batch

No.

of

units

Orientation

Phase

Involve Temperature

(oC)

Pressure

(kPa)

Phase

Change

R-101 MTBE

Reactor Stainless Steel 90

oC

1100

kPa

No phase

change

To allow

etherification to

occur in the presence

of catalyst that

convert isobutylene

and methanol to

MTBE

Continuous 1 Vertical Liquid

T-101 MTBE

Tower Carbon Steel 90

oC

500

kPa

Stream 6 to

7: phase

change from

liquid to

vapour.

Stream 6 to

10: Remain

as liquid

To separate the

desired product

which MTBE form

undesired product

Continuous 1 Vertical Liquid-

Vapour

70

T-102 Methanol

Absorber Stainless Steel 140

oC

100

kPa

No phase

changes

To absorb unreacted

methanol and recycle

it back to the feed

Continuous 1 Vertical Liquid-

Vapour

T-103

Methanol

Recovery

Tower

Carbon Steel 77oC

100

kPa

Stream 16 to

17: phase

change from

liquid to

vapour.

Stream 16 to

22: Remain

as liquid

To separate methanol

and water in order to

recycle methanol to

the feed

Continuous 1 Vertical Liquid-

Vapour

E-101 Feed

Heater Stainless Steel 28

oC

1050

kPa

No phase

changes

To supply heat to the

reactant before

entering the reactor

Continuous 1 Horizontal Liquid

E-102 Condenser Stainless Steel 70 oC

750

kPa

From vapour

to liquid

To remove heat from

vapor, for reflux

purpose

Continuous 1 Horizontal Liquid-

Vapour

E-103 Reboiler Stainless Steel 130oC

750

kPa

From liquid

to vapour

To supply heat to the

process fluid Continuous 1 Horizontal

Liquid-

Vapour

E-104 Heater Stainless Steel 110oC

700

kPa

From liquid

to vapour

To supply heat to the

process fluid Continuous 1 Horizontal Vapour

71

E-105 Condenser Stainless Steel 70oC

100

kPa

From vapour

to liquid

To remove heat from

vapor, for reflux

purpose

Continuous 1 Horizontal Liquid-

Vapour

E-106 Reboiler Stainless Steel 100oC

100

kPa

From liquid

to gas

To supply heat to the

process fluid Continuous 1 Horizontal

Liquid-

Vapour

P-101 Feed Pump

Stainless Steel

+ Chromium

(content > 12)

25 815

kPa

No phase

changes

To mix isobutylene

and methanol before

entering the reactor

and also to lift the

operating pressure to

desired pressure.

Continuous

1

Vertical

Liquid

P-102 Reflux

Pump

Cast Steel/

Iron/ Copper

alloy

60oC

550

kPa

No phase

changes

To recycle liquid to

increase the purity of

overhead product

Continuous

1

Vertical

Liquid

P-103 Reflux

Pump

Cast Steel/

Iron/ Copper

alloy

65oC

100

kPa

No phase

changes

To recycle liquid to

increase the purity of

overhead product

Continuous 1 Vertical Liquid

P-104 Distillate

Pump

Cast Steel/

Iron/ Copper

alloy

65oC

100

kPa

No phase

changes

To recycle back

methanol to feed

section

Continuous 1 Vertical Liquid

P-105 Bottom

Pump

Cast Steel/

Iron/ Copper

alloy

100oC

100

kPa

No phase

changes

To recycle back

water to methanol

scrubber

Continuous 1 Vertical Liquid

72

6.2 Separation Operations Used in Production of MTBE

There are only 3 unit operations that are installed to perform separation processes, which

are MTBE distillation tower, methanol absorber and methanol recovery tower. Two out of these

three unit operations are distillation column and the third one is a scrubber. The purpose of the

installation of all these separation units is to help in yielding high quality of MTBE and reduce the

cost of raw material in long term of time.

MTBE Distillation Tower

This is the first separation unit in this plant. It is a distillation column that is installed after a

reactor where etherification process occurs. The product stream from the MTBE reactor that

contains the desired product, side products and unreacted reactants is fed into this distillation

column. MTBE will be collected at the bottom as the product of the plant, while the unreacted

C4’s and side products formed are collected as distillate. A condenser and a reboiler are installed

at the top and bottom outlet of the distillation column, respectively.

Methanol Absorber

Next, since methanol is always in excess, the distillate collected from the MTBE distillation tower

must contain high amount of methanol. In order to reuse back the unreacted methanol, the

simplest way is by using a scrubber. All the distillate collected is first heated until they turn into

vapour phase, and then is feed into the bottom of the second separation unit which is known as

methanol absorber. Meanwhile, water at room temperature is splashed from the top of the

absorber. Water and methanol mixture is collected at the bottom of the scrubber and the

undissolved butane waste gas is discharged from top of the unit. Methanol which has the OH

group in its structure is able to dissolve in water and other alkanes (C4’s) are insoluble. Hence,

methanol can be extracted by using this scrubber.

Methanol Recovery Tower

The last separation unit is also a distillation column, which is also known as methanol recovery

tower. As the name stated, this separation unit is used to recover the methanol. The water and methanol

mixture from the previous separation unit, methanol absorber is channelled into the distillation column.

Water which has higher boiling point is collected as bottom product; methanol is vaporised, flow out from

the top of the column and later is condensed by a condenser at the top outlet. Both water and methanol are

recycled back to use in the production plant to reduce the cost of methanol and water.

73

Table 12: Separation Operation Used in Methyl Tert-Butyl Ether (MTBE) MTBE Production

Separation

Equipment

Code of

Equipment

Phase

Involved

Operating

Condition Function

MTBE

Distillation

Tower

(Distillation

Column)

T-101

Liquid-

Vapour

Temperature:

50oC - 90

oC

Pressure:

1100 kPa

To separate the MTBE with

undesired side-product and

unreacted reactants.

MTBE which has the highest

boiling point will be collected as

the bottom.

Other side product and unreacted

reactants are collected as the

distillate of this distillation

column.

Methanol

Absorber T-102

Liquid-

Vapour

Temperature:

30oC - 120

oC

Pressure:

750 kPa

To enable methanol recovery.

The entering feed will be a

mixture of waste butene and

methanol in vapour phase.

Unreacted methanol which has

high solubility towards water will

be separated from waste butene

so that methanol can be recycled.

Methanol

Recovery

Tower

(Distillation

Column)

T-103 Liquid-

Vapour

Temperature:

25oC - 100

oC

Pressure:

100 kPa

To separate methanol from water

Methanol with lower boiling

point will be collected as

distillate and then recyled back as

the feedstock for etherification

process.

Water which has higher boiling

point will go to the bottom and

mixed with water inlet to use in

Methanol Absorber.

74

Chapter 7: Mass Balance and Energy Balance of the Process Plant

7.1 Mixing Point

Inlet Outlet

Stream 1 2 21 3

Temperature (℃) 25 25 60 28.00

Pressure (kPa) 2000 100 150 815

Vapour Fraction 0 0 0 0

Component

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 26040.00 1.00 465.00 1.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 26040.00 0.60 465.00 0.47

Methanol 0.00 0.00 0.00 0.00 13541.92 1.00 423.18 1.00 2826.08 0.82 88.32 0.82 16368.00 0.38 511.50 0.51

MTBE 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 329.93 0.10 3.75 0.03 329.93 0.01 3.75 0.00

Water 0.00 0.00 0.00 0.00 27.14 0.00 1.51 0.00 273.49 0.08 15.19 0.14 300.62 0.01 16.70 0.02

Butene 26.09 0.00 0.47 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 13.05 0.00 0.24 0.00

Butane 13.05 0.00 0.22 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 13.05 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 26092.18 1.00 465.93 1.00 13569.06 1.00 424.69 1.00 3429.50 1.00 107.26 1.00 43090.74 1.00 997.88 1.00

Mass Balance (kg/hr) 43090.74 43090.74

Accumulation 0

Energy Flow (MJ/hr) -17541.88821 -101614.4722 -26561.40551 -145719.526

Heat Duty (MJ/hr) 0

Power requirement (kW) -

75

7.2 Feed Pump (P-101)

Inlet Outlet

Stream 3 4

Temperature (℃) 28 28

Pressure (kPa) 815 1050

Vapour Frection 0 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 26040.00 0.60 465.00 0.47 26040.00 0.60 465.00 0.47

Methanol 16368.00 0.38 511.50 0.51 16368.00 0.38 511.50 0.51

MTBE 329.93 0.01 3.75 0.00 329.93 0.01 3.75 0.00

Water 300.62 0.01 16.70 0.02 300.62 0.01 16.70 0.02

Butene 26.09 0.00 0.47 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 13.05 0.00 0.24 0.00

Butane 13.05 0.00 0.22 0.00 13.05 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 43090.74 1.00 997.88 1.00 43090.74 1.00 997.88 1.00

Mass Balance (kg/hr) 43090.74 43090.74

Accumulation 0

Energy Flow (MJ/hr) -145719.53 -145719.53

Heat Duty (MJ/hr) -

Power requirement (kW) 17.25

7.3Heat Exchanger (E-101) Inlet Outlet

Stream 4 5

Temperature (℃) 28 90

Pressure (kPa) 1050 1000

Vapour Frection 0 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 26040.00 0.60 465.00 0.47 26040.00 0.60 465.00 0.47

Methanol 16368.00 0.38 511.50 0.51 16368.00 0.38 511.50 0.51

MTBE 329.93 0.01 3.75 0.00 329.93 0.01 3.75 0.00

Water 300.62 0.01 16.70 0.02 300.62 0.01 16.70 0.02

Butene 26.09 0.00 0.47 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 13.05 0.00 0.24 0.00

Butane 13.05 0.00 0.22 0.00 13.05 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 43090.74 1.00 997.88 1.00 43090.74 1.00 997.88 1.00

Mass Balance (kg/hr) 43090.74 43090.74

Accumulation 0

Energy Flow (MJ/hr) -145719.526 -144099.8761

Heat Duty (MJ/hr) 1619.649932

Power requirement (kW) -

76

7.4 MTBE Reactor (R-101)

Inlet Outlet

Stream 5 6

Temperature (℃) 90 90

Pressure (kPa) 1000 550

Vapour Frection 0 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 26040.00 0.60 465.00 0.47 1833.09 0.04 32.73 0.06

Methanol 16368.00 0.38 511.50 0.51 3157.54 0.07 98.67 0.17

MTBE 329.93 0.01 3.75 0.00 36658.70 0.85 416.58 0.73

Water 300.62 0.01 16.70 0.02 0.00 0.00 0.00 0.00

Butene 26.09 0.00 0.47 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 13.05 0.00 0.24 0.00

Butane 13.05 0.00 0.22 0.00 13.05 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 1235.90 0.03 16.70 0.03

Diisobutylene 0.00 0.00 0.00 0.00 153.32 0.00 1.37 0.00

Total 43090.74 1.00 997.88 1.00 43090.74 1.00 566.99 1.00

Mass Balance (kg/hr) 43090.74 43090.74

Accumulation 0

Total Energy Flow (MJ/hr) -144099.8761 -325030.6773

Heat Duty (MJ/hr) -180930.8012

Power requirement (kW) -

77

7.5 MTBE Tower (T-101)

Inlet

Stream 6 9 11

Temperature (℃) 90 60 130

Pressure (kPa) 550 500 500

Vapour Frection 0 0 1

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass Fraction

Mole

Flow Rate

(kmol/hr)

Mole Fraction

Isobutylene 1833.09 0.04 32.73 0.06 7332.37 0.34 130.94 0.24 0.00 0.00 0.00 0.00

Methanol 3157.54 0.07 98.67 0.17 12630.14 0.58 394.69 0.72 0.00 0.00 0.00 0.00

MTBE 36658.70 0.85 416.58 0.73 1466.35 0.07 16.66 0.03 36013.36 0.96 409.24 0.96

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 26.09 0.00 0.47 0.00 104.37 0.00 1.86 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 52.18 0.00 0.97 0.00 0.00 0.00 0.00 0.00

Butane 13.05 0.00 0.22 0.00 51.66 0.00 0.89 0.00 0.13 0.00 0.00 0.00

TBA 1235.90 0.03 16.70 0.03 0.00 0.00 0.00 0.00 1226.40 0.03 16.57 0.04

Diisobutylene 153.32 0.00 1.37 0.00 0.00 0.00 0.00 0.00 152.15 0.00 1.36 0.00

Total 43090.74 1.00 566.99 1.00 21637.07 1.00 546.01 1.00 37392.04 1.00 427.18 1.00

Mass Balance (kg/hr) 102119.85

Accumulation 0

Total Energy Flow (MJ/hr) -688628.321

Heat Duty (MJ/hr) 2660.613274

Power requirement (kW) -

78

Outlet

Stream 7 10

Temperature (℃) 70 130

Pressure (kPa) 550 530

Vapour Frection 1 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole

Flow Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 9165.46 0.34 163.67 0.24 0.00 0.00 0.00 0.00

Methanol 15787.68 0.58 493.37 0.72 0.00 0.00 0.00 0.00

MTBE 1832.94 0.07 20.83 0.03 72305.47 0.96 821.65 0.96

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 26.09 0.00 2.33 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 65.23 0.00 1.21 0.00 0.00 0.00 0.00 0.00

Butane 64.58 0.00 1.11 0.00 0.26 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 2462.30 0.03 33.27 0.04

Diisobutylene 0.00 0.00 0.00 0.00 305.47 0.00 2.73 0.00

Total 27046.34 1.00 682.51 1.00 75073.50 1.00 857.66 1.00

Mass Balance (kg/hr) 102119.85

Accumulation 0

Total Energy Flow (MJ/hr) -685967.7077

Heat Duty (MJ/hr) 2660.613274

Power requirement (kW) -

7.6 Condenser (E-102)

Inlet Outlet

Stream 7 8

Temperature (℃) 70 60

Pressure (kPa) 550 470

Vapour Frection 1 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 9165.46 0.34 163.67 0.24 9165.46 0.34 163.67 0.24

Methanol 15787.68 0.58 493.37 0.72 15787.68 0.58 493.37 0.72

MTBE 1832.94 0.07 20.83 0.03 1832.94 0.07 20.83 0.03

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 130.46 0.00 2.33 0.00 130.46 0.00 2.33 0.00

1,3-butadienes 65.23 0.00 1.21 0.00 65.23 0.00 1.21 0.00

Butane 64.58 0.00 1.11 0.00 64.58 0.00 1.11 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 27046.34 1.00 682.51 1.00 27046.34 1.00 682.51 1.00

Mass Balance (kg/hr) 27046.34 27046.34

Accumulation 0

Total Energy Flow (MJ/hr) -105463.5417 -143058.9341

Heat Duty (MJ/hr) -37595.39242

Power requirement (kW) -

79

7.7 Reflux Pump (P-102)

Inlet Outlet

Stream 8 9 13

Temperature (℃) 60 60 140.00

Pressure (kPa) 470 500 100

Vapour Fraction 0 0 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 9165.46 0.34 163.67 0.24 7332.37 0.34 130.94 0.24 1833.09 0.34 32.73 0.24

Methanol 15787.68 0.58 493.37 0.72 12630.14 0.58 394.69 0.72 3157.54 0.58 98.67 0.72

MTBE 1832.94 0.07 20.83 0.03 1466.35 0.07 16.66 0.03 366.59 0.07 4.17 0.03

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 130.46 0.00 2.33 0.00 104.37 0.00 1.86 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 65.23 0.00 1.21 0.00 52.18 0.00 0.97 0.00 13.05 0.00 0.24 0.00

Butane 64.58 0.00 1.11 0.00 51.66 0.00 0.89 0.00 12.92 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 27046.34 1.00 682.51 1.00 21637.07 1.00 546.01 1.00 5409.27 1.00 136.50 1.00

Mass Balance (kg/hr) 27046.34 27046.34

Accumulation 0.00

Total Energy Flow (MJ/hr) -143058.9341 -143058.9341

Heat Duty (MJ/hr) 0

Power requirement (kW) -

80

INLET OUTLET

Stream 9a 9

Temperature (°C) 62.08 62.08

Pressure (kPa) 750 770

Component

Mass

flow rate Mass

fraction

Density Density

Fraction

Mass flow

rate Mass

fraction

Density Density

Fraction

(kg/hr) (kg/m3) (kg/m3) (kg/hr) (kg/m3) (kg/m3)

Isobutylene 7332.37 0.34 587.90 199.23 7332.37 0.34 587.90 199.23

Methanol 12630.14 0.58 790.00 461.14 12630.14 0.58 790.00 461.14

MTBE 1466.35 0.07 740.50 50.18 1466.35 0.07 740.50 50.18

Water 0.00 0.00 1000.00 0.00 0.00 0.00 1000.00 0.00

Butene 104.37 0.00 770.00 3.71 104.37 0.00 770.00 3.71

1,3-butadiene 52.18 0.00 621.00 1.50 52.18 0.00 621.00 1.50

Butane 51.66 0.00 789.00 1.88 51.66 0.00 789.00 1.88

TBA 0.00 0.00 720.00 0.00 0.00 0.00 720.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Subtotal 21637.07 1.00 6018.40 717.65 21637.07 1.00 6018.40 717.65

Volumetric Flow Rate (m3/h) 30.15 30.15

Total Energy Flow (MJ/hr) -114447.15 -114447.15

Heat Duty (MJ/hr) 0

Power requirement (kW) 0.20

7.8 Heater (E-104)

Inlet Outlet

Stream 13 14

Temperature (℃) 60 60

Pressure (kPa) 550 550

Vapour Frection 0 1

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 1833.09 0.34 32.73 0.24 1833.09 0.34 32.73 0.24

Methanol 3157.54 0.58 98.67 0.72 3157.54 0.58 98.67 0.72

MTBE 366.59 0.07 4.17 0.03 366.59 0.07 4.17 0.03

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 26.09 0.00 0.47 0.00 26.09 0.00 0.47 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 13.05 0.00 0.24 0.00

Butane 12.92 0.00 0.22 0.00 12.92 0.00 0.22 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 5409.27 1.00 136.50 1.00 5409.27 1.00 136.50 1.00

Mass Balance (kg/hr) 5409.27 5409.27

Accumulation 0

Total Energy Flow (MJ/hr) -28611.78683 -20764.75679

Heat Duty (MJ/hr) 7847.030039

Power requirement (kW) -

81

7.9 Bottom Reboiler (E-103)

Inlet Outlet

Stream 10 11 12

Temperature (℃) 130 130 130.00

Pressure (kPa) 530 500 500

Vapour Fraction 0 1 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

MTBE 72305.47 0.96 821.65 0.96 36013.36 0.96 409.24 0.96 36292.12 0.96 412.41 0.96

Water 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.26 0.00 0.00 0.00 0.13 0.00 0.00 0.00 0.13 0.00 0.00 0.00

TBA 2462.30 0.03 33.27 0.04 1226.40 0.03 16.57 0.04 1235.90 0.03 16.70 0.04

Diisobutylene 305.47 0.00 2.73 0.00 152.15 0.00 1.36 0.00 153.32 0.00 1.37 0.00

Total 75073.50 1.00 857.66 1.00 37392.04 1.00 427.18 1.00 37681.47 1.00 430.48 1.00

Mass Balance (kg/hr) 75073.50 75073.50

Accumulation 0.00

Total Energy Flow (MJ/hr) -580504.166 -539541.5926

Heat Duty (MJ/hr) 40962.57336

Power requirement (kW) -

82

7.10 Methanol Absorber Column (T-102)

Inlet

Stream 14 28

Temperature (℃) 140 62

Pressure (kPa) 100 100

Vapour Fraction 1 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 1833.09 0.34 32.73 0.24 0.00 0.00 0.00 0.00

Methanol 3157.54 0.58 98.67 0.72 14.27 0.00 0.45 0.00

MTBE 366.59 0.07 4.17 0.03 0.00 0.00 0.00 0.00

Water 0.00 0.00 0.00 0.00 27624.79 1.00 1534.71 1.00

Butene 26.09 0.00 0.47 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 13.05 0.00 0.24 0.00 0.00 0.00 0.00 0.00

Butane 12.92 0.00 0.22 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 5409.27 1.00 136.50 1.00 27639.06 1.00 1535.16 1.00

Mass Balance (kg/hr) 33048.33

Accumulation 0.00

Total Energy Flow (MJ/hr) -455315.787

Heat Duty (MJ/hr) -268.6952467

Power requirement (kW) -

Outlet

Stream 15 16

Temperature (℃) 105 77.00

Pressure (kPa) 100 100

Vapour Fraction 1 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 1833.09 0.73 32.73 0.55 0.00 0.00 0.00 0.00

Methanol 317.18 0.13 9.91 0.17 2854.63 0.09 89.21 0.06

MTBE 36.66 0.01 0.42 0.01 329.93 0.01 3.75 0.00

Water 276.25 0.11 15.35 0.26 27348.54 0.90 1519.36 0.94

Butene 26.09 0.01 0.47 0.01 0.00 0.00 0.00 0.00

1,3-butadienes 13.05 0.01 0.24 0.00 0.00 0.00 0.00 0.00

Butane 12.92 0.01 0.22 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 2515.23 1.00 59.34 1.00 30533.10 1.00 1612.32 1.00

Mass Balance (kg/hr) 33048.33

Accumulation 33048.33

Total Energy Flow (MJ/hr) -455584.4823

Heat Duty (MJ/hr) -267.6952467

Power requirement (kW) -

83

7.11 Methanol Recovery Tower (T-103) Mass Balance Inlet

Stream 16 19 23

Temperature (℃) 77 65 100

Pressure (kPa) 100 100 100

Vapour Frection 0 0 1

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass Fraction

Mole

Flow Rate

(kmol/hr)

Mole Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 2854.63 0.09 89.21 0.06 16956.49 0.82 529.89 0.82 1.73 0.00 0.05 0.00

MTBE 329.93 0.01 3.75 0.00 1979.57 0.10 22.50 0.03 0.00 0.00 0.00 0.00

Water 27348.54 0.90 1519.36 0.94 1640.91 0.08 91.16 0.14 1638.41 1.00 91.02 1.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 30533.10 1.00 1612.32 1.00 20576.97 1.00 643.55 1.00 1640.14 1.00 91.08 1.00

Mass Balance (kg/hr) 52750.21

Accumulation 0.00

Total Energy Flow (MJ/hr) -630746.07

Heat Duty (MJ/hr) 26533.02

Power requirement (kW) -

84

Energy Balance Outlet

Stream 17 22

Temperature (℃) 70 100

Pressure (kPa) 100 100

Vapour Frection 1 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 19782.57 0.82 618.21 0.82 30.27 0.00 0.95 0.00

MTBE 2309.50 0.10 26.24 0.03 0.00 0.00 0.00 0.00

water 1914.40 0.08 106.36 0.14 28713.46 1.00 1595.19 1.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 24006.47 1.00 750.81 1.00 28743.74 1.00 1596.14 1.00

Mass Balance (kg/hr) 52750.21

Accumulation 0.00

Total Energy Flow (MJ/hr) -604213.05

Heat Duty (MJ/hr) 26534.02

Power requirement (kW) -

7.12 Distillate Condenser (E-105)

Inlet Outlet

Stream 17 18

Temperature (℃) 70 65

Pressure (kPa) 100 100

Vapour Frection 1 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 19782.57 0.82 618.21 0.82 19782.57 0.82 618.21 0.82

MTBE 2309.50 0.10 26.24 0.03 2309.50 0.10 26.24 0.03

Water 1914.40 0.08 106.36 0.14 1914.40 0.08 106.36 0.14

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 24006.47 1.00 750.81 1.00 24006.47 1.00 750.81 1.00

Mass Balance (kg/hr) 24006.47 24006.47

Accumulation 0.00

Total Energy Flow (MJ/hr) -155839.91 -185929.8385

Heat Duty (MJ/hr) -30089.92853

Power requirement (kW) -

85

7.13 Reflux Pump (P-103) Mass Balance Inlet Outlet

Stream 18 19 20

Temperature (℃) 65 65 65.00

Pressure (kPa) 100 100 100

Vapour Fraction 0 0 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate (kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 19782.57 0.82 618.21 0.82 16956.49 0.82 529.89 0.82 2826.08 0.82 88.32 0.82

MTBE 2309.50 0.10 26.24 0.03 1979.57 0.10 22.50 0.03 329.93 0.10 3.75 0.03

water 1914.40 0.08 106.36 0.14 1640.91 0.08 91.16 0.14 273.49 0.08 15.19 0.14

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 24006.47 1.00 750.81 1.00 20576.97 1.00 643.55 1.00 3429.50 1.00 107.26 1.00

Mass Balance (kg/hr) 24006.47 24006.47

Accumulation 0.00

Total Energy Flow (MJ/hr) -185929.8385 -185929.8385

Heat Duty (MJ/hr) -

Power requirement (kW) -

86

Energy Balance IN OUT

Stream 19a 19

Temperature (°C) 32.88 32.88

Pressure (kPa) 100 120

Component

Mass flow

rate Mass

fraction

Density Density

Fraction

Mass flow

rate Mass

fraction

Density Density

Fraction

(kg/hr) (kg/m3) (kg/m3) (kg/hr) (kg/m3) (kg/m3)

Isobutylene 0.00 0.00 587.90 0.00 0.00 0.00 587.90 0.00

Methanol 16956.49 0.78 790.00 619.11 16956.49 0.78 790.00 619.11

MTBE 1979.57 0.09 740.50 67.75 1979.57 0.09 740.50 67.75

Water 1640.91 0.08 1000.00 75.84 1640.91 0.08 1000.00 75.84

Butene 0.00 0.00 770.00 0.00 0.00 0.00 770.00 0.00

1,3-butadiene 0.00 0.00 621.00 0.00 0.00 0.00 621.00 0.00

Butane 0.00 0.00 789.00 0.00 0.00 0.00 789.00 0.00

TBA 0.00 0.00 720.00 0.00 0.00 0.00 720.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Subtotal 20576.97 0.95 6018.40 762.69 20576.97 0.95 6018.40 762.69

Volumetric Flow Rate (m3/h) 26.98 26.98

Total Energy Flow (MJ/hr) -159368.43 -159368.43

Heat Duty (MJ/hr) 0

Power requirement (kW) 0.18

7.14 Methanol Recycle Pump

Inlet Outlet

Stream 19 20

Temperature (℃) 65 60

Pressure (kPa) 100 150

Vapour Frection 0 0

Component

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 2826.08 0.82 88.32 0.82 2826.08 0.82 88.32 0.82

MTBE 329.93 0.10 3.75 0.03 329.93 0.10 3.75 0.03

Water 273.49 0.08 15.19 0.14 273.49 0.08 15.19 0.14

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 3429.50 1.00 107.26 1.00 3429.50 1.00 107.26 1.00

Mass Balance (kg/hr) 3429.50 3429.50

Accumulation 0

Total Energy Flow (MJ/hr) -26561.40551 -26561.40551

Heat Duty (MJ/hr) 0

Power requirement (kW) 0.440840177

87

7.15 Bottom Reboiler (E-106)

Inlet Outlet

Stream 22 23 24

Temperature (℃) 100 100 100.00

Pressure (kPa) 100 100 100

Vapour Fraction 0 1 0

Component

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 30.27 0.00 0.95 0.00 1.73 0.00 0.05 0.00 28.55 0.00 0.89 0.00

MTBE 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

water 28713.46 1.00 1595.19 1.00 1638.41 1.00 91.02 1.00 27075.05 1.00 1504.17 1.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 28743.74 1.00 1596.14 1.00 1640.14 1.00 91.08 1.00 27103.60 1.00 1505.06 1.00

Mass Balance (kg/hr) 28743.74 28743.74

Accumulation 0.00

Total Energy Flow (MJ/hr) -448373.141 -443713.4531

Heat Duty (MJ/hr) 4659.687904

Power requirement (kW) -

88

7.16 Water Recycle Pump (P-105) Mass Balance Inlet Outlet

Stream 24 25 26

Temperature (℃) 100 100 100.00

Pressure (kPa) 100 100 100

Vapour Fraction 0 0 0

Component

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow Rate

(kmol/hr)

Mole

Fraction

Mass

Flow

Rate

(kg/hr)

Mass

Fraction

Mole

Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 28.55 0.00 0.89 0.00 14.27 0.00 0.45 0.00 14.27 0.00 0.45 0.00

MTBE 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

water 27075.05 1.00 1504.17 1.00 13537.53 1.00 752.08 1.00 13537.53 1.00 752.08 1.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 27103.60 1.00 1505.06 1.00 13551.80 1.00 752.53 1.00 13551.80 1.00 752.53 1.00

Mass Balance (kg/hr) 27103.60 27103.60

Accumulation 0.00

Total Energy Flow (MJ/hr) -421692.1737 -421692.1737

Heat Duty (MJ/hr) 0

Power requirement (kW) -

89

Energy Balance IN OUT

Stream 24 24a

Temperature (°C) 99.60 99.60

Pressure (kPa) 100 120

Component

Mass

flow rate Mass

fraction

Density Density

Fraction

Mass

flow rate Mass

fraction

Density Density

Fraction

(kg/hr) (kg/m3) (kg/m

3) (kg/hr) (kg/m

3) (kg/m

3)

Isobutylene 0.00 0.00 587.90 0.00 0.00 0.00 587.90 0.00

Methanol 28.55 0.00 790.00 1.04 14.27 0.00 790.00 0.52

MTBE 0.00 0.00 740.50 0.00 0.00 0.00 740.50 0.00

Water 27075.05 1.25 1000.00 1251.33 13537.53 0.63 1000.00 625.66

Butene 0.00 0.00 770.00 0.00 0.00 0.00 770.00 0.00

1,3-butadiene 0.00 0.00 621.00 0.00 0.00 0.00 621.00 0.00

Butane 0.00 0.00 789.00 0.00 0.00 0.00 789.00 0.00

TBA 0.00 0.00 720.00 0.00 0.00 0.00 720.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Subtotal 27103.60 1.25 6018.40 1252.37 13551.80 0.63 6018.40 626.18

Volumetric Flow Rate

(m3/h)

21.64 21.64

Total Energy Flow (MJ/hr) -421692.17 -421692.17

Heat Duty (MJ/hr) 0.00

Power requirement (kW) 0.14

90

7.17 Water Mixing Point

Inlet Outlet

Stream 26 27 28

Temperature (℃) 100 25 62.00

Pressure (kPa) 100 100 100

Vapour Fraction 0 0 0

Component

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass

Flow Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Mass Flow

Rate

(kg/hr)

Mass

Fraction

Mole Flow

Rate

(kmol/hr)

Mole

Fraction

Isobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 14.27 0.00 0.45 0.00 0.00 0.00 0.00 0.00 14.27 0.00 0.45 0.00

MTBE 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

water 13537.53 1.00 752.08 1.00 14087.26 1.00 782.63 1.00 27624.79 1.00 1534.71 1.00

Butene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

1,3-butadienes 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Butane 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

TBA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Diisobutylene 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

Total 13551.80 1.00 752.53 1.00 14087.26 1.00 782.63 1.00 27639.06 1.00 1535.16 1.00

Mass Balance (kg/hr) 27639.06 27639.06

Accumulation 0.00

Total Energy Flow (MJ/hr) -434551.7756 -434551.0302

Heat Duty (MJ/hr) 0.74542565

Power requirement (kW) -

91

7.18 Comparison Aspen and Excel Calculation Aspen Flowsheet

Figure 29: Aspen Flowsheet

92

Stream Table from Aspen

Table 13: Stream Table from Aspen

93

Table 14: Mass Balance Comparison

STREAM Mass Flow rate (kg/hr)

JUSTIFICATION EXCEL ASPEN PLUS

C4's Feed Stream

(Stream 1) 26092.18 26142.28

The difference between two data (Spreadsheet and Aspen) are insignificant can be

considered as no error. The insignificant different may cause by the different source of

molecular weight taken for the calculation of mass flowrate in Excel Spreadsheet and

Aspen Plus.

Methanol Feed

Stream

(Stream 2)

13569.06 13586.91

The difference between two data (Spreadsheet and Aspen) are insignificant can be

considered as no error. The insignificant different may cause by the different source of

molecular weight taken for the calculation of mass flowrate in Excel Spreadsheet and

Aspen Plus.

Methanol Recycle

Stream (Stream 21) 3350.15 1156.50 Carry on effect of stream 16 and also the composition of distillate and bottom product

is different from the composition used in Aspen Plus

Stream 3 43011.39 40885.69 There is slight discrepancy between the mass flow rate from Aspen Plus and Excel

calculation because it is affected by the mass flowrate of recycled stream 21

Stream 4 43011.39 40885.69 Carry on the effect of stream 3

Stream 5 43011.39 40885.69 Carry on the effect of stream 3

94

Stream 6 43011.39 40885.69 There is slight discrepancy between the mass flow rate from Aspen Plus and Excel

calculation because it is affected by the mass flowrate of recycled stream 21.

MTBE Product

Stream

(Stream 12)

37355.26 37510.12

There is slight discrepancy between the mass flow rate from Aspen Plus and Excel

calculation because the composition of distillate and bottom product is different from

the composition used in Aspen Plus

Stream 13 5656.13 3375.57

There is significant deviation of the mass flow rate in Excel calculation from Aspen

Plus because the composition of distillate and bottom product is different from the

composition used in Aspen Plus

Stream 14 5656.13 3375.57 Carry on effect of stream 13

Flare Gas Stream

(Stream 15) 2681.95 2631.47 Carry on effect of stream 14

Stream 16 22598.23 20331.84 Carry on effect of recycle stream 21

Water Recycle

Stream

(Stream 28)

19624.04 19587.67

Stream 28 is basically the fresh water stream (stream 27) mix with waste water stream

(stream 25). There is slight discrepancy between the mass flow rate from Aspen Plus

and Excel calculation because it carries on the effect of stream 25 which caused by the

difference composition of distillate and bottom product of Aspen Plus and Excel

calculation

95

Stream 20 3350.15 1156.50 Carry on effect of stream 16 and also the composition of distillate and bottom product

is different from the composition used in Aspen Plus

Stream 24 19248.08 19175.34

There is slight discrepancy between the mass flow rate from Aspen Plus and Excel

calculation because the composition of distillate and bottom product is different from

the composition used in Aspen Plus

Waste Water

Stream

(Stream 25)

9624.04 9590.00 Carry on effect of stream 24

Stream 26 9624.04 9587.67 Carry on effect of stream 24

Fresh Water Stream

(Stream 27) 10000.00 10000.00 No error as the mass flow rate of water is set by user

96

Table 15: Energy Balance Comparison

STREAM ENTHALPHY (MJ/HR)

JUSTIFICATION EXCEL ASPEN PLUS

C4's Feed Stream

(Stream 1) -17541.89 -17628.72

The difference between two data (Spreadsheet and Aspen) are insignificant can be

considered as no error. The insignificant different may cause by the different source of

specific heat capacity taken for the calculation of molar enthalpy in Excel Spreadsheet

and Aspen Plus.

Methanol Feed

Stream

(Stream 2)

-101614.47 -101341.03

The difference between two data (Spreadsheet and Aspen) are insignificant can be

considered as no error. The insignificant different may cause by the different source of

specific heat capacity taken for the calculation of molar enthalpy in Excel Spreadsheet

and Aspen Plus.

Methanol Recycle

Stream (Stream 21) -25303.97 -9995.23

The same reason as in Stream 1 and Stream 2 plus the effects of pressure changes on

specific enthalpy, Ĥ and heat of mixing are neglected in excel spreadsheet calculation.

Stream 3 -144460.33 -128963.47 This same reason as in Stream 1 and Stream 2 plus the effects of pressure changes on

specific enthalpy, Ĥ and heat of mixing are neglected in excel spreadsheet calculation.

Stream 4 -144460.33 -128888.16 The effects of pressure changes on specific enthalpy, Ĥ and heat of mixing are

neglected in excel spreadsheet calculation.

Stream 5 -142856.42 -122214.13

The increase in percentage of difference in this stream compared to Stream 3 and

Stream 4 is probably caused by the different sources of specific heat capacity values

used in both calculations. The preheater, E-101 that increase the temperature in this

stream has actually further intensified the effect of the application of different Cp values

in both Excel and Aspen.

97

Stream 6 -323635.26 -139529.56 During the reaction, a few side products are generated but somehow in Excel

calculation, some assumption have been made to ignore the formation of very small

amount of side product.

MTBE Product

Stream

(Stream 12)

-288925.42 -125133.17 Carry on effect from stream 6.

Stream 13 -28755.63 -9211.25 Different in mole flow rate is the main reason for this large deviation.

Stream 14 -20803.31 -7215.06 Carry on effect from stream 13.

Flare Gas Stream

(Stream 15) -5207.89 -4600.43

The efficiency of the scrubber in Excel is assumed based on literatures review while

Aspen Plus do not allow the setting of the efficiency.

Stream 16 -325343.79 -310053.97 Depend on different specific enthalpy

Water Recycle

Stream

(Stream 28)

-308501.42 -307448.22 This stream mainly constitutes of water and thus the deviation is low compared to other

streams.

98

Stream 20 -25303.97 -9995.23 Same like stream 3

Stream 24 -299402.84 -297959.08 Same like stream 3

Waste Water

Stream

(Stream 25)

-149701.42 -148978.03 Carry on effect from stream 24.

Stream 26 -149701.42 -148978.03 Carry on effect from stream 24.

Fresh Water Stream

(Stream 27) -158800.00 -158468.68

The temperature and pressure of water can be set exactly same into the Aspen, but the

different is contributed by the different specific heat capacity values applied.

99

7.18.1 Mass Balance Justification between Manual Calculation and Aspen Simulation

In the manual (Excel Spreadsheet) calculation, ideal state assumption is made. While the

calculation based on Aspen Plus stimulation, UNIFAC is selected as the property method to

simulate the process [1]. Hence, some deviations are observed due to different basis of calculation

and phase determination.

As stated in previous section, this MTBE production plant with capacity of 300,000 tonnes

per annum is operating 24 hours and 350 days throughout a year. Hence, the mass flow rate of the

isobutylene setting is 26092.18 kg per hour. By looking the mass flow rate of isobutylene at

stream 1 for both excel hand calculation and aspen plus, the total mass flow rate is almost the

same, which are 26142.48 kg per hour. This is because the total mass flow rate of stream 1 is

depending on the capacity of production.

Mass flow rate of stream 2 is the mass flow rate of fresh feed methanol. The mass flow

rate of the methanol at stream 2 for bothe excel hand calculation and aspen plus is almost the

same, which is 13586.91 kg per hour. This is because the total mass flow rate of stream 2 is

depending on the capacity of production.

Mass flow rate of stream 3 is combination of mass flow rate of stream 1 and 2 together

with recycle stream 21. The total mass flow rate of stream 3 for excel hand calculation and aspen

plus are 43011.39 kg/hr and 40885.69/hr respectively. There are 2125.70kg/hr deviation. The

mass flow rate of methanol and also isobutylene have small deviation. Besides, the composition of

the distillate and bottom product of distillation column is different in excel hand calculation and

aspen plus. This is due to:

i) The molecular weight of component using in the excel is exact value, for example

molecular weight of methanol is 32kg/kmol, while the molecular weight using in aspen

have many decimal places. This cause the value deviate from the excel hand calculation.

ii) The recycled stream 21 is from the outlet of distillation column. In hand calculation,

assumption is made so that only light key and heavy key will distributed. For example,

water is heavy than heavy key, so that it wont distributed at the top product of distillation

column. Doing stage by stage equilibirum on hand calculation is very time consuming

and required huge times of try an errors. But on the other hand, aspen is using rigorous

method, it will run stage by stage equilibrim, so that the mass flow rate of each

component will have some deviation from our hand calculation.

100

Stream 4 and 5, which is the stream come out from pump and heater respectively, the total

mass flow rate of the stream for excel and aspen was mentioned above. Thus, the effect of stream

3 is carry on to stream 4 and 5.

Stream 6 which is the stream come out from reactor. The total mass flow rate of the

stream for excel and aspen plus is 43011.39 kg/hr and 40885.69 kg/hr respectively. We can notice

that the deviation is same as the previous stream. This is because the mass flow rate of the stream

is affected by stream 21 which is recycled methanol.

Stream 12 which is the MTBE product stream from T-101 (distillation column). The total

mass flow rate of the stream for excel and aspen plus is 37355.26 kg/hr and 37510.12 kg/hr

respectively. There is devation of the mass flowrate in excel calculation from aspen plus. Same as

stream 13 which is the distillate product from T-101. The total mass flow rate of the stream for

excel and aspen plus is 5656.13 kg/hr and 3375.57 kg/hr respectively. Same as stream 12, there is

deviation in excel calculation compared to aspen plus. This is due to the composition of distillate

and bottom product set by excel hand calculation is different from aspen plus. Following by

stream 14, the total mass flow rate of the stream for excel and aspen plus also different as it carry

on the effect from stream 13.

By looking at the total mass flow rate of stream 15 (flare gas stream), the total mass flow

rate of excel hand calculation is 2681.95 kg/hr whereas for aspen plus, we get 2631.47 kg/hr.

There is slight deviation due to the composition of MTBE escape through flare gas stream is

different for excel calculation and aspen plus. In excel hand calculation, we assume 10% of

MTBE will escape through the flare gas stream. However, in aspen plus, we found out that 97.6%

of MTBE will escape through the flare gas stream. This cause the difference in the total mass flow

rate of excel calculation and also the aspen plus. Same as stream 16, the total mass flow rate also

deviate due to the difference composition of MTBE used.

For stream 28, which is the stream of fresh feed water plus recycle stream of water, the

total mass flow rate of water in excel and also aspen are 19624.04 kg/hr and 19587.67 kg/hr. The

deviation is due to in excel calculation, we assume that 1% of water will evaporate and escape

through flare gas stream. While, in aspen plus, all water will dissolve with methanol and send to

the distillation column, T-103.

For stream 20, which is the distillate product stream come out from distillation column,T-

103. The total mass flow rate in excel and aspen are 3350.15 kg/hr and 1156.50 kg/hr

respectively. It show large deviation due to it carry on the effect of previous stream especialy

101

stream 13. This is because in stream 13, the composition of methanol in distillate product is

74.83% in aspen plus, whereas in excel calculation, we assume all methanol will distillated out as

top product. For stream 24, which is the bottom product stream come out from distillation column,

T-103. The total mass flow rate in excel and aspen are 19248.08 kg/hr and 19175.34 kg/hr

respectively. It show little discrepancy compared to distillate product stream. This is because in

stream 24, the composition of methanol is only 1%. Thus, it wont affect much.

For stream 25 and 26 which are the stream of recyled water and waste water stream

respectively. The reason of deviation is due to it carry on the effect of previous stream. On the

other hands, the total mass flow rate of stream 27 is same (10000 kg/hr). This is because stream

27 is fresh water feed. The value of mass flow rate is set by us in excel hand calculation as well as

aspen plus.

102

7.18.2 Energy Balance Justification between Manual Calculation and Aspen Simulation

For the energy balance, some of the streams are having huge differences when comparing

the manual calculation and the calculation generated by IT tools, Aspen Plus. The differences in

the calculation are basically due to the usage of different source of heat capacity coefficient. The

specific heat capacity for the excel manual calculation are mainly obtained either from Perry's

Chemical Engineers' Handbook or Elementary Principles of Chemical Processes. Meanwhile,

Aspen Plus calculated the enthalpy according to the database in Aspen Plus.

Also, another main contributor to the large deviation between Excel manual calculation

and Aspen simulate on is because of the application of different types of thermodynamic model.

In Aspen Plus simulation, UNIFAC method is chosen whereas in Excel manual calculation, the

ideal model is assumed. In addition, the calculation of energy or enthalpy in Aspen Plus software

is based on the hyperbolic function (from the Aspen Plus database) but for Excel manual

calculation, the polynomial function (mostly obtained from handbook) is used for the specific

enthalpy, Cp. Hence, the heat capacities applied in both manual Excel calculation and Aspen Plus

simulation are not same. Moreover, in the UNIFAC (Universal Functional Group Activity

Coefficient model) method, the activity coefficient, (splits into two components: a

combinatorial and a residual component ) of a component is considered in the equation

where for manual calculation, the following equation is used.

Since energy/enthalpy is the product if molar flow rate and specific enthalpy, so the

different in molar flow rate will also result in the deviation of energy. In other words, in the

energy balance, another major factor that affects the difference of enthalpy between Excel and

Aspen Plus is the carried on effect of the mass balance. The different mole flow rates will

eventually change the enthalpy in each stream. When mole flow rate deviate, the enthalpy must be

affected as well.

Generally, in the heat exchangers and pumps, the enthalpies do not show a large different

(below 1%); yet, for reactor and separation units especially distillation column, huge differences

between Excel’s calculation and Aspen’s simulation result are observed. This is due to in the

separation unit, the distribution of the components is different as mentioned above and also the

consideration of Gibbs energy of mixing, heat of absorption, heat of state changes and so on in

Aspen calculation. When the components distribution is different in both Excel and Aspen, then it

will definitely affect the mass balance and consequently the energy balance. In our case, a recycle

𝑄 + 𝑊 = ∆𝐻, where ∆𝐻 = ∫ 𝐶𝑃

𝑇

25

𝑑𝑇 + ∆𝐻𝑓25

103

stream is connected from the exit of distillation column to inlet of reactor, so, the composition

(mass flow) of the inlet stream to reactor will deviate and thus also the energy balance.

Chapter 8 Utilities and Other Issues

8.1 Utilities

Table 16: Utilities for Heater, Cooling Jacket, Condenser and Reboiler

Unit Code Types of

utility

Temperature

range, oC

Heat duty,

MJ/hr

Amount of

utility, ton/hr

Heater E-101 Cooling

Water

30-50

1603.91 19.19

E-104 7952.32 95.12

Cooling

Jacket R-101

Cooling

Water -180778.85 2162.43

Condenser E-102 Cooling

Water

-38025.46 454.85

E-105 -28749.70 343.90

Reboiler E-103 Saturated

Steam -

41140.11 18.22

E-106 4341.06 1.92

Total 3095.63

Assumption: Saturated steam flow in and saturated water flow out.

Heat of vaporization of water, Hv (25oC) = 2257.9 𝑘𝐽/𝑘𝑔

Cp water = 4.18 kJ/ kg

Example of Calculation:

1. Heater (E-101)

𝑚 = (𝑄

𝐶𝑝∆𝑇)/1000

= (1603.91 𝑥 1000

4.18 𝑥 20)/1000

=19.19 ton cooling water / hr

2. Reboiler (E-103)

𝑚 = (𝑄

𝐻𝑣)/1000

104

= (41140.11 𝑥 1000

2257.9)/1000

=18.22-ton steam / hr

Table 17: Total Electrical Energy Consumption per Year

Type of

utility Unit Code

Pressure

in

Pressure

Out

Power

Quantity,

kW

Total electrical

energy consumption

per year, kWh/yr

Electricity Pump

P-101 815 1150 17.21 144564.00

P-102 750 770 0.23 1932.00

P-103 100 120 0.20 1680.00

P-104 100 150 0.07 588.00

P-105 100 120 0.13 1092.00

Total 149856.00

Example of Calculation:

1. Pump (P-101)

Total electrical energy consumption per year

= Power Quantity ×350days

𝑦𝑒𝑎𝑟×

24ℎ𝑜𝑢𝑟𝑠

𝑑𝑎𝑦𝑠

= 17.21 ×350days

𝑦𝑒𝑎𝑟×

24ℎ𝑜𝑢𝑟𝑠

𝑑𝑎𝑦𝑠

= 144564.00 kWh/year

Table 18: Total Power Requirement

Requirement Type of utility Total amount of

utility, ton/hr

Total power

requirement, kWh/yr.

Heating Saturated steam 134.45 -

Cooling Cooling water 2961.18 -

Power Electricity - 149856.00

105

8.2 Amount of Waste Generated

8.2.1 Liquid Waste There is one stream produce liquid waste which is stream 25 from T-103 which is

methanol recovery tower. The waste stream produced from methanol recovery tower consists of

water and methanol. 50% of it is recycle back to the water scrubber by mixing it with fresh feed

water. The rest is disposed. The outlet stream liquid produced contains 0.15 wt% of methanol and

99.85 wt% of water. The liquid waste generate 9624.039 kg/hr. Amount of waste generated per

year can be calculated as below.

𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑤𝑎𝑠𝑡𝑒 𝑔𝑒𝑛𝑒𝑟𝑎𝑡𝑒𝑑 𝑝𝑒𝑟 𝑦𝑒𝑎𝑟 = 9624.039𝑘𝑔

ℎ𝑟 ×

1 𝑡𝑜𝑛

1000 𝑘𝑔 ×

24 ℎ𝑟

1 𝑑𝑎𝑦 ×

350 𝑑𝑎𝑦𝑠

1 𝑦𝑒𝑎𝑟

= 80841.93𝑡𝑜𝑛

𝑦𝑟

𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑 𝑤𝑎𝑠𝑡𝑒 = 80841.93 𝑡𝑜𝑛

𝑦𝑟 ×

0.15

100

= 121.26𝑡𝑜𝑛

𝑦𝑟

𝑤𝑎𝑡𝑒𝑟 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑 𝑤𝑎𝑠𝑡𝑒 = 80841.39𝑡𝑜𝑛

𝑦𝑟 ×

99.85

100

= 80720.67 𝑡𝑜𝑛

𝑦𝑟

Thus, the total liquid waste produced in the MTBE plant is 80841.93 ton/yr. and the

amount of methanol and water present in the liquid waste is 121.26 ton and 80720.67 ton

respectively.

8.2.2 Vapor waste

There is one stream produce vapor waste which is stream 16 from T-102 which is water

scrubber. The waste stream produced from methanol scrubber consists of C4 mixture, unreacted

isobutylene, trace amount of methanol and MTBE. Besides, 1% of water will evaporate in the

water scrubber and escape out from stream 15. The outlet stream vapor will send to burn as flare

gas. The waste produced is carbon dioxide, carbon monoxide and water. The vapor waste generate

2681.945 kg/hr. Amount of waste generated per year can be calculated as below.

𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑤𝑎𝑠𝑡𝑒𝑔𝑒𝑛𝑒𝑟𝑎𝑡𝑒𝑑 𝑝𝑒𝑟 𝑦𝑒𝑎𝑟 = 2681.945 𝑘𝑔

ℎ𝑟 ×

1 𝑡𝑜𝑛

1000 𝑘𝑔 ×

24 ℎ𝑟

1 𝑑𝑎𝑦 ×

350 𝑑𝑎𝑦𝑠

1 𝑦𝑒𝑎𝑟

106

= 22528.34 𝑡𝑜𝑛

𝑦𝑟

Thus, the total vapor waste produced in the MTBE plant is 22528.34 ton/yr.

8.2.3 Mode of liquid waste and vapour waste disposal

Methanol is a colorless, flammable liquid used in the manufacture of formaldehyde and

acetic acid. Methanol is released to the environment during industrial uses and naturally from

volcanic gases, vegetation and microbes. Exposure may occur from ambient air and during the use

of solvents. Acute (short term) or chronic (long term) exposure of humans to methanol by

inhalation or ingestion may result in blurred vision, headache, dizziness and nausea. Thus, the

liquid waste produced from the bottom of methanol recovery tower (distillation column, T-103)

need to be treated prior to discharge. Although the concentration of methanol in the effluent is low

which is only 0.15 wt%, it is still recommended to treat the effluent prior to discharge. The plant

will send the liquid waste to the wastewater treatment plant to remove the trace amount of

methanol. After methanol is being removed from the liquid mixture, then treated water can be

safely dispose to the environment.

Meanwhile, vapor waste is also produced in the MTBE production plant. The vapor waste

produced consists of carbon dioxide and water. At low carbon dioxide concentrations, our

breathing rate increases, capillaries dilate and the skin becomes flushed. With more severe

exposure, the rapid breathing becomes labored, causing restless, faintness, headache, and dulling

of consciousness. High concentration of carbon dioxide can cause asphyxiation quickly, without

warning, regardless of the oxygen concentration. Liquid carbon dioxide is so cold that skin

contact can result in severe frostbite, skin burns and other tissue damage. Thus, the vapor mixture

is first sent to treatment in order to separate carbon dioxide and water. The carbon dioxide cannot

directly dispose to the atmosphere, as it will cause the greenhouse effect. Carbon dioxide can be

sold to other industry such as food industry, electronic industry and etc. Carbon dioxide can be

converted into dry ice and is then used in the food industry for freezing food, for keeping food

cold during transport and for adding carbonation to beverages. On the other hands, in the

electronics industry, carbon dioxide is used in manufacturing applications, including

semiconductor device manufacturing, surface cleaning and circuit board assembly. Furthermore,

the chemical industry uses carbon dioxide to produce fertilizers, plastics and polymers. It is also

used to purge, pressurize and cool equipment. This is the most profitable way to manage the vapor

waste (CO2 and H2O) and at the same time, we will not contribute to the greenhouse effect.

107

Chapter 9

9.1 Mass transfer Equipment Design

9.1.1 Distillation Column, T-101 Design Criteria:

This distillation column is used to separate desired product, MTBE from mixture of unreacted methanol,

C4 mixture and by-product.

Design Parameters:

Component

Distribution

Column Sizing Plate Hydraulic

Design

Mechanical Design

Number of Stages Tray Spacing Active Area Design Pressure

Reflux Ratio Flooding Velocity Hole Area Design Temperature

Number of Actual

Stages

Net Area Tray Thickness Material of

Construction

Tray Efficiency Downcomer Area Hole Diameter Column Wall

Thickness

Location of Feed

Stage

Column Diameter Liquid Flow

Arrangement

Column Head Design

Column Height Column Pressure Drop Insulation

Weeping Checking Stress Analysis

Downcomer Liquid

Backup

Column Support

Residence Time Nozzle Size

Entrainment Checking

Number of Holes

Design Basic:

Feed stream into the distillation column T-101 consist of a mixture of unreacted methanol, C4 mixture and

by product, TBA and diisobutylene. The total mass flow rate of feed is 43011.388 kg/hr at 75 oC and

1000kPa. Distillate is carried out from the top of the column operating at 67 oC and 750kPa. On the other

hand, the bottom of column operate at 120 oC and 750kPa.

Design Method:

Fenske-Underwood-Gilliland method is used for component distribution calculation. The column sizing,

plate hydraulic design and mechanical design of the distillation column is based on Coulson and

Richardson’s Chemical Engineering Design and Ray Sinnott and Gavin Towler’s Chemical Engineering

Design.

108

Table 19: Specification sheet for distillation column T-101

Distillation Column

Identification: T-101

Item: Distillation Column

No of unit: 1

Date: 2/12/2015

By: Elaine Ooi Chin Wen

Function: To separate desired product, MTBE from mixture of unreacted methanol, C4 mixture and

by-product.

Operation: Continuous

Operating Data

Material Handled: Feed Distillate Bottom

Methanol (ton/hr) 3.158 15.788 0.00

MTBE (ton/hr) 36.659 1.833 72.620

Isobutylene (ton/hr) 2.080 10.400 0.00

Butene (ton/hr) 0.026 0.130 0.00

1,3-butadienes (ton/hr) 0.013 0.065 0.00

Butane (ton/hr) 0.013 0.065 0.0003

TBA (ton/hr) 0.910 0.00 1.820

Diisobutylene (ton/hr) 0.153 0.00 0.307

Temperature (oC) 75 67 120

Pressure (kPa) 1100 750 750

Operational Design

Number of trays: 33

Feed stage from bottom: 31

Column diameter: 5.05 m

Maximum liquid flow rate: 31.64 kg/s

Reflux ratio: 0.4356

Tray spacing: 0.6m

Functional Height: 22.77 m

Maximum vapour flow rate: 2.99m3/s

Plate Hydraulic Design

Active area: 12.02m2

Type of tray: sieve tray

Hole diameter: 5mm

Active holes: 36731

Flowrate turndown: 70%

Percentage of flooding: 64%

Tray thickness: 2mm

Weir length: 4.34m

Weir height: 0.05m

Total plate pressure drop: 115.08 mm liquid/tray

Entrainment: 0.001

Mechanical Design

Design pressure: 1100 kPa

Material of construction: Carbon steel

Type of head: Torispherical head

Insulation: Rock wool

Vessel Support: Conical skirt

Feed inlet nozzle size: 6in

Reflux inlet nozzle size: 4in

Reboiler inlet nozzle size: 2in

Design temperature: 130 oC

Column wall thickness: 30mm

Head thickness: 51mm

Insulation thickness: 75mm

Skirt thickness: 11mm

Corrosion allowance: 2mm

Top outlet nozzle size:18in

Bottom outlet nozzle size: 8in

109

Distillation Column

Item Code T-101

Date 12/12/2015

Drawn By Elaine Ooi Chin Wen

110

9.1.2 METHANOL ABSORBER/SCRUBBER (T-102) Design Basic:

Feed stream that is channelled into the absorption tower (T-102) consists of a mixture of methanol,

isobutylene, MTBE, butene, 1,3-butadiene and also butane. The total mass flow rate of feed is

5656.13 kg/hr at 393.15K and 700 kPa. Water will acts as solvent and is sprayed from top of the

column while the feed stream in vapor state that contain methanol will flow from bottom of the

column and will contact with the downcoming water. Methanol will then be absorbed into the

water solvent. The exit gas will flow to stream 15, discharge into atmosphere from the top of the

column operating at 343.15K and 100kPa whereas the bottom of the column operating at 358.15K

and 100kPa will be remove as the exit liquid through stream 16. The solvent stream will enter this

column through stream 28 that carries out 27639.06 kg/hr component at 334.81K and 100kPa.

Design Parameter:

Absorber design Mechanical design

i) Number of stages

ii) Column diameter

iii) Overall height of transfer unit

iv) Height of packings

i) Design temperature

ii) Design pressure

iii) Material of construction

iv) Absorber head design

v) Wall thickness (vessel and head)

vi) Vessel support and base

vii) Nozzle size

Design Criteria:

Operating Temperature : 110 oC

Operating Pressure : 700 kPa

Vessel Orientation : Vertical

Type of Absorber : Random Packing Absorber

Type of Packing : Intalox Saddler Ceramic (1.5 inch)

Design Method:

Cornell et al. (1960) reviewed the previously published data and presented empirical equations for

predicting the height of the gas and liquid film transfer units. Their correlation takes into account

the physical properties of the system, the gas and liquid flow-rates; and the column diameter and

height. By referring the textbook (Coulson and Richardson's Chemical Engineering), the

calculations are performed and shown after the specification table.

111

Table 20: Specification sheet for methanol absorber, T-102

Absorber

Identification: T-102

Item: Methanol Absorber

No of unit: 1

Date: 12/12/2015

By: Soon Kah Aik

Function: To absorb unreacted methanol from other C4’s components so that it can be recycle back to the

MTBE Reactor, R-101.

Operation: Continuous

Operating Data

Mass Flow Rate (ton/h)

Isobutylene

Methanol

MTBE

Water

Butene

1,3-butadienes

Butane

TBA

Diisobutylene

Feed

1.83

3.16

0.37

0

0.03

0.01

0.01

0

0

Exit Gas

0.18

0.32

0.04

0.28

0.03

0.01

0.01

0

0

Exit Liquid

0

2.85

0.393

27.35

0

0

0

0

0

Solvent

0

0.01

0

27.62

0

0

0

0

0

Total

Temperature (oC)

5.41

110

2.52

70

30.53

85

27.64

60

Absorber Design

Height of Packing: 3.0 m

Height of Tower:

Operating Pressure: 700 kPa

Solvent Flow Rate: 0.1382 m3/s

Feed Flow rate: 0.0023 m3/s

Diameter of Column: 1.1 m

Solvent: Water

Pressure Drop Across Packing: 10mm H2O

Material of Construction: Stainless Steel 316

Packing Data

Type of Packing: Intalox Saddles Ceramic

Size of Packing: 1.5in.(38mm)

Bulk Density: 625 kg/m3

Surface Area: 194 m2/m

3

Packing Factor: 170 m-1

Mechanical Design

Design Pressure: 770 kPa

Outer Diameter: 1.3 m

Vessel Wall Thickness: 6 mm

Type of Head: Torispherical Head

Head Thickness: 6 mm

Vessel Support: Conical Skirt

Height of Vessel Support: 2 m

Type Insulation: Mineral Wool

Insulation Thickness: 75 mm

Design Temperature: 75 Oc

Corrosion Allowance: 2 mm

Feed Inlet Connection:3 inch

Exit Gas Connection: 2 inch

Exit Liquid Connection: 4 inch

Solvent Inlet Connection: 4 inch

112

METHANOL ABSORBER/SCRUBBER

Item Code T-103

Date 12/12/2015

Drawn By Soon Kah Aik

113

9.1.3Distillation Column, T-103

Design Criteria:

This distillation column is used to separate methanol from mixture of MTBE and water. The recover

methanol and water can recycle back to the feed.

Design Parameters:

Component

Distribution

Column Sizing Plate Hydraulic

Design

Mechanical Design

Number of Stages Tray Spacing Active Area Design Pressure

Reflux Ratio Flooding Velocity Hole Area Design Temperature

Number of Actual

Stages

Net Area Tray Thickness Material of

Construction

Tray Efficiency Downcomer Area Hole Diameter Column Wall

Thickness

Location of Feed

Stage

Column Diameter Liquid Flow

Arrangement

Column Head Design

Column Height Column Pressure Drop Insulation

Weeping Checking Stress Analysis

Downcomer Liquid

Backup

Column Support

Residence Time Nozzle Size

Entrainment Checking

Number of Holes

Design Basic:

Feed stream into the distillation column T-103 consist of a mixture of methanol, water and MTBE. The

total mass flow rate of feed is 30533.095 kg/hr at 85 oC and 100kPa. Distillate is carried out from the top of

the column operating at 38 oC and 100kPa. On the other hand, the bottom of column operate at 90

oC and

100kPa.

Design Method:

Fenske-Underwood-Gilliland method is used for component distribution calculation. The column sizing,

plate hydraulic design and mechanical design of the distillation column is based on Coulson and

Richardson’s Chemical Engineering Design and Ray Sinnott and Gavin Towler’s Chemical Engineering

Design.

114

Table 21: Specification sheet for distillation column T-103

Distillation Column

Identification: T-103

Item: Distillation Column

No of unit: 1

Date: 2/12/2015

By: Elaine Ooi Chin Wen

Function: To separate methanol from mixture of methanol, MTBE and water

Operation: Continuous

Operating Data

Material Handled: Feed Distillate Bottom

Methanol (ton/hr) 2.855 19.783 0.03

MTBE (ton/hr) 0.330 2.309 0.00

Water (ton/hr) 27.349 1.914 28.713

Temperature (oC) 85 38 90

Pressure (kPa) 100 100 100

Operational Design

Number of trays: 30

Feed stage from bottom: 23

Column diameter: 6.84 m

Maximum liquid flow rate: 44.44 kg/s

Reflux ratio: 7.245

Tray spacing: 0.6m

Functional Height: 20.72 m

Maximum vapour flow rate: 50.67m3/s

Plate Hydraulic Design

Active area: 22.08m2

Type of tray: sieve tray

Hole diameter: 5mm

Active holes: 67461

Flowrate turndown: 70%

Percentage of flooding: 50%

Tray thickness: 2mm

Weir length: 5.89m

Weir height: 0.05m

Total plate pressure drop: 178.94 mm liquid/tray

Entrainment: 0.02

Mechanical Design

Design pressure: 110 kPa

Material of construction: Carbon steel

Type of head: Torispherical head

Insulation: Rock wool

Vessel Support: Conical skirt

Feed inlet nozzle size: 6in

Reflux inlet nozzle size: 4in

Reboiler inlet nozzle size: 12in

Design temperature: 100 oC

Column wall thickness: 6mm

Head thickness: 9mm

Insulation thickness: 75mm

Skirt thickness: 16mm

Corrosion allowance: 2mm

Top outlet nozzle size: 30in

Bottom outlet nozzle size: 4in

115

Distillation Column

Item Code T-103

Date 12/12/2015

Drawn By Elaine Ooi Chin Wen

Top Outlet

Column

Height

Feed

Inlet

116

9.2 Heat Transfer Equipment

9.2.1 Feed Heater, E-101 Design Criteria:

The feed heater E-101 is used to heat up the mixture of methanol, water, dimethyl ether, hydrogen,

nitrogen, carbon dioxide and carbon monoxide from storage tank and also recycle stream at 11.00

bar from T=90OC to T= 100

OC, before this stream enters the synthesis reactor (R-101). The steam

used to heat up the mixture enters at T=250OC and leaves at T=150

OC at 11.10 bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

117

Table 22: Specification Sheet for Feed Heater, E-101

HEAT EXCHANGER E-101

Identification: Item: Heater Date: 12th

December 2015

Item No. E-101

No. Required: 1 By: Syed Zulfadi Syed Putra

Function: The feed heater E-101 is used to heat up the mixture of methanol, water, dimethyl ether,

hydrogen, nitrogen, carbon dioxide and carbon monoxide from storage tank and also recycle stream at

11.00 bar from T=90OC to T= 100

OC, before this stream enters the synthesis reactor (R-101). The steam

used to heat up the mixture enters at T=250OC and leaves at T=150

OC at 11.10 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 2 Tube Passes

Duty: 445.53 kW

Overall Coefficient: 500 W/m2.oC

Tube-side: Tubes:

Fluid Handled Process fluid Outside Diameter 19.05 mm

Flow Rate 3.98 kg/s Inside Diameter 15.8 mm

Temperature 28 to 75 oC Nozzle Diameter 80 mm

Pressure 11 Bar Length 1.83 m

Pressure Drop 0.018 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 99 tubes

Number of Passes 2 Passes

Shell-side: Shell:

Fluid Handled Steam Shell Diameter 0.34 m

Flow Rate 1.78 kg/s Baffle Spacing 0.068 m

Temperature 150 to 120 oC Nozzle Diameter 50 mm

Pressure 11.10 Bar Number of Shells 1 Shell

Pressure Drop 0.019 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m. K , the radius of insulator = 0.0072 mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

118

Heat Exchanger

Item Code E-101

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

119

9.2.2 Condenser, E-102 Design Criteria:

The Condenser E-102 is used to condense the mixture of methanol, water, dimethyl ether,

hydrogen, nitrogen, carbon dioxide and carbon monoxide from synthesis reactor (R-101) at 7.50

bar from T=67OC to T= 62

OC, before this stream enters the distillation column (T-101). The brine

solution used to cool down the mixture enters at T=5OC and leaves at T=15

OC at 7.50 bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

120

Table 23: Specification Sheet for Condenser, E-102

HEAT EXCHANGER E-102

Identification: Item: Condenser Date: 12th

December 2015

Item No. E-102

No. Required: 1 By: Syed Zulfadli Syed Putra

Function: The condenser E-102 is used to cool down the mixture of methanol, water, dimethyl ether,

hydrogen, nitrogen, carbon dioxide and carbon monoxide at 7.50 bar from T=67OC to T= 62

OC. The

brine solution used to cool down the mixture enters at T=5OC and leaves at T=15

OC at 7.50 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 4 Tube Passes

Duty: 10562.63 kW

Overall Coefficient: 500 W/m2.oC

Tube-side: Tubes:

Fluid Handled Brine solution Outside Diameter 19.05 mm

Flow Rate 126.35 kg/s Inside Diameter 15.80 mm

Temperature 5 to 15 oC Nozzle Diameter 328 mm

Pressure 7.50 Bar Length 5 m

Pressure Drop 0.556 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 1585 tubes

Number of Passes 4 Passes

Shell-side: Shell:

Fluid Handled Process Fluid Shell Diameter 1.10 m

Flow Rate 7.86 kg/s Baffle Spacing 0.22 m

Temperature 68 to 62 oC Nozzle Diameter 113 mm

Pressure 7.50 Bar Number of Shells 1 Shell

Pressure Drop 0.0146 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m.K , the radius of insulator = 0.0067mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

121

Condenser

Item Code E-102

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

122

9.2.3 Reboiler, E-103 Design Criteria:

The reboiler E-103 is used to vaporise the mixture of methanol and water at 7.50 bar from T =

120OC to T = 130

OC. The steam used to vaporise the mixture enters at T=350

OC and leaves at

T=150OC at 7.50 bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

123

Table 24: Specification Sheet for Reboiler, E-103

HEAT EXCHANGER E-103

Identification: Item: Reboiler Date: 12th

December 2015

Item No. E-103

No. Required: 1 By: Syed Zulfadli Syed Putra

Function: The reboiler E-103 is used to vaporise the mixture of methanol and water at 7.50 bar from T =

120OC to T = 130

OC. The steam used to vaporise the mixture enters at T=350

OC and leaves at T=150

OC

at 7.50 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 8 Tube Passes

Duty: 2104.97 kW

Overall Coefficient: 750 W/m2.oC

Tube-side: Tubes:

Fluid Handled Process Fluid Outside Diameter 19.05 mm

Flow Rate 20.76 kg/s Inside Diameter 14.83 mm

Temperature 120 to 130 oC Nozzle Diameter 179 mm

Pressure 7.50 Bar Length 2.44 m

Pressure Drop 0.20 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 1293 tubes

Number of Passes 8 Passes

Shell-side: Shell:

Fluid Handled Steam Shell Diameter 1.027 m

Flow Rate 7.50 kg/s Baffle Spacing 0.029 m

Temperature 5 to 25 oC Nozzle Diameter 86 mm

Pressure 7.50 Bar Number of Shells 1 Shell

Pressure Drop 00.74 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m.K , the radius of insulator = 0.005mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

124

Reboiler

Item Code E-103

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

125

9.2.4 Heater, E-104 Design Criteria:

The heater E-104 is used to heat up the process fluid from T= 62OC to T= 110

OC. The steam used

to heat the mixture enters at T=250OC and leaves at T=150

OC at 7 bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

126

Table 25: Specification Sheet for Heater, E-104

HEAT EXCHANGER E- 104

Identification: Item: Heater Date: 12th

December 2015

Item No. E-104

No. Required: 1 By: Syed Zulfadli Syed Putra

Function: The heater E-104 is used to heat up the process fluid from T= 62OC to T= 110

OC. The steam

used to heat the mixture enters at T=250OC and leaves at T=150

OC at 7 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 1 Tube Passes

Duty: 2208.98 kW

Overall Coefficient: 950 W/m2.oC

Tube-side: Tubes:

Fluid Handled Steam Outside Diameter 19.05 mm

Flow Rate 26.42 kg/s Inside Diameter 14.83 mm

Temperature 250 to 150 oC Nozzle Diameter 180 mm

Pressure 7.50 Bar Length 3.66 m

Pressure Drop 0.066 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 119 tubes

Number of Passes 1 Passes

Shell-side: Shell:

Fluid Handled Process Fluid Shell Diameter 0.354 m

Flow Rate 12.39 kg/s Baffle Spacing 0.0177 m

Temperature 445.35 to 100 oC Nozzle Diameter 56 mm

Pressure 7.50 Bar Number of Shells 1 Shell

Pressure Drop 0.80 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m.K , the radius of insulator = 0.012 mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

127

Heater

Item Code E-104

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

128

9.2.5 Condenser, E-105 Design Criteria:

The condenser E-105 is used to condense the process mixture at 1 bar from T=38OC to T=

33OC.The brine solution used to condense the mixture enters at T=5

OC and leaves at T=15

OC at 1

bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

129

Table 26: Specification Sheet for Condenser, E-105

HEAT EXCHANGER E-105

Identification: Item: Condenser Date: 12th

December 2015

Item No. E-105

No. Required: 1 By: Syed Zulfadli Syed Putra

Function: The condenser E-105 is used to condense the process mixture at 1 bar from T=38OC to T=

33OC.The brine solution used to cool down the mixture enters at T=5

OC and leaves at T=15

OC at 1 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 2 Tube Passes

Duty: 7989.03 kW

Overall Coefficient: 550 W/m2.oC

Tube-side: Tubes:

Fluid Handled Brine Solution Outside Diameter 19.05 mm

Flow Rate 95.53 kg/s Inside Diameter 18.43 mm

Temperature 5 to 15 oC Nozzle Diameter 300 mm

Pressure 1.00 Bar Length 5 m

Pressure Drop 0.28 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 2332 tubes

Number of Passes 6 Passes

Shell-side: Shell:

Fluid Handled Steam Shell Diameter 1.28 m

Flow Rate 6.51 kg/s Baffle Spacing 0.26 m

Temperature 38 to 33 oC Nozzle Diameter 100 mm

Pressure 1.00 Bar Number of Shells 1 Shell

Pressure Drop 0.0055 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m.K , the radius of insulator = 0.045 mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

130

Condenser

Item Code E-105

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

131

9.2.6 Reboiler, E-106

Design Criteria:

The Reboiler E-106 is used to vaporise the process mixture at 25 bar from T=90OC to T= 100

OC.

The steam used to heat up the mixture enters at T=250OC and leaves at T=150

OC at 26 bar.

Design Parameter:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

Design Method:

The heat exchanger design is based on Coulson and Richardson’s Chemical Engineering Design. For the

properties of the components in stream, it is determined from Elementary Principles of Chemical Processes,

Handbook of Chemistry and Physics and Perry Chemical Engineer’s Handbook.

132

Table 27: Specification Sheet for Reboiler, E-106

HEAT EXCHANGER E-106

Identification: Item: Reboiler Date: 12th

December 2015

Item No. E-106

No. Required: 1 By: Syed Zulfadli Syed Putra

Function: The Reboiler E-106 is used to vaporise the process mixture at 25 bar from T=90OC to T= 100

OC. The steam used to heat up the mixture enters at T=250

OC and leaves at T=150

OC at 26 bar.

Operation: Continuous

Type: Horizontal shell and tube

Split-ring floating head

1 Shell Pass – 2 Tube Passes

Duty: 5919.03 kW

Overall Coefficient: 800 W/m2.oC

Tube-side: Tubes:

Fluid Handled Process Fluid Outside Diameter 12.60 mm

Flow Rate 5.80 kg/s Inside Diameter 16.00 mm

Temperature 90 to 100 oC Nozzle Diameter 96.3 mm

Pressure 25 Bar Length 3.66 m

Pressure Drop 0.013 Bar Pitch and Arrangement 23.81 mm (triangle)

Material Stainless Steel

316 Tubes per Pass 305 tubes

Number of Passes 2 Passes

Shell-side: Shell:

Fluid Handled Steam Shell Diameter 0.51 m

Flow Rate 0.53 kg/s Baffle Spacing 0.023 m

Temperature 250 to 150 oC Nozzle Diameter 30.1 mm

Pressure 26 Bar Number of Shells 1 Shell

Pressure Drop 0.602 Bar Number of Passes 1 Pass

Material Stainless Steel 316

Insulation: Fiber glass with K=0.04W/m.K , the radius of insulator = 0.0033 mm

Tolerances: Tubular Exchanger Manufactures Association (TEMA) standards

Comment and Drawings: Schematic diagram included.

133

Reboiler

Item Code E-106

Date 12/12/2015

Drawn By Syed Zulfadi Syed Putra

134

9.3 Reactor Design

9.3.1 MTBE REACTOR (R-101) DESIGN Design Basic:

This plant design is aimed to produce 300,000 metric tonnes of Methyl Tert-Butyl Ether (MTBE)

per annum to fulfil the demand from market either local or international. Reactor is important as it

is where the desired product (MTBE) is formed from feed reactants. In this design, since a

continuous reaction is desired, so the reactor used is catalytic packed bed reactor where its

packings are made up catalyst named Amberlyst-15. Isobutylene will feed together with methanol

into the reactor. The operating temperature of the reactor is fixed at 75oC and pressure 1100kPa.

Water coolant is used to cool down the heat generated by the exothermic reaction in the reactor by

circulating cold water around the reactor. Since this reaction is reversible, to ensure the reaction

equilibrium always shift to right (towards the formation of MTBE), the temperature of reaction

must be low. Also, at low temperature the catalyst activity and life span can be prolonged. At the

operating condition, the conversion and selectivity of isobutylene to MTBE is 92% and 96.5%,

respectively.

Design Parameter:

Reactor design Mechanical design

v) Weight of catalysts

vi) Number of tubes

vii) Tubes configuration

viii) Shell dimension

ix) Baffle configuration

x) Cooling requirement analysis

xi) Heat transfer area

xii) Heat transfer coefficient

viii) Design temperature

ix) Design pressure

x) Material of construction

xi) Reactor head design

xii) Wall thickness (Shell, tubes, vessel head)

xiii) L/D ratio

xiv) Stress analysis

xv) Vessel support and base

xvi) Nozzle size

Design Criteria:

Operating Temperature : 75oC

Operating Pressure : 1100kPa

Vessel Orientation : Vertical

Type of Catalyst : Heterogeneous

Type of Reactor : Multi-tubular Packed Bed Reactor

Design Method:

This MTBE reactor in this plant is designed based on the kinetic data collected for MTBE

production. With the aids of POLYMATH®

software, the weight of catalyst required to achieve

the production rate can be determined. The cooling requirement design is based on shell and tube

heat exchanger design based on the requirement of TEMA. The mechanical design is based on

Coulson and Richardson’s Chemical Engineering Design. Physical property data of the process

fluid are obtained either from Perry’s Chemical Engineer’s Handbook or calculated using Aspen

Plus®

software.

135

Table 28: Specification sheet for MTBE reactor, R-101

Reactor

Identification: R-101

Item: MTBE Reactor

No of unit: 1

Date: 12/12/2015

By: Soon Kah Aik

Function: To produce main product, Methyl Tert-Butyl Ether(MTBE) via Etherification of

Isobutylene and Methanol

Operation: Continuous

Operating Data

Tube Side Shell Side

Pressure (kPa)

Inlet Temperature(oC)

Outlet Temperature(oC)

1100

75

75

Pressure (kPa)

Inlet Temperature(oC)

Outlet Temperature(oC)

101.3

30

50

Mass Flow Rate (ton/h) Inlet Outlet Mass Flow Rate (ton/h) Inlet Outlet

Isobutylene

Methanol

MTBE

Water

Butene

1,3-butadienes

Butane

TBA

Diisobutylene

26.04

16.37

0.33

0.30

0.03

0.01

0.01

0

0

1.83

3.16

36.66

0

0.03

0.01

0.01

1.24

0.15

Water 7.87 7.87

Total 43.09 43.09 Total 7.87 7.87

Catalyst Data

Type of Reactor: Catalytic, multi-tubular packed

bed reactor accomplished with

cooling system (Isothermal)

Catalyst: Amberlyst-15

Catalyst Bulk Density: 770kg/m3

Porosity/Void Fraction: 0.30

Reactor Design

Tube Side Shell Side

Material of Construction

No. of Tube

Schedule Designation

Outside Diameter (mm)

Inside Diameter (mm)

Pitch -Triangle (mm)

Length (m)

No. of Passes

Bundle Diameter (m)

Stainless Steel 316

1360

ASME 10/10S

60.3

54.76

75.38

7.32

1

2.98

Material of Construction

No. of Shell

Outside Diameter (m)

Inside Diameter (m)

No. of Baffle

Baffle Spacing (m)

Baffle Cut (%)

Stainless Steel 316

1

3.66

3.61

10

0.78

25

Heat Transfer Area : 1885.89 m2

Overall Heat Transfer Coefficient : 75.88 W/m2 K

Mechanical Design

Design Pressure: 110 kPa

Material Of Construction: Stainless Steel 316

Type Of Head: Ellipsoidal Head

Vessel Support: Conical Skirt

Feed Inlet Nozzle Size: 6 in

Product Outlet Nozzle Size: 8 in

Shell/Head MAWP: 61.8 bar

Design Temperature: 75 OC

Operating Weight: 852894 N

Head Thickness: 25.4 mm

Skirt Thickness: 25.4 mm

Corrosion Allowance: 2 mm

Coolant Inlet/Outlet Nozzle Size: 2.5 in

Tube MAWP: 425.6 bar

136

METHYL TERT-BUTYL ETHER (MTBE) REACTOR

Item Code R-101

Date 12/12/2015

Drawn By Soon Kah Aik

137

9.4 Auxiliary Equipment Design

9.4.1 Pump Design Criteria:

The purpose of pump is to pump and transport liquid to the next unit by mechanical means. There are total

5 pumps involved which are P-101, P-102, P-103, P-104 and P-105.

The functions of each different pump are stated as below:

P-101: To pump the mixture of fresh feed (isobutylene and methanol) and recycled methanol to the feed

heater (E-101)

P-102: To pump the distillate product back to the distillation column (T-101) via reflux inlet

P-103: To pump the distillate product back to the distillation column (T-103) via reflux inlet

P-104: To pump the recovery methanol from distillation column (T-103) back to the fresh methanol feed

stream.

P-105: To pump the recovery water from the distillation column (T-103) back to fresh water feed stream.

Design Parameters:

Pump

Nozzle Size

Total Head

NPSH

Motor Power

Design Method:

The pump power design is based on the Bernoulli’s Equation which is:

𝑃1

𝜌𝑔+ 𝑧1 +

𝑣12

2𝑔+ ℎ𝑝 =

𝑃2

𝜌𝑔+ 𝑧2 +

𝑣22

2𝑔+ ℎ𝑓

The overall pump design is based on the pump supplier’s pump performance curve.

138

9.4.1.1 Feed Pump, P-101

Table 29: Specification Sheet of Feed Pump, P-101

FEED PUMP (P-101)

Item: Centrifugal Pump

Identification Item no: P-101

Date 13/12/2015

No. required: 1 By Syafiqah

Function: To mix isobutylene and methanol before entering the reactor, R-101

Operation: Continuous

Operating Data

Inlet Temperature (◦C) 28.0

Inlet Pressure (kPa) 815.0

Outlet Pressure (kPa) 1150.0

Pressure Difference (kPa) 1020.0

Orientation & Dimension

Mass Flow Rate (kg/hr) 43011.39

Volumetric Flow Rate (m3/hr) 45.2077

Actual Motor Power (kW) 277809.1

Power Required (kW) 175019.8

Design Data

Total Head (m) 41.4796

NPSH available (m) 81.0197

NPSH required (m) 150

Pump Speed (rpm) 3500

Efficiency (%) Single-stage

M.O.C Stainless steel +Chromium content>12

Utility Electrical Supply

Mechanical Design Data

Length of suction side, L1(m) 3.00

Length of discharge side, L2(m) 10.00

Total length of pipe,L(m) 13.00

Inlet elevation, Z1 (m) 5.00

Outlet elevation,Z2(m) 10.00

139

9.4.1.2 Reflux Pump, P-102

Table 30: Specification Sheet of Reflux Pump, P-102

REFLUX PUMP (P-102)

Item: Diaphragm Pump

Identification Item no: P-102

Date 01/12/2015

No. required: 1 By Ezati

Function: To pump the liquid from condenser (E-102) at stream 9a to stream 9 into MTBE

Tower(T-101).

Operation: Continuous

Operating Data

Inlet Temperature (◦C) 62.0

Inlet Pressure (kPa) 750.0

Outlet Pressure (kPa) 770.0

Pressure Difference (kPa) 20.0

Orientation & Dimension

Mass Flow Rate (kg/hr) 22624.52

Volumetric Flow Rate (m3/hr) 33.42

Actual Motor Power (kW) 3244.52

Power Required (kW) 1784.49

Design Data

Total Head (m) 6.7998

NPSH available (m) 100.9757

NPSH required (m) 7.62

Pump Speed (rpm) 3500

Efficiency (%) 55.00

M.O.C Cast Steel/ Iron/ Copper alloy

Utility Electricity Supply

Mechanical Design Data

Length of suction side, L1(m) 5.00

Length of discharge side, L2(m) 5.00

Total length of pipe,L(m) 10.00

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

140

9.4.1.3 Reflux Pump, P-103

Table 31: Specification Sheet of Reflux Pump, P-103

REFLUX PUMP (P-103)

Item: Diaphragm Pump

Identification Item no: P-103

Date 01/12/2015

No. required: 1 By Ezati

Function: To pump the liquid from condenser (E-105) at stream 19a to stream 19 into

Methanol Recovery (T-103)

Operation: Continuous

Operating Data

Inlet Temperature (◦C) 33.0

Inlet Pressure (kPa) 100.0

Outlet Pressure (kPa) 120.0

Pressure Difference (kPa) 20.0

Orientation & Dimension

Mass Flow Rate (kg/hr) 3350.15

Volumetric Flow Rate (m3/hr) 28.38

Actual Motor Power (kW) 3244.52

Power Required (kW) 2520548.01

Design Data

Total Head (m) 6.24

NPSH available (m) 3.147

NPSH required (m) 7.62

Pump Speed (rpm) 3500

Efficiency (%) 55.00

M.O.C Cast Steel/ Iron/ Copper alloy

Utility Electricity Supply

Mechanical Design Data

Length of suction side, L1(m) 5.00

Length of discharge side, L2(m) 5.00

Total length of pipe,L(m) 10.00

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

141

9.4.1.4 Methanol Recycle Pump, P-104

Table 32: Specification Sheet of Methanol Recycle Pump, P-104

METHANOL RECYCLE PUMP (P-104)

Item: Centrifugal Pump

Identification Item no: P-104

Date 01/12/2015

No. required: 1 By Ezati

Function: To pump the liquid which is mostly methanol from stream 20 to stream 21 to feed

back into the process.

Operation: Continuous

Operating Data

Inlet Temperature (◦C) 33.0

Inlet Pressure (kPa) 100.0

Outlet Pressure (kPa) 150.0

Pressure Difference (kPa) 50.0

Orientation & Dimension

Mass Flow Rate (kg/hr) 20576.974

Volumetric Flow Rate (m3/hr) 25.62

Actual Motor Power (kW) 3244.52

Power Required (kW) 2520548.01

Design Data

Total Head (m) 10.17

NPSH available (m) 3.19

NPSH required (m) 7.62

Pump Speed (rpm) 3500

Efficiency (%) 55.00

M.O.C Cast Steel/ Iron/ Copper alloy

Utility Electricity Supply

Mechanical Design Data

Length of suction side, L1(m) 1.00

Length of discharge side, L2(m) 20.00

Total length of pipe,L(m) 21.00

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

142

9.4.1.5 Water Recycle Pump, P-105

Table 33: Specification Sheet of Water Recycle Pump, P-105

WATER RECYCLE PUMP (P-105)

Item: Diaphragm Pump

Identification Item no: P-105

Date 13/12/2015

No. required: 1 By Syafiqah

Function: To recycle back water to Methanol Scrubber (T-102)

Operation: Continuous

Operating Data

Inlet Temperature (◦C) 100.0

Inlet Pressure (kPa) 100.0

Outlet Pressure (kPa) 120.0

Pressure Difference (kPa) 20.0

Orientation & Dimension

Mass Flow Rate (kg/hr) 19248.08

Volumetric Flow Rate (m3/hr) 20.0908

Actual Motor Power (kW) 1230.139

Power Required (kW) 492.0556

Design Data

Total Head (m) 2.6059

NPSH available (m) 4.5521

NPSH required (m) 1.00

Pump Speed (rpm) 3500

Efficiency (%) 40.00

M.O.C Cast Steel/ Iron/ Copper alloy

Utility Electrical Supply

Mechanical Design Data

Length of suction side, L1(m) 6.00

Length of discharge side, L2(m) 7.00

Total length of pipe,L(m) 13.00

Inlet elevation, Z1 (m) 5.00

Outlet elevation,Z2(m) 5.00

143

9.5 Comparison between Aspen and Excel Calculation

9.5.1 Mass Transfer Equipment 9.5.1.1 Distillation Column, T-101

Figure 30: Aspen Result for Distillation Column, T-101

Table 34: Comparison between Aspen and Excel Calculation Value for T-101

Aspen Calculation Excel Calculation

Minimum Reflux Ratio 3.78 0.36

Actual Reflux Ratio 4.3 0.44

Minimum Number of Stages 6.96 5.73

Actual Number of Stages 14.99 33

Feed Stages 6.87 31

Justification:

In aspen calculation, we are using DSTWU method to calculate the design parameter of distillation column.

In Excel calculation, we are using Fenske-Underwood-Gilliland (FUG) to calculate the design parameter of

distillation column. Both methods are quite similar as DSTWU method is based on the well-known FUG

correlations. Through the calculation, the minimum and actual reflux ratios, minimum and actual number

of stages and optimum feed location are estimated.

However, we found out that there are some differences between the value from Aspen and Excel

calculation. This is due to the difference value we used for vapour pressure. In Excel calculation, the value

of vapour pressure is get from Perry Handbook. On the other hands, Aspen will use their own value from

its database. This causes the difference value in relative volatility which will further lead to difference

value in the minimum reflux ratio and also minimum number of stages.

144

9.5.1.2 Distillation Column, T-103

Figure 31: Aspen Result for Distillation Column, T-103

Table 35: Comparison between Aspen and Excel Calculation Value for T-103

Aspen Calculation Excel Calculation

Minimum Reflux Ratio 7.08 6.04

Actual Reflux Ratio 7.2 7.2

Minimum Number of Stages 4.56 16.56

Actual Number of Stages 35.4 30

Feed Stages 18.9 23

Justification:

In aspen calculation, we are using DSTWU method to calculate the design parameter of distillation column.

In Excel calculation, we are using Fenske-Underwood-Gilliland (FUG) to calculate the design parameter of

distillation column. Both methods are quite similar as DSTWU method is based on the well-known FUG

correlations. Through the calculation, the minimum and actual reflux ratios, minimum and actual number

of stages and optimum feed location are estimated.

However, we found out that there are some differences between the value from Aspen and Excel

calculation. This is due to the difference value we used for vapour pressure. In Excel calculation, the value

of vapour pressure is get from Perry Handbook. On the other hands, Aspen will use their own value from

its database. This causes the difference value in relative volatility which will further lead to difference

value in the minimum reflux ratio and also minimum number of stages.

145

9.5.2 Heat Transfer Equipment 9.5.2.1 Feed Heater, E-101

Figure 32: Aspen Result for Feed Heater, E-101

Table 36: Comparison between Aspen and Excel Calculation Value for E-101

Aspen Calculation Excel Calculation

Temperature (oC) 75 75

Vapor fraction 0 0

Heat Duty 447.51 445.53

Net Duty 447.59 445.53

In aspen calculation, we got heat duty much more than excel calculation. This is because

calculation aspen is much accurate then excel calculation. The assumption for heat exchanger for

aspen is directly taken from the data base but for the excel calculation, the assumption is based on

our group. The excel calculation is much lower in term of heat duty although the temperature for

aspen calculation and excel calculation has the same temperature. They are also having the same

vapor fraction which is zero means that the mixture is exist totally in liquid.

146

9.5.2.2 Heater, E-104

Figure 33: Aspen Result for Heater, E-104

Table 37: Comparison between Aspen and Excel Calculation Value for E-104

Aspen Calculation Excel Calculation

Temperature (oC) 110 110

Vapor fraction 0 0

Heat Duty 2291.04 2208.98

Net Duty 2291.04 2208.98

In aspen calculation, we got heat duty much more than excel calculation. This is because

calculation aspen is much accurate then excel calculation. The assumption for heat exchanger for

aspen is directly taken from the data base but for the excel calculation, the assumption is based on

our group. The excel calculation is much lower in term of heat duty although the temperature for

aspen calculation and excel calculation has the same temperature. They are also having the same

vapor fraction which is zero means that the mixture is exist totally in liquid.

9.5.3 Reactor Design 9.5.3.1 MTBE Reactor, R-101

Please refer to energy balance as only heat duty provided by aspen.

147

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http://www.praxair.com/~/media/North%20America/US/Documents/Specification%20Sheet

s%20and%20Brochures/Gases/Isobutylene%20C4H8%20Spec%20Sheet%20SS%20P4614.

pdf

102. MTBE Production using Methanol and Isobutylene [Online, Accessed On 27th

September

2015], Available From:

http://www.gasinnovations.com/literature/HYDROCARBON/Isobutylene-C.P.-Grade.pdf

103. F.Collignon et.al, Liquid Phase Synthesis of MTBE from Methanol and Isobutene over Acid

Zeolites and Amberlyst-15, Journal of Catalysis

104. MTBE Synthesis in A Riser Simulators [Online, Accessed On: 22nd

September 2015],

Available From: http://www.collectionscanada.gc.ca/obj/s4/f2/dsk2/ftp01/MQ28568.pdf

105. Andreas Beckmann et.al, Industrial experience in the scale-up of reactive distillation with

examples from C4-chemistry

155

Appendix A

Thermodynamic Data of Reactants and Product Table 38:: Thermodynamic Data of Isobutene, Methanol and MTBE

[63] [64] [65]

Properties Value

Isobutene Methanol MTBE

Critical Temperature 144˚C 240˚C 223.9 ˚C

Critical pressure 4000 kPa 78.50 atm 223.9 KPc

Heat of fusion at

melting point & 1 atm 105.714 kJ/kg 98.8 kJ/kg 94021 kJ/kg

Heat of evaporation at

boiling point & at 1 atm 391.634kJ/kg 846 kJ/kg 318.77 kJ/kg

Heat of formation at

25˚C & 1 atm

-301.3 kJ/kg

(gas phase)

-238.6 kJ/kmol(l)

-201.2 kJ/mol(g) -3216.1 kJ/kg (g)

Heat of combustion at

25˚C & 1 atm -16.9 kJ/mol

726.6 kJ/mol (L)

-764.0 kJ/mol (g) 38.21 MJ/kg

Heat of vaporisation at

boiling point& 1 atm 391.634 kJ/kg 846 kJ/kg 318.77 kJ/kg

Heat of polymerization Not pertinent Not pertinent Not pertinent

Specific heat

At 25˚C

1.487 kJ/ kg˚C

2.531 kJ/kg ˚C

2.092 kJ/kg. ˚C

Gibbs free energy of

formation 58.08 MJ/kmol

-162.62 MJ/kmol

-117.5 MJ/kmol

156

Table 39: Thermodynamic Data of Di-isobutylene, Dimethyl ether, TBA and Water

[66][67][68]

Properties Value

Di-isobutylene Dimethyl ether TBA Water

Critical

Temperature 286.7°C 127.15 °C 82.6°C 374 °C

Critical pressure 25.85 atm 52.70 atm 39.2 atm 218 atm

Heat of fusion

at melting point

& 1 atm

78.33 kJ/kg

107.00 kJ/kg

91.61 kJ/kg

334.774 kJ/kg

Heat of

evaporation at

boiling point &

at 1 atm

250 kJ/kg

461.55 kJ/kg

544 kJ/ kg

2256.16 kJ/kg

Heat of

formation at

25˚C & 1 atm

-0.1699

kJ/kmol

-184.18

kJ/ kmol

-312.4

kJ/kmol

-285.84 kJ/mol

(liquid)

-241.83 kJ/mol

(gas)

Heat of

combustion at

25˚C & 1 atm

-44 MJ/kg

-31.3 MJ/kg

-32.57 MJ/kg

0 kJ/kg

Heat of

vaporisation at

boiling point &

1 atm

0.25 MJ/kg

461.55 kJ/kg

544 kJ/ kg

2256.16 kJ/kg

Heat of

polymerization Not pertinent Not pertinent Not pertinent Not pertinent

Specific heat

At 25˚C

1.049

kJ/ mol.K

0.0681

kJ/ mol.K

0.2153

kJ/mol.K

75.43

g/mol.k

Gibbs Free

878.72 kJ/kg

-24.48 kJ/kg

-2.396 kJ/kg

-237.14

kJ/mol(liquid)

157

Energy -228.61

kJ/mol(gas)

Physical Data Table 40: Physical Data of Isobutene, Methanol and MTBE

[63] [64] [65]

Properties Value

Isobutene Methanol MTBE

Molecular Formula C4H8 /

CH2=C(CH3)2

CH3OH C5H12O

Molecular Weight 56.11 32.04 88.15

State Gas Liquid Liquid

Colour Colourless Colourless Colourless

Odour Sweetish Mild characteristic

alcohol odour

sweet, solvent-like,

alcohol, or turpentine

Density 2.5326 kg/m

3 at

15˚Cand 1.013 bar 791 kg/m³ at 20 °C 740.6 kg/m3 (20℃)

Melting Point -140.3˚C -97.8˚C -109 ˚C

Boiling Point -6.9˚C 64.7˚C 55.2 ˚C

Refractive Index 1.3811

1.33066 (15 ˚C)

1.32840 (20°C)

1.32652 (25°C)

1.3689(20°C)

Water Solubility

Level of solubility

in isobutylene

0.263 g/l at 25 °C

Soluble in all

proportions in

ethanol, benzene,

other alcohols,

chloroform, diethyl

ether, other ethers,

esters, ketones and

most organic

solvents

Soluble in methanol,

diethyl ether. Partially

soluble in cold water

158

Table 41: Physical Data of Di-isobutylene, Dimethyl ether, TBA and Water

[66][67][68]

Properties Value

Di-isobutylene Dimethyl ether TBA Water

Molecular

Formula

C8H16 C2H6O C4H10O H20

Molecular

Weight

112.22 g/mol 46.068 g/mol 74.12g/mol 18.02 g/mol

State Liquid Gas Liquid Liquid

Colour Colourless Colourless Colourless Colourless

Odour A petroleum

like odour

Ethereal Camphor Odourless

Density 0.7166 g/ml

at 20 °C

0.6683 g/ml

at 20 °C

0.786 g/ml at

20 °C

0.9980 g/ml

at 20 °C

Melting Point -101 °C -141.5 °C 25.7°C 0oC

Boiling Point 102 °C -24.8 °C 82.41°C 100°C

Refractive

Index

1.411

at 20 °C

1.3330

at 20 °C

1.3689

at 20 °C

1.3330

at 20 °C

Water

Solubility

2.3 mg/l

at 25°C

45.6 g/l

At 25°C

Miscible -

159

MSDS of All Chemical Components in Process

1) Methyl tert-butyl ether [65]

Table 42: MSDS of Methyl Tert-Butyl Ether

Identification

Name Methyl tert-butyl ether

Hazards Identification

Potential Acute Health

Effects

Extremely hazardous in case of eye contact (irritant), of

ingestion. Very hazardous in case of skin contact (irritant), of

inhalation. Hazardous in case of skin contact. Inflammation of

the eye is characterized by redness, watering, and itching.

Skin inflammation is characterized by itching, scaling,

reddening, or, occasionally, blistering.

Potential Chronic Health

Effects

Extremely hazardous in case of eye contact (irritant), of

ingestion. Very hazardous in case of skin contact (irritant), of

inhalation. Hazardous in case of skin contact (permeator).

- CARCINOGENIC EFFECTS: Not available.

- MUTAGENIC EFFECTS: Not available.

- TERATOGENIC EFFECTS: Not available.

- - DEVELOPMENTAL TOXICITY: Not available.

The substance is toxic to lungs, the nervous system,

mucous membranes. Repeated or prolonged exposure

to the substance can produce target organs damage.

Repeated or prolonged inhalation of vapors may lead

to chronic respiratory irritation.

Eye Contact

Check for and remove any contact lenses. Immediately flush

eyes with running water for at least 15 minutes, keeping

eyelids open. Cold water may be used. Do not use an eye

ointment.

Skin Contact

After contact with skin, wash immediately with plenty of

water. Gently and thoroughly wash the contaminated skin

with running water and non-abrasive soap. Be particularly

careful to clean folds, crevices, creases and groin. Cold water

may be used. Cover the irritated skin with an emollient. Wash

160

contaminated clothing before reusing.

Serious Skin Contact Wash with a disinfectant soap and cover the contaminated

skin with an anti-bacterial cream. Seek medical attention.

Inhalation Allow the victim to rest in a well ventilated area. Seek

immediate medical attention.

Serious Inhalation

Evacuate the victim to a safe area as soon as possible. Loosen

tight clothing such as a collar, tie, belt or waistband. If

breathing is difficult, administer oxygen. If the victim is not

breathing, perform mouth-to-mouth resuscitation. Seek

medical attention.

Ingestion

Do not induce vomiting. Loosen tight clothing such as a

collar, tie, belt or waistband. If the victim is not breathing,

perform mouth-to-mouth resuscitation. Seek immediate

medical attention.

Serious Ingestion Not available

Fire and Explosion Data

Flammability Of the

Product

Flammable

Auto-Ignition

Temperature

224°C (435.2°F)

Flash Points CLOSED CUP: -28°C (-18.4°F)

Flammable Limits LOWER: 2.5% UPPER: 15.1%

Products of Combustion These products are carbon oxides (CO, CO2)

Fire Hazards in Presence

of Various Substances

Flammable in presence of open flames and sparks.

Explosion Hazards in

Presence of Various

Substances

Risks of explosion of the product in presence of mechanical

impact: Not available. Risks of explosion of the product in

presence of static discharge: Not available

Fire Fighting Media and

Instructions

Flammable liquid, soluble or dispersed in water. SMALL

FIRE: Use DRY chemical powder. LARGE FIRE: Use

alcohol foam, water spray or fog.

Special Remarks on Fire

Hazards

Not available.

Special Remarks on Not available

161

Explosion Hazards

Accidental Release Measures

Small Spill Dilute with water and mop up, or absorb with an inert dry

material and place in an appropriate waste disposal container

Large Spill

Flammable liquid. Keep away from heat. Keep away from

sources of ignition. Stop leak if without risk. Absorb with

DRY earth, sand or other non-combustible material. Do not

touch spilled material. Prevent entry into sewers, basements or

confined areas; dike if needed. Eliminate all ignition sources.

Exposure Controls/Personal Protection

Engineering Controls

Provide exhaust ventilation or other engineering controls to

keep the airborne concentrations of vapors below their

respective threshold limit value. Ensure that eyewash stations

and safety showers are proximal to the work-station location.

Personal Protection Splash goggles. Lab coat. Vapor respirator. Be sure to use an

approved/certified respirator or equivalent. Gloves.

Personal Protection in

Case of a Large Spill

Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A

self-contained breathing apparatus should be used to avoid

inhalation of the product. Suggested protective clothing might

not be sufficient; consult a specialist BEFORE handling this

product

Physical and Chemical Properties

Physical state and

appearance

Liquid

Odour Characteristic

Taste Not available

Molecular Weight 88.15 g/mole

Colour Clear Colourless

pH (1% soln/water) Not available.

Boiling Point 55.2°C (131.4°F)

Melting Point -109°C (-164.2°F)

Critical Temperature Not available

Specific Gravity 0.7405 (Water = 1)

162

Vapour Pressure 245 mm of Hg (@ 20°C)

Vapour Density 3.1 (Air = 1)

Volatility 100% (v/v)

Odour Threshold Not available

Water/Oil Dist. Coeff. Not available

Iconicity (in Water) Not available

Dispersion Properties See solubility in water, methanol, diethyl ether

Solubility Soluble in methanol, diethyl ether. Partially soluble in cold

water

Stability and Reactivity Data

Stability The product is stable.

Instability Temperature Not available.

Conditions of Instability Not available.

Incompatibility with

various substances

Not available.

Corrosivity Non-corrosive in presence of glass

Special Remarks on

Reactivity

Not available.

Special Remarks on

Corrosivity

Not available.

Polymerization

No

Toxicological Information

Routes of Entry Dermal contact. Eye contact. Inhalation. Ingestion.

Toxicity to Animals

WARNING: THE LC50 VALUES HEREUNDER ARE

ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE.

Acute oral toxicity (LD50): 4000 mg/kg [Rat]. Acute toxicity

of the vapour (LC50): 23576 ppm 4 hour(s) [Rat].

Chronic Effects on

Humans

The substance is toxic to lungs, the nervous system, mucous

membranes.

Other Toxic Effects on

Humans

Extremely hazardous in case of ingestion. Very hazardous in

case of skin contact (irritant), of inhalation. Hazardous in case

163

of skin contact (permeator).

Special Remarks on

Toxicity to Animals

Not available.

Special Remarks on

Chronic Effects on

Humans

Not available.

Special Remarks on other

Toxic Effects on Humans

Not available.

Ecological Information

Ecotoxicity Not available

BOD5 and COD Not available

Products of

Biodegradation

Possibly hazardous short term degradation products are not

likely. However, long term degradation products may arise.

Toxicity of the Products

of Biodegradation

The products of degradation are more toxic.

Special Remarks on the

Products of

Biodegradation

Not available.

Transport Information

DOT Classification Class 3: Flammable liquid

Identification Methyl tert-butyl ether : UN2398 PG: II

Special Provisions for

Transport

Not available.

164

Other Regulatory Information

Federal and State

Regulations

Pennsylvania RTK: Methyl tert-butyl ether Massachusetts

RTK: Methyl tert-butyl ether TSCA 8(b) inventory: Methyl

tert-butyl ether SARA 313 toxic chemical notification and

release reporting: Methyl tert-butyl ether CERCLA:

Hazardous substances.

Methyl tert-butyl ether

Other Regulations OSHA: Hazardous by definition of Hazard Communication

Standard (29 CFR 1910.1200)

WHMIS (Canada)

CLASS B-2: Flammable liquid with a flash point lower than

37.8°C (100°F). CLASS D-2A: Material causing other toxic

effects

(VERY TOXIC).

DSCL (EEC) R11- Highly flammable. R38- Irritating to skin. R41- Risk of

serious damage to eyes

HMIS (U.S.A.) Health Hazard: 2

Fire Hazard: 3

Reactivity: 0

Personal Protection: h

National Fire Protection

Association (U.S.A.)

Health: 2

Flammability: 3

Reactivity: 0

Protective Equipment

Gloves. Lab coat. Vapour respirator. Be sure to use an

approved/certified respirator or equivalent. Wear appropriate

respirator when ventilation is inadequate. Splash goggles.

Other Information

References Not available

Other Special

Considerations

Not available

Created 10/10/2005 08:23 PM

Last Updated 05/21/2013 12:00 PM

165

2) Methanol [69]

Table 43: MSDS of Methanol

Identification

Product Name Methanol

Recommended Use Solvent, fuel, feedstock

Hazard identification

Emergency Overview

Colourless liquid, with a mild, characteristic alcohol odour

when pure. Readily absorbs moisture.

Flammable liquid and

vapour

Burns with a clean, clear flame, which is almost invisible in

daylight, or a light blue flame. Can decompose at high

temperatures forming carbon monoxide and formaldehyde.

Confined space hazard.

Toxic

May be harmful if inhaled, absorbed through the skin or

swallowed. Mild central nervous system depressant. May

cause headache, nausea, dizziness, drowsiness, and

incoordination. Severe vision effects, including increased

sensitivity to light, blurred vision, and blindness may develop

following an 8-24 hour symptom-free period. Coma and death

may result.

Irritant Causes eye irritation

Possible teratogen/embryo

toxin

May harm the unborn child, based on animal information.

Potential Health Effects

Inhalation

Causes mild central nervous system (CNS) depression with

nausea, headache, vomiting, dizziness, incoordination and an

appearance of drunkenness. Metabolic acidosis and severe

visual effects can occur following an 8-24 hour latent period.

Coma and death, usually due to respiratory failure, may occur

if medical treatment is not received. Visual effects may

include reduced reactivity and/or increased sensitivity to light,

blurred, double and/or snowy vision, and blindness.

166

Eye Contact Moderate eye irritant

Skin Contact

In general, primary alcohols such as methanol are not

considered to be irritant to the skin. Repeated or prolonged

exposure to methanol may cause dry, itchy, scaling skin

(dermatitis).

Skin Absorption Can be absorbed through the skin and cause harmful effects as

described in “Inhalation” above.

Skin Sensitization Not considered to be a sensitizer.

Respiratory Sensitization Not considered to be a sensitizer.

Ingestion

There have been reports of accidental or intentional ingestion

of methanol although ingestion is not a typical route of

occupational exposure. Ingestion of as little as 10 ml of

methanol can cause blindness and 30 ml (1 ounce) can cause

death if victim is not treated. Ingestion causes mild central

nervous system (CNS) depression with nausea, headache,

vomiting, dizziness, incoordination and an appearance of

drunkenness. Metabolic acidosis and severe visual effects can

occur following an 8-24 hour latent period. Coma and death,

usually due to respiratory failure, may occur if medical

treatment is not received. Visual effects may include reduced

reactivity and/or increased sensitivity to light, blurred, double

and/or snowy vision, and blindness.

Birth

Defects/Developmental

Effects

Caused teratogenic and fetotoxic effects, in the absence of

maternal toxicity in animal studies.

Reproductive Effects Not considered a reproductive toxin

First-aid Measures

Inhalation

Methanol is toxic and flammable. Take proper precautions to

ensure your own safety before attempting rescue (e.g. wear

appropriate protective equipment and remove any sources of

ignition). Remove source of contamination or move victim to

fresh air, provide oxygen therapy if available. Immediately

transport victim to an emergency care facility.

Avoid direct contact. Wear chemical protective clothing, if

necessary. As quickly as possible, remove contaminated

167

Skin Contact

clothing, shoes and leather goods (e.g. watchbands, belts).

Immediately flush with lukewarm, gently flowing water for

15-20 minutes. Immediately obtain medical attention.

Completely decontaminate clothing, shoes and leather goods

before re-use or discard.

Eye Contact

Avoid direct contact. Wear chemical protective goggles, if

necessary. Immediately flush the contaminated eye(s) with

lukewarm, gently flowing water for 15-20 minutes, while

Methanol Material Safety Data Sheet

Methanex Corporation - 3 - July 11, 2013

Holding the eyelid(s) open. If a contact lens is present, Do not

delay irrigation or attempt to remove the lens until flushing is

done. Take care not to rinse contaminated water into the

unaffected eye or onto the face. Immediately obtain medical

attention.

Ingestion

Never give anything by mouth if victim is rapidly losing

consciousness, is unconscious or convulsing. Have victim

rinse mouth thoroughly with water. Do not induce vomiting.

If vomiting occurs naturally, have victim rinse mouth with

water again. Quickly transport victim to an emergency care

facility

First Aid Comments

Provide general supportive measures (comfort, warmth, rest).

Consult a physician and/or the nearest Poison Control Centre

for all exposures. All first-aid procedures should be

periodically reviewed by a physician familiar with the

material and its conditions of use in the workplace

Note to Physicians

The severity of outcome following methanol ingestion may be

more related to the time between ingestion and treatment,

rather than the amount ingested. Therefore, there is a need for

rapid treatment of any ingestion exposure. Both ethanol and

fomepizole are effective antidotes for methanol poisoning,

although fomepizole is preferred.

168

Fire-fighting Measures

Suitable Extinguishing

Media

Synthetic Firefighting foam AR-FFF (3% solution), carbon

dioxide, dry chemical powder, water spray or fog. Water may

be effective for cooling, diluting, or dispersing methanol, but

may not be effective for extinguishing a fire because it will

not cool methanol below its flash point. Fire-fighting foams,

such as multipurpose alcohol-resistant foams, are

recommended for most flammable liquid fires. If water is used

for cooling, the solution will spread if not contained. Mixtures

of methanol and water at concentrations greater than 20%

methanol can burn.

Hazardous Combustion

Products

During a fire, carbon monoxide, carbon dioxide and irritating

and toxic gases such as formaldehyde may be generated.

Unusual Fire and

Explosion Hazards

Can accumulate in confined spaces, resulting in a toxicity and

flammability hazard. Closed containers may rupture violently

and suddenly release large amounts of product when exposed

to fire or excessive heat for a sufficient period of time. Flame

may be invisible during the day. The use of infrared and or

heat detection devices is recommended.

Fire-Fighting Procedures

Evacuate area and fight fire from a safe distance or protected

location. Approach fire from upwind. Cool fire-exposed

containers, tanks or equipment by applying hose streams.

Special Protective

Equipment for

Firefighters

Full face, positive pressure, self-contained breathing apparatus

(NIOSH approved or equivalent) or airline and appropriate

chemical protective fire-fighting clothing.

Accidental Release Measures

Personal Precautions,

Protective Equipment and

Emergency Procedures

Restrict access to area until completion of cleanup. Ensure

cleanup is conducted by trained personnel only. Wear

adequate personal protective equipment. Extinguish or

remove all sources of ignition. Notify government

occupational health and safety and environmental authorities.

Do not touch spilled material. Prevent material from entering

sewers, waterways or confined spaces. Stop or reduce leak if

safe to do so. Contain spill with earth, sand, or absorbent

169

Methods and Materials for

Containment and

Cleaning up

material which does not react with spilled

Methanol Material Safety Data Sheet

Methanex Corporation - 4 - July 11, 2013 material. Remove

liquid by intrinsically safe pumps or vacuum equipment

designed for vacuuming flammable materials (i.e. equipped

with inert gases and ignition sources controlled). Place in

suitable, covered, labelled containers. SMALL SPILLS: Soak

up spill with absorbent material which does not react with

spilled chemical. Put material in suitable, covered, labelled

containers. Flush area with water. Contaminated absorbent

material may pose the same hazards as the spilled product.

LARGE SPILLS: If necessary, contain spill by diking.

Alcohol resistant foams may be applied to spill to diminish

vapour and fire hazard. Collect liquid with explosion proof

pumps.

Handling and Storage

Precautions for Handling

No smoking or open flame in storage, use or handling areas.

Use explosion proof electrical equipment. Ensure proper

electrical grounding and bonding equipment procedures are in

place.

Storage

Store this material in a cool, dry, well-ventilated area away

from oxidizing materials and corrosive atmospheres, in a

fireproof area. Keep amount in storage to a minimum. Storage

area should be clearly identified, clear of obstruction and

accessible only to trained and authorized personnel. It is

recommended that storage procedures be evaluated using

NFPA 70E standard and NFPA 497 practice. Do not store

below ground level, or in confined spaces. Have appropriate

fire extinguishers and spill cleanup equipment in or near

storage area. Store away from strong oxidizers, mineral acids

and metals. See Section 10, Stability and reactivity for more

information. Ground and bond all containers and storage

vessels. Store away from heat and ignition sources and out of

direct sunlight. Post storage area as a “No Smoking” area.

170

Exposure Controls/Personal Protection

Exposure Limits

ACGIH

Time-Weighted Average (TLV-TWA): 200 ppm - Skin

Short-Term Exposure Limit (TLV-STEL): 250 ppm - Skin

TLV Basis - Critical Effect(s):

Headache, Eye damage, Dizziness, Nausea

Eye/face Protection Chemical safety goggles. A face shield may also be necessary

Skin Protection

Chemical protective gloves, coveralls, boots, and/or other

chemical protective clothing. Safety shower/eye-wash

fountain should be readily available in the immediate work

area.

Hand protection

Since methanol is recognized as a skin absorption hazard,

check with glove manufacturers for appropriate glove

material, thickness and resistance to breakthrough.

Respiratory Protection

Respiratory protection should be worn when there is a

potential to exceed the exposure limit requirements or

guidelines. Use an approved positive-pressure full face self-

contained breathing apparatus or a full-face supplied air

respirator. The person wearing the respirator should be

medically approved, fit tested and trained to operate the

breathing apparatus.

Ventilation

Engineering methods to control hazardous conditions are

preferred. Methods include mechanical (local exhaust)

ventilation, process or personnel enclosure and control of

process conditions. Administrative controls and personal

protective equipment may also be required. Because of the

high potential hazard associated with this substance, stringent

control measures such as enclosure (closed handling systems)

should be considered. To reduce the fire/explosion hazard,

consider the use of an inert gas in the process system. Use

approved explosion-proof equipment and intrinsically safe

electrical systems in areas of use. For large-scale operations,

consider the installation of leak and fire detection equipment

along with a suitable, automatic fire suppression system. Use

a non-sparking, grounded, ventilation system separate from

other exhaust ventilation systems. Exhaust directly to the

171

outside. Supply sufficient replacement air to make up for air

removed by exhaust system.

Physical and Chemical Properties

Appearance Liquid, clear, colourless

Odour Mild characteristic alcohol odour

Odour Threshold

detection: 4.2 - 5960 ppm

(geometric mean) 160 ppm

recognition: 53 – 8940 ppm

(geometric mean) 690 ppm

pH Not applicable

Freezing Point 97.8°C

Boiling Point 64.7°C

Boiling Range Not determined

Flash Point 11.0oC

Solubility Completely soluble

Partial Coefficient Log P (oct) = -0.82

Vapour Pressure 12.8 kPa @ 20°C

Viscosity 0.3 cP@ 25°C

Upper Explosive Limit

(UEL)

36.5 %

Lower Explosive Limit

(LEL)

6%

Auto Ignition

Temperature

464°C

Solvent Solubility

Soluble in all proportions in ethanol, benzene, other alcohols,

chloroform, diethyl ether, other ethers, esters, ketones and

most organic solvents

Critical Temperature 239.4°C

Specific Gravity 0.791-0.793 @ 20°C

Evaporation Rate 4.1 (n-butyl acetate =1)

Vapour Density 1.105 @ 15°C (air = 1)

Decomposition

Temperature

Not determined

Sensitivity to Impact No

172

Sensitivity to Static

Charge

Low

Percent Volatility 100

Stability and Reactivity

Chemical Stability Stable as supplied.

Possibility of Hazardous

Reactions

Polymerization will not occur.

Conditions to Avoid

Heat, open flames, static discharge, sparks and other ignition

sources.

Incompatible Materials

Avoid contact with strong oxidizers, strong mineral or organic

acids, and strong bases. Contact with these materials may

cause a violent or explosive reaction. Methanol is not

compatible with gasket and O-rings materials made of Buna-

N and Nitrile. Methanol is corrosive to type 12L14 carbon

steel at room temperature and type 3003 aluminium, copper

(10-100% methanol solution) and admiralty brass, at 93 deg

C. Methanol is not corrosive to most metals. Methanol

attacks some forms of plastic, rubber and coatings.

Hazardous Decomposition

Products

Decomposes on heating to produce carbon monoxide and

formaldehyde.

Toxicological Information

Ingestion LD50 (oral, rat): 5600 mg/kg

LD50 (oral, rabbit): 14200 mg/kg

Dermal LD50 (dermal, rabbit): 15800 mg/kg

Inhalation

LC50 (rabbit): 81000 mg/m3/14h

LC50 (rat): 64000 ppm/4h

Eye Damage/Irritation Moderate eye irritant.

Skin Corrosion/Irritation Not considered to be an irritant.

Sensitization Not considered to be a sensitizer

Repeated Dose Toxicity No relevant data found

Chronic Toxicity and Not listed by IARC, NTP, ACGIH OR OSHA as a carcinogen

173

Carcinogenicity

Teratogenicity,

Embryotoxicity and/or

Fetotoxicity

Methanol has produced fetotoxicity in rats and teratogenicity

in mice exposed by inhalation to high concentrations that did

not produce significant maternal toxicity

Reproductive Toxicity Not considered to be a reproductive toxin.

Mutagenicity There is insufficient information available to conclude that

methanol is mutagenic.

Ecological Information

Persistence and

degradability

Readily biodegradable

Bioaccumulation Does not bioaccumulation. Partition coefficient: n-

octanol/water 0.77

Mobility in Soil Mobile in soils

PBT/vPvB

This substance is not considered to be persistent, bio

accumulating nor toxic (PBT). This substance is not

considered to be very persistent nor very bio accumulating

(vPvB).

Terrestrial Fate

The mobility of methanol in the subsurface will not be

significantly limited by adsorption. Sorption of methanol to

organic carbon in soil will be minor, and methanol will tend to

remain in soil pore water.

Aquatic Fate

Methanol is completely miscible with water. Accordingly, its

mobility in the subsurface will not be limited by solubility.

Methanol has been shown to undergo rapid biodegradation in

a variety of screening studies using sewage seed and activated

sludge inoculum, which suggests that biodegradation will

occur in aquatic environments where the concentration does

not inhibit bacterial activity

Atmospheric Fate

Methanol has a vapour pressure of 127 mm Hg at 25°C and is

expected to exist solely as a vapour in the ambient

atmosphere. Vapour-phase methanol is degraded in the

174

atmosphere by reaction with photo chemically-produced

hydroxyl radicals; the half-life for this reaction in air is

estimated to be 17 days.

Other Adverse Effects Do not flush into surface water or sanitary sewer system.

Disposal Considerations

Handling and storage

Disposal by controlled incineration or by secure land fill may

be acceptable. Recycle wherever possible. Large volumes

may be suitable for re-distillation or, if contaminated,

incineration. Can be disposed of in a sewage treatment

facility. Methanol levels of up to 0.1% act as a food source for

bacteria; above this level may be toxic to bacteria. When

pumping through sewage collection systems, the level of

methanol should be kept below the flammable range (a 25%

methanol/water mixture is non-flammable at temperatures

below 39°C). 1 ppm of methanol is equivalent to 1.5 ppm

BOD loading in the sewage plant.

Container disposal

Empty containers may contain hazardous residue. Return to

supplier for reuse if possible. Never weld, cut or grind empty

containers. If disposing of containers, ensure they are well

rinsed with water, then disposed of at an authorized landfill.

After cleaning, all existing labels should be removed.

Regulatory Information (Canadian Federal Regulations)

Hazardous Products Act

Information: CPR

Compliance

This product has been classified in accordance with the hazard

criteria of the Canadian Controlled Products Regulations

(CPR) and the MSDS contains all the information required by

the CPR

WHMIS Classification

B2 - Flammable and combustible material - Flammable liquid

D1B - Poisonous and infectious material - Immediate and

serious effects - Toxic D2A - Poisonous and infectious

material - Other effects - Very toxic D2B - Poisonous and

infectious material - Other effects - Toxic

175

CEPA, Domestic

Substances List

Methanol is listed on the Domestic Substances List.

WHMIS Ingredient

Disclosure List

Listed at 1%

Other Information

References SAX, N.I. Dangerous Properties of Indutrial Materials.

Toronto, Van Nostrand Reinold, 6e ed. 1984. -Material safety

Data sheet emitted by: la Commission de la Santé et de la

Sécurité du Travail du Québec. -Hawley, G.G... The

Condensed Chemical Dictionary, 11e ed., New York N.Y.,

Van Nostrand Reinold, 1987. LOLI, HSDB, RTECS,

HAZARDTEXT,

REPROTOX databases

Other Special

Considerations

Not available

Created 10/10/2005 08:23 PM

Last Updated 05/21/2013 12:00 PM

3) Isobutylene [70]

Table 44: MSDS of Isobutylene

Identification

Name Isobutylene

Formula C4H8 / CH2=C(CH3)2

Other means of

identification

Isobutene

Hazards Identification

Signal word (GHS-US) DANGER

Hazard statements (GHS-

US)

H220 - EXTREMELY FLAMMABLE GAS

H280 - CONTAINS GAS UNDER PRESSURE; MAY

EXPLODE IF HEATED

OSHA-H01 - MAY DISPLACE OXYGEN AND CAUSE

RAPID SUFFOCATION.

176

CGA-HG04 - MAY FORM EXPLOSIVE MIXTURES WITH

AIR CGA-HG01 - MAY CAUSE FROSTBITE

Precautionary statements

(GHS-US)

P202 - Do not handle until all safety precautions have been

read and understood

P210 - Keep away from Heat, Open flames, Sparks, Hot

surfaces. - No smoking

P271+P403 - Use and store only outdoors or in a well-

ventilated place.

P377 - Leaking gas fire: Do not extinguish, unless leak can be

stopped safely

P381 - Eliminate all ignition sources if safe to do so

CGA-PG05 - Use a back flow preventive device in the piping.

CGA-PG12 - Do not open valve until connected to equipment

prepared for use.

CGA-PG06 - Close valve after each use and when empty.

CGA-PG11 - Never put cylinders into unventilated areas of

passenger vehicles.

CGA-PG02 - Protect from sunlight when ambient temperature

exceeds 52°C (125°F).

First Aid Measures

First-aid measures after

inhalation

Immediately remove to fresh air. If not breathing, give

artificial respiration. If breathing is difficult, qualified

personnel may give oxygen. Call a physician.

First-aid measures after

skin contact

For exposure to liquid, immediately warm frostbite area with

warm water not to exceed 105°F (41°C). Water temperature

should be tolerable to normal skin. Maintain skin warming for

at least 15 minutes or until normal colouring and sensation

have returned to the affected area. In case of massive

exposure, remove clothing while showering with warm water.

Seek medical evaluation and treatment as soon as possible

First-aid measures after

eye contact

Immediately flush eyes thoroughly with water for at least 15

minutes. Hold the eyelids open and away from the eyeballs to

ensure that all surfaces are flushed thoroughly. Contact an

ophthalmologist immediately.

177

First-aid measures after

ingestion

Ingestion is not considered a potential route of exposure.

Firefighting measures

Suitable extinguishing

media

Carbon dioxide, Dry chemical, Water spray or fog.

Fire hazard

EXTREMELY FLAMMABLE GAS. If venting or leaking

gas catches fire, do not extinguish flames. Flammable vapors

may spread from leak, creating an explosive reignition hazard.

Vapors can be ignited by pilot lights, other flames, smoking,

sparks, heaters, electrical equipment, static discharge, or other

ignition sources at locations distant from product handling

point. Explosive atmospheres may linger. Before entering an

area, especially a confined area, check the atmosphere with an

appropriate device.

Explosion hazard EXTREMELY FLAMMABLE GAS. Forms explosive

mixtures with air and oxidizing agents.

Reactivity No reactivity hazard other than the effects described in sub-

sections below.

Firefighting instructions

DANGER: FLAMMABLE LIQUID AND VAPOR. Evacuate

all personnel from danger area. Use self-contained breathing

apparatus. Immediately cool surrounding containers with

water spray from maximum distance, taking care not to

extinguish flames. Avoid spreading burning liquid with water.

Remove ignition sources if safe to do so. If flames are

accidentally extinguished, explosive reigniting may occur.

Reduce vapors with water spray or fog. Stop flow of liquid if

safe to do so, while continuing cooling water spray. Remove

all containers from area of fire if safe to do so. Allow fire to

burn out. On-site fire brigades must comply with OSHA 29

CFR 1910.156 and applicable standards under 29 CFR 1919

Subpart L - Fire Protection

Special protective

equipment for fire fighters

Standard protective clothing and equipment (Self Contained

Breathing Apparatus) for fire fighters

Other information Containers are equipped with a pressure relief device.

178

(Exceptions may exist where authorized by DOT.).

Accidental Release Measures

General measures

DANGER: Flammable liquid and gas under pressure. Forms

explosive mixtures with air. Immediately evacuate all

personnel from danger area. Use self-contained breathing

apparatus where needed. Remove all sources of ignition if

safe to do so. Reduce vapors with fog or fine water spray,

taking care not to spread liquid with water. Shut off flow if

safe to do so. Ventilate area or move container to a well-

ventilated area. Flammable vapors may spread from leak and

could explode if reignited by sparks or flames. Explosive

atmospheres may linger. Before entering area, especially

confined areas, check atmosphere with an appropriate device.

Handling and storage

Precautions for safe

handling

Keep away from heat, hot surfaces, sparks, open flames and

other ignition sources. No smoking. Use only non-sparking

tools. Use only explosion-proof equipment. Wear leather

safety gloves and safety shoes when handling cylinders.

Protect cylinders from physical damage; do not drag, roll,

slide or drop. While moving cylinder, always keep in place

removable valve cover. Never attempt to lift a cylinder by its

cap; the cap is intended solely to protect the valve. When

moving cylinders, even for short distances, use a cart (trolley,

hand truck, etc.) designed to transport cylinders. Never insert

an object (e.g., wrench, screwdriver, and pry bar) into cap

openings; doing so may damage the valve and cause a leak.

Use an adjustable strap wrench to remove over-tight or rusted

caps. Slowly open the valve. If the valve is hard to open,

discontinue use and contact your supplier. Close the container

valve after each use; keep closed even when empty. Never

apply flame or localized heat directly to any part of the

container. High temperatures may damage the container and

could cause the pressure relief device to fail prematurely,

venting the container contents. For other precautions in using

179

this product, see section 16.

Storage conditions

Store only where temperature will not exceed 125°F (52°C).

Post “No Smoking or Open Flames” signs in storage and use

areas. There must be no sources of ignition. Separate

packages and protect against potential fire and/or explosion

damage following appropriate codes and requirements (e.g.,

NFPA 30, NFPA 55, NFPA 70, and/or NFPA 221 in the U.S.)

or according to requirements determined by the Authority

Having Jurisdiction (AHJ). Always secure containers upright

to keep them from falling or being knocked over. Install valve

protection cap, if provided, firmly in place by hand when the

container is not in use. Store full and empty containers

separately. Use a first-in, first-out inventory system to prevent

storing full containers for long periods. For other precautions

in using this product, see section 16. OTHER

PRECAUTIONS FOR HANDLING, STORAGE, and USE:

When handling product under pressure, use piping and

equipment adequately designed to withstand the pressures to

be encountered. Never work on a pressurized system. Use a

back flow preventive device in the piping. Gases can cause

rapid suffocation because of oxygen deficiency; store and use

with adequate ventilation. If a leak occurs, close the container

valve and blow down the system in a safe and

environmentally correct manner in compliance with all

international, federal/national, state/provincial, and local laws;

and then repair the leak. Never place a container where it may

become part of an electrical circuit.

Exposure controls/personal protection

Appropriate engineering

controls

Use an explosion-proof local exhaust system. Local exhaust

and general ventilation must be adequate to meet exposure

standards. MECHANICAL (GENERAL): Inadequate - Use

only in a closed system. Use explosion proof equipment and

lighting.

Eye protection

: Wear safety glasses when handling cylinders; vapor-proof

goggles and a face shield during cylinder change out or

180

whenever contact with product is possible. Select eye

protection in accordance with OSHA 29 CFR 1910.133.

Skin and body protection

Wear metatarsal shoes and work gloves for cylinder handling,

and protective clothing where needed. Wear neoprene gloves

during cylinder change out or wherever contact with product

is possible. Select per OSHA 29 CFR 1910.132, 1910.136,

and 1910.138.

Respiratory protection

When workplace conditions warrant respirator use, follow a

respiratory protection program that meets OSHA 29 CFR

1910.134, ANSI Z88.2, or MSHA 30 CFR 72.710 (where

applicable). Use an air-supplied or air-purifying cartridge if

the action level is exceeded. Ensure that the respirator has the

appropriate protection factor for the exposure level. If

cartridge type respirators are used, the cartridge must be

appropriate for the chemical exposure (e.g., an organic vapor

cartridge). For emergencies or instances with unknown

exposure levels, use a self-contained breathing apparatus

(SCBA).

Thermal hazard protection Wear cold insulating gloves when trans filling or breaking

transfer connections.

Physical and chemical properties

Physical state Gas

Molecular mass 56 g/mol

Colour colourless

Odour Sweetish

Odour threshold Odour threshold is subjective and inadequate to warn for

overexposure

pH

Not applicable

Relative evaporation rate

(butyl acetate=1)

No data available

Relative evaporation rate

(ether=1)

Not applicable

181

Melting point 140.3 °C

Freezing point No data available

Boiling point -6.9 °C

Flash point -80 °C (closed cup)

Critical temperature 144 °C

Auto-ignition

temperature

465 °C

Decomposition

temperature

No data available

Flammability (solid, gas) 1.8 - 8.8 vol %

Vapour pressure 260 kPa

Critical pressure 4000 kPa

Relative vapor density at

20 °C

No data available

Specific gravity / density 0.599 g/cm³ (at 20 °C)

Relative gas density 2

Solubility Water: 388 mg/l

Log Pow 2.35

Log Kow Not applicable

Viscosity, kinematic Not applicable

Viscosity, dynamic Not applicable

Explosive properties Not applicable

Oxidizing properties None

Explosive limits No data available

Gas group Liquefied gas

Additional information Gas/vapour heavier than air. May accumulate in confined

spaces, particularly at or below ground level.

Stability and Reactivity

Reactivity No reactivity hazard other than the effects described in sub-

sections below

Chemical stability Stable under normal conditions

Possibility of hazardous

reactions

May occur

Conditions to avoid High temperature. Catalyst.

182

Incompatible materials Halogens. Oxidizing agents. Acids.

Hazardous decomposition

products

Thermal decomposition may produce: Carbon monoxide.

Carbon dioxide.

Toxicological information

Acute toxicity Not classified

Isobutylene ( \f )115-11-7

LC50 inhalation rat (mg/l) 620 mg/l/4h

LC50 inhalation rat (ppm) ≥ 10000

ATE US (gases) 10000.000 ppm V/4h

ATE US (vapors) 620.000 mg/l/4h

ATE US (dust, mist) 620.000 mg/l/4h

Skin corrosion/irritation Not classified

Serious eye

damage/irritation

Not classified

pH Not applicable

Respiratory or skin

sensitization

Not classified

Germ cell mutagenicity Not classified

Carcinogenicity Not classified

Reproductive toxicity Not classified

Specific target organ

toxicity (single exposure)

Not classified

Specific target organ

toxicity (repeated

exposure

Not classified

Aspiration hazard Not classified

Ecological information

Ecology

general

No known ecological damage caused by this product.

Persistence and

degradability

Isobutylene (115-11-7)

Persistence and degradability The substance is biodegradable.

Bio accumulative

potential

Isobutylene (115-11-7)

Log Pow = 2.35

Log Kow = Not applicable.

183

Bio accumulative potential is not expected to bio accumulate

due to the low log Kow (log Kow < 4). Refer to section 9

Mobility in soil

Isobutylene (115-11-7)

Mobility in soil = No data available.

Ecology - soil Because of its high volatility, the product is

unlikely to cause ground or water pollution.

Other adverse effects

Effect on ozone layer: None.

Effect on the global warming: No known effects from this

product.

Disposal considerations

Waste disposal

recommendations

Do not attempt to dispose of residual or unused quantities.

Return container to supplier.

Transport information

Proper Shipping Name

(DOT)

Isobutylene

Department of

Transportation (DOT)

Hazard Classes

2.1 - Class 2.1 - Flammable gas 49 CFR 173.115

Hazard labels (DOT) 2.1 - Flammable gas

DOT Special Provisions

(49 CFR 172.102)

19 - For domestic transportation only, the identification

number UN1075 may be used in place of the identification

number specified in column (4) of the 172.101 table. The

identification number used must be consistent on package

markings, shipping papers and emergency response

information. T50 - When portable tank instruction T50 is

referenced in Column (7) of the 172.101 Table, the applicable

liquefied compressed gases are authorized to be transported in

portable tanks in accordance with the requirements of 173.313

of this subchapter.

Special transport

precautions

Avoid transport on vehicles where the load space is not

separated from the driver's compartment. Ensure vehicle

driver is aware of the potential hazards of the load and knows

what to do in the event of an accident or an emergency.

184

Before transporting product containers: - Ensure there is

adequate ventilation. - Ensure that containers are firmly

secured. - Ensure cylinder valve is closed and not leaking. -

Ensure valve outlet cap nut or plug (where provided) is

correctly fitted. - Ensure valve protection device (where

provided) is correctly fitted.

Transport by sea

UN-No. (IMDG) : 1055

Proper Shipping Name (IMDG) :

ISOBUTYLENE Class (IMDG) : 2

Gases MFAG-No : 115

Air transport

UN-No.(IATA) : 1055

Proper Shipping Name (IATA) : Isobutylene

Class (IATA) : 2

Civil Aeronautics Law : Gases under pressure/Gases

flammable under pressure

Regulatory information

US Federal regulations

Listed on the United States TSCA (Toxic Substances Control

Act) inventory

SARA Section 311/312 Hazard Classes - Immediate

(acute) health hazard, Delayed (chronic) health hazard,

Sudden release of pressure hazard, Fire hazard

US State regulations

U.S. - California - Proposition 65 - Carcinogens List = No

U.S. - California - Proposition 65 - Developmental Toxicity =

No

U.S -California-Proposition 65 - Reproductive Toxicity -

Female = No

U.S. - California - Proposition 65 - Reproductive Toxicity –

Male = No

State or local regulations 1) U.S. - Massachusetts - Right To

Know List

2) U.S. - New Jersey - Right to

Know Hazardous Substance List

3) U.S. - Pennsylvania - RTK

(Right to Know) List

185

Other information When you mix two or more chemicals, you can create

additional, unexpected hazards. Obtain and evaluate the safety

information for each component before you produce the

mixture. Consult an industrial hygienist or other trained

person when you evaluate the end product. Before using any

plastics, confirm their compatibility with this product. Praxair

asks users of this product to study this SDS and become aware

of the product hazards and safety information. To promote

safe use of this product, a user should (1) notify employees,

agents, and contractors of the information in this SDS and of

any other known product hazards and safety information, (2)

furnish this information to each purchaser of the product, and

(3) ask each purchaser to notify its employees and customers

of the product hazards and safety information. The opinions

expressed herein are those of qualified experts within Praxair,

Inc. We believe that the information contained herein is

current as of the date of this Safety Data Sheet. Since the use

of this information and the conditions of use are not within the

control of Praxair, Inc., it is the user's obligation to determine

the conditions of safe use of the product. Praxair SDSs are

furnished on sale or delivery by Praxair or the independent

distributors and suppliers who package and sell our products.

To obtain current SDSs for these products, contact your

Praxair sales representative, local distributor, or supplier, or

download from www.praxair.com. If you have questions

regarding Praxair SDSs, would like the document number and

date of the latest SDS, or would like the names of the Praxair

suppliers in your area, phone or write the Praxair Call Center

(Phone: 1-800-PRAXAIR/1-800-772-9247; Address: Praxair

Call Center, Praxair, Inc., P.O. Box 44, Tonawanda, NY

14151-0044). PRAXAIR and the Flowing Airstream design

are trademarks or registered trademarks of Praxair

Technology, Inc. in the United States and/or other countries.

NFPA health hazard 2 - Intense or continued exposure could cause temporary

incapacitation or possible residual injury unless prompt

186

medical attention is given.

NFPA fire hazard 4 - Will rapidly or completely vaporize at normal pressure and

temperature, or is readily dispersed in air and will burn

readily.

NFPA reactivity 1 - Normally stable, but can become unstable at elevated

temperatures and pressures or may react with water with some

release of energy, but not violently.

HMIS III Rating Health : 1 Slight Hazard - Irritation or minor reversible injury

Possible Flammability : 4 Severe Hazard

Physical : 2 Moderate Hazard

Other information

References Not Available

Special Considerations Not available

Created 01/01/1979

Last Updated 27/2/2015

4) Diisobutylene [71]

Table 45: MSDS of Diisobutylene

Identification

Name Diisobutylene

Hazard Identification

Potential Acute Health

Effects

Very hazardous in case of eye contact (irritant). Hazardous in

case of skin contact (irritant). Slightly hazardous in case of

ingestion. Inflammation of the eye is characterized by redness,

watering, and itching.

Potential Chronic

Health Effects

CARCINOGENIC EFFECTS: Not available. MUTAGENIC

EFFECTS: Not available. TERATOGENIC EFFECTS: Not

available. DEVELOPMENTAL TOXICITY: Not available. The

substance is toxic to the nervous system. Repeated or prolonged

187

exposure to the substance can produce target organs damage.

First Aid Measures

Eye Contact Check for and remove any contact lenses. Do not use an eye

ointment. Seek medical attention

Skin Contact After contact with skin, wash immediately with plenty of water.

Gently and thoroughly wash the contaminated skin with running

water and non-abrasive soap. Be particularly careful to clean

folds, crevices, creases and groin. Cover the irritated skin with an

emollient. If irritation persists, seek medical attention. Wash

contaminated clothing before reusing.

Serious Skin Contact Wash with a disinfectant soap and cover the contaminated skin

with an anti-bacterial cream. Seek medical attention.

Inhalation Allow the victim to rest in a well ventilated area. Seek immediate

medical attention.

Serious Inhalation Evacuate the victim to a safe area as soon as possible. Loosen

tight clothing such as a collar, tie, belt or waistband. If breathing

is difficult, administer oxygen. If the victim is not breathing,

perform mouth-to-mouth resuscitation. Seek medical attention

Ingestion Do not induce vomiting. Loosen tight clothing such as a collar,

tie, belt or waistband. If the victim is not breathing, perform

mouth-to-mouth resuscitation. Seek immediate medical attention.

Serious Ingestion Not available.

Fire and Explosion Data

Flammability of the

Product

Flammable

Auto-Ignition

Temperature

305°C (581°F)

Flash Points CLOSED CUP: -8°C (17.6°F)

188

Flammable Limits LOWER: 0.7% UPPER: 5.6%

Products of

Combustion

These products are carbon oxides (CO, CO2)

Fire Hazards in

Presence of Various

Substances

Extremely flammable in presence of open flames and sparks.

Highly flammable in presence of heat.

Explosion Hazards in

Presence of Various

Substances

Risks of explosion of the product in presence of mechanical

impact: Not available. Risks of explosion of the product in

presence of static discharge: Not available.

Fire Fighting Media

and Instructions

Flammable liquid, insoluble in water. SMALL FIRE: Use DRY

chemical powder. LARGE FIRE: Use water spray or fog.

Special Remarks on

Fire Hazards

Not available

Special Remarks on

Explosion Hazards

Not available

Accidental Release Measures

Small Spill Absorb with an inert material and put the spilled material in an

appropriate waste disposal

Large Spill Flammable liquid, insoluble in water. Keep away from heat. Keep

away from sources of ignition. Stop leak if without risk. Absorb

with DRY earth, sand or other non-combustible material. Do not

get water inside container. Do not touch spilled material. Prevent

entry into sewers, basements or confined areas; dike if needed.

Eliminate all ignition sources. Call for assistance on disposal.

Handling and Storage

Precautions Keep away from heat. Keep away from sources of ignition.

Ground all equipment containing material. Do not breathe gas/

fumes/ vapour/spray. If you feel unwell, seek medical attention

and show the label when possible. Avoid contact with skin and

189

eyes

Storage Flammable materials should be stored in a separate safety storage

cabinet or room. Keep away from heat. Keep away from sources

of ignition. Keep container tightly closed. Keep in a cool, well-

ventilated place. Ground all equipment containing material. A

refrigerated room would be preferable for materials with a flash

point lower than 37.8°C (100°F).

Engineering Controls Provide exhaust ventilation or other engineering controls to keep

the airborne concentrations of vapors below their respective

threshold limit value. Ensure that eyewash stations and safety

showers are proximal to the work-station location.

Personal Protection Splash goggles. Lab coat. Gloves.

Personal Protection in

Case of a Large Spill

Splash goggles. Full suit. Boots. Gloves. Suggested protective

clothing might not be sufficient; consult a specialist BEFORE

handling this product.

Exposure Limits Not available

Physical state and

appearance

Liquid

Odor Characteristic

Taste Not available

Molecular Weight 112.22 g/mole

Color Colorless

pH (1% soln/water Not applicable

Boiling Point 102°C (215.6°F)

Melting Point -101°C (-149.8°F)

Critical Temperature Not available

Specific Gravity 0.708 (Water = 1)

Vapor Pressure Not available

190

Vapor Density Not available

Volatility Not available

Odor Threshold Not available

Water/Oil Dist. Coeff Not available

Ionicity (in Water) Not available

Dispersion Properties See solubility in water, methanol, diethyl ether, acetone

Solubility Soluble in acetone. Partially soluble in methanol, diethyl ether.

Insoluble in cold water

Stability and Reactivity Data

Stability The product is stable

Instability

Temperature

Not available

Conditions of

Instability

Not available

Incompatibility with

various substances

Not available

Corrosivity Not available

Special Remarks on

Reactivity

Not available

Special Remarks on

Corrosivity

Not available

Polymerization No

Toxicological Information

Routes of Entry

Toxicity to Animals LD50: Not available. LC50: Not available.

Chronic Effects on The substance is toxic to the nervous system.

191

Humans

Other Toxic Effects on

Humans

Hazardous in case of skin contact (irritant). Slightly hazardous in

case of ingestion.

Special Remarks on

Toxicity to Animals

Not available.

Special Remarks on

Chronic Effects on

Humans

Not available.

Special Remarks on

Chronic Effects on

Humans

Not available.

Special Remarks on

other Toxic Effects on

Humans

Not available.

Ecological Information

Ecotoxicity Not available.

BOD5 and COD Not available.

Products of

Biodegradation

Possibly hazardous short term degradation products are not likely.

However, long term degradation products may arise.

Toxicity of the

Products of

Biodegradation

The product itself and its products of degradation are not toxic.

Special Remarks on

the Products of

Biodegradation

Not available

Transport Information

DOT Classification Class 3: Flammable liquid.

192

Identification Diisobutlyene : UN2050 PG: II

Special Provisions for

Transport:

Not available.

Other Regulatory Information

Federal and State

Regulations

Pennsylvania RTK: 2,4,4-Trimethyl-1-pentene Florida: 2,4,4-

Trimethyl-1-pentene Massachusetts RTK: 2,4,4-Trimethyl-1-

pentene TSCA 8(b) inventory: 2,4,4-Trimethyl-1-pentene

Other Regulations OSHA: Hazardous by definition of Hazard Communication

Standard (29 CFR 1910.1200).

Other Classifications CLASS B-2: Flammable liquid with a flash point lower than

37.8°C (100°F), WHMIS (Canada).

DSCL (EEC) R11- Highly flammable. R38- Irritating to skin. R41- Risk of

serious damage to eyes.

HMIS (U.S.A.) Health Hazard: 2,Fire Hazard: 3, Reactivity: 0 ,Personal

Protection: j

National Fire

Protection Association

(U.S.A.)

Health: 2, Flammability: 3, Reactivity: 0

Protective Equipment Gloves. Lab coat. Wear appropriate respirator when ventilation is

inadequate. Splash goggles

Other Information

References Not available

Other Special

Considerations

Not available

Created 10/10/2005 12:09 AM

Last Updated 05/21/2013 12:00 PM

193

5) Dimethyl ether [72]

Table 46: MSDS of Dimethyl Ether

Identification

Name DIMETHYL ETHER

HAZARDS IDENTIFICATION

GHS Classification Flammable gas = Category 1

Gas under pressure = Liquefied gas

Skin Corrosion / Irritation = Category 2

Eye Damage / Irritation = Category 2B

Specific Target Organ Toxicity - Single Exposure,Category 3

(central nervous system and respiratory system)

Hazard Statement(s) Extremely flammable gas Contains gas under pressure; may

explode if heated Causes skin irritation Causes eye irritation May

cause respiratory irritation May cause drowsiness and dizziness

Prevention Keep away from heat, sparks, open flame, and hot surfaces - No

smoking. Avoid breathing gas. Wash thoroughly after handling.

Wear protective gloves. Use only outdoors or in a well-ventilated

area.

Response Leaking gas fire: Do not extinguish, unless leak can be stopped

safely. Eliminate all ignition sources if safe to do so. IF

INHALED: Remove victim to fresh air and keep at rest in a

position comfortable for breathing. Call a POISON CENTER or

doctor/physician if you feel unwell. IF ON SKIN: Wash with

plenty of soap and water. If skin irritation occurs: Get medical

advice/attention. Take off contaminated clothing and wash before

re-use. IF IN EYES: Rinse cautiously with water for several

minutes. Remove contact lenses, if present and easy to do.

194

Continue rinsing. If eye irritation persists: Get medical

advice/attention.

Storage Store in a well-ventilated place. Protect from sunlight. Keep

container tightly closed. Store locked up.

Disposal Dispose of in accordance with applications with applicable

regulations.

Other Hazards which

do not Result in

Classification

May cause frostbite upon sudden release of compressed gas.

FIRST AID MEASURES

Inhalation If adverse effects occur, remove to uncontaminated area. Give

artificial respiration if not breathing. If breathing is difficult,

oxygen should be administered by qualified personnel. Get

immediate medical attention.

Skin If frostbite or freezing occur, immediately flush with plenty of

lukewarm water (105-115 F; 41-46 C). DO NOT USE HOT

WATER. If warm water is not available, gently wrap affected

parts in blankets. Get immediate medical attention.

Eyes Flush eyes with plenty of water for at least 15 minutes. Then get

immediate medical attention.

Ingestion If a large amount is swallowed, get medical attention.

Note to Physicians For inhalation, consider oxygen.

Symptoms: Immediate Respiratory tract irritation, skin irritation, eye irritation, central

nervous system depression, frostbite

FIRE FIGHTING MEASURES

Specific Hazards Severe fire hazard. Severe explosion hazard. The vapor is heavier

195

Arising from the

Chemical

than air. Vapours or gases may ignite at distant ignition sources

and flash back. Vapour/air mixtures are explosive. Containers

may rupture or explode if exposed to heat. Electrostatic

discharges may be generated by flow or agitation resulting in

ignition or explosion.

Extinguishing Media carbon dioxide, regular dry chemical Large fires: Flood with fine

water spray

Unsuitable

Extinguishing Media

None known

Protective Equipment

and Precautions for

Firefighters

Wear full protective firefighting gear including self-contained

breathing apparatus (SCBA) for protection against possible

exposure.

Fire Fighting

Measures

Move container from fire area if it can be done without risk. Cool

containers with water spray until well after the fire is out. Stay

away from the ends of tanks. For fires in cargo or storage area:

Cool containers with water from unmanned hose holder or

monitor nozzles until well after fire is out. If this is impossible

then take the following precautions: Keep unnecessary people

away, isolate hazard area and deny entry. Let the fire burn.

Withdraw immediately in case of rising sound from venting

safety device or any discoloration of tanks due to fire. For tank,

rail car or tank truck: Stop leak if possible without personal risk.

Let burn unless leak can be stopped immediately. For smaller

tanks or cylinders, extinguish and isolate from other flammables.

Evacuation radius: 800 meters (1/2 mile). Do not attempt to

extinguish fire unless flow of material can be stopped first. Flood

with fine water spray. Cool containers with water spray until well

after the fire is out. Apply water from a protected location or from

a safe distance. Avoid inhalation of material or combustion by-

products. Stay upwind and keep out of low areas. Evacuate if fire

gets out of control or containers are directly exposed to fire.

Evacuation radius: 500 meters (1/3 mile). Consider downwind

evacuation if material is leaking.

196

Hazardous

Combustion Products

Combustion: formaldehyde, oxides of carbon, peroxides

ACCIDENTAL RELEASE MEASURES

Personal Precautions Wear personal protective clothing and equipment

Environmental

Precautions

Avoid release to the environment

Methods for

Containment

Leaking gas fire: Do not extinguish, unless leak can be stopped

safely. Keep unnecessary people away, isolate hazard area and

deny entry. Remove sources of ignition. Ventilate closed spaces

before entering.

Clean-up Methods Avoid heat, flames, sparks and other sources of ignition. Do not

touch spilled material. Stop leak if possible without personal risk.

Reduce vapours with water spray.

HANDLING AND STORAGE

Handling Procedures Wash thoroughly after handling.

Storage Procedures Store and handle in accordance with all current regulations and

standards. Protect from physical damage. Store outside or in a

detached building. Inside storage: Store in a cool, dry place. Store

in a well-ventilated area. Avoid heat, flames, sparks and other

sources of ignition. Subject to storage regulations: U.S. OSHA 29

CFR 1910.101. Keep separated from incompatible substances.

Incompatibilities combustible materials, halogens, oxidizing materials, strong acids

EXPOSURE CONTROLS / PERSONAL PROTECTION

Component Exposure

Limits

Europe: 1000 ppm TWA

1920 mg/m3 TWA

AIHA: 1000 ppm TWA

Component Biological There are no biological limit values for any of this product's

197

Limit Values components.

Engineering Controls Ventilation equipment should be explosion-resistant if explosive

concentrations of material are present. Provide local exhaust

ventilation system. Ensure compliance with applicable exposure

limits.

PERSONAL

PROTECTIVE

EQUIPMENT

Eyes/Face

Wear splash resistant safety goggles. Contact lenses should not be

worn. Provide an emergency eye wash fountain and quick drench

shower in the immediate work area.

Protective Clothing For the gas

Wear appropriate chemical resistant clothing. For the liquid:

Wear appropriate protective, cold insulating clothing.

Glove Recommendations For the gas

Wear appropriate chemical resistant gloves. For the liquid: Wear

insulated gloves.

Respiratory Protection

Under conditions of frequent use or heavy exposure, respiratory

protection may be needed. Respiratory protection is ranked in

order from minimum to maximum. Consider warning properties

before use. For Unknown Concentrations or Immediately

Dangerous to Life or Health - Any supplied-air respirator with a

full face piece that is operated in a pressure-demand or other

positive-pressure mode in combination with an auxiliary self-

contained breathing apparatus operated in pressure-demand or

other positive-pressure mode. Any self-contained breathing

apparatus that has a full face piece and is operated in a pressure-

demand or other positive-pressure mode

PHYSICAL AND CHEMICAL PROPERTIES

Physical State Gas

198

Colour colourless

odour sweet odor

pH Not available

Appearance Colourless gas

Physical Form Liquefied gas

odour Threshold Not available

Boiling Point -24.8 °C

Decomposition Not available

Vapour Pressure 77 psia @ 20 °C

Vapour Density (air =

1)

1.6

Water Solubility 7.6 %

Viscosity Not available

Melting/Freezing

Point

142 °C

Flash Point -41 °C

Evaporation Rate Not available

Henry's Law Constant 0.00317683 atm-m3/mol

Specific Gravity

(water=1)

1.92 g/L @ 25 °C

Auto Ignition 350 °C

Molecular Weight 46.08

Solvent Solubility Soluble: alcohol, ether, chloroform, acetone, organic solvents

STABILITY AND REACTIVITY

Chemical Stability May form explosive peroxides. Avoid prolonged storage or

contact with air, light or storage and use above room temperature.

199

Conditions to Avoid Avoid heat, flames, sparks and other sources of ignition.

Minimize contact with material. Containers may rupture or

explode if exposed to heat.

Possibility of

Hazardous Reactions

Will not polymerize.

Incompatible

Materials

Combustible materials, halogens, oxidizing materials, strong

acids

Hazardous

Decomposition

Combustion: formaldehyde, oxides of carbon, peroxides

TOXICOLOGICAL INFORMATION

Component Analysis -

LD50/LC50

The components of this material have been reviewed in various

sources and the following selected endpoints are published:

Dimethyl ether (115-10-6) = Inhalation LC50 Rat 308.5 mg/L 4 h

RTECS Acute

Toxicity (selected)

The components of this material have been reviewed, and RTECS

publishes the following endpoints:

Dimethyl ether (115-10-6)

Inhalation: 93000 mg/m3/15 minute(s) Inhalation Mouse LC50;

72600 mg/m3/30 minute(s) Inhalation Mouse LC50 164000

ppm/4 hour Inhalation Rat LC50; 308 gm/m3 Inhalation Rat

LC50; 309 gm/m3/4 hour Inhalation Rat LC50

Immediate Effects Respiratory tract irritation, skin irritation, eye irritation, central

nervous system depression, frostbite

Delayed Effects No information on significant adverse effects.

Irritation/Corrosivity

Data

No animal testing data available for skin or eyes.

RTECS Irritation The components of this material have been reviewed and RTECS

200

publishes no data as of the date on this document.

Local Effects Irritant: inhalation, skin, eye

Target Organs Central nervous system

Respiratory Sensitizer No data available

Dermal Sensitizer No data available

Component

Carcinogenicity

None of this product's components are listed by ACGIH, IARC,

NTP, OSHA or DFG.

Mutagenic Data No data available

RTECS Mutagenic The components of this material have been reviewed, and RTECS

publishes data for one or more components.

RTECS Reproductive

Effects

The components of this material have been reviewed, and RTECS

publishes the following endpoints: 200 mg/kg Intraperitoneal

Hamster TDLo (pregnant 8 day(s)); 20000 ppm Inhalation Rat

TCLo (pregnant 6-15 day(s)

Tumorigenic Data No data available

RTECS Tumorigenic The components of this material have been reviewed, and RTECS

publishes data for one or more components.

Specific Target Organ

Toxicity - Single

Exposure

Respiratory system, skin, eye, central nervous system

Specific Target Organ

Toxicity - Repeated

Exposure

No data available

Aspiration Hazard Not applicable

Medical Conditions

Aggravated by

Exposure

None known

ECOLOGICAL INFORMATION

201

Component Analysis -

Aquatic Toxicity

No LOLI ecotoxicity data are available for this product's

components

Persistence and

Degradability

No data available

Bio accumulative

Potential

No data available

Mobility in

Environmental Media

No data available

DISPOSAL CONSIDERATIONS

Disposal Methods Dispose in accordance with all applicable regulations. Subject to

disposal regulations: U.S. EPA 40 CFR 262. Hazardous Waste

Number(s): D001

Component Waste

Numbers

The U.S. EPA has not published waste numbers for this product's

components.

TRANSPORT INFORMATION

US DOT Information Shipping Name: Dimethyl ether

UN/NA #: UN1033

Hazard Class: 2.1 Required Label(s): 2.1

IMDG Information Shipping Name: Dimethyl ether

UN #: UN1033 Hazard Class: 2.1

OTHER INFORMATION

References Not available

Other Special

Considerations

Not available

Created 12/10/2012

202

Last Update 20/11/2014

6) Tert-butyl alcohol [73]

Table 47: MSDS of Tert-Butyl Alcohol

Identification

Name Tert-Butyl Alcohol

Hazards Identification

Potential Acute Health

Effects

Hazardous in case of skin contact (irritant, permeator), of eye

contact (irritant), of ingestion, of inhalation.

Potential Chronic

Health Effects

CARCINOGENIC EFFECTS: A4 (Not classifiable for human or

animal.) by ACGIH. MUTAGENIC EFFECTS: Mutagenic for

bacteria and/or yeast. TERATOGENIC EFFECTS: Not available.

DEVELOPMENTAL TOXICITY: Not available. Repeated or

prolonged exposure is not known to aggravate medical condition.

First Aid Measures

Eye Contact Check for and remove any contact lenses. Immediately flush eyes

with running water for at least 15 minutes, keeping eyelids open.

Cold water may be used. Get medical attention.

Skin Contact In case of contact, immediately flush skin with plenty of water.

Cover the irritated skin with an emollient. Remove contaminated

clothing and shoes. Cold water may be used. Wash clothing

before reuse. Thoroughly clean shoes before reuse. Get medical

attention.

Serious Skin Contact Wash with a disinfectant soap and cover the contaminated skin

with an anti-bacterial cream. Seek immediate medical attention.

Inhalation If inhaled, remove to fresh air. If not breathing, give artificial

respiration. If breathing is difficult, give oxygen. Get medical

203

attention if symptoms appear.

Serious Inhalation Evacuate the victim to a safe area as soon as possible. Loosen

tight clothing such as a collar, tie, belt or waistband. If breathing

is difficult, administer oxygen. If the victim is not breathing,

perform mouth-to-mouth resuscitation. Seek medical attention.

Ingestion Do NOT induce vomiting unless directed to do so by medical

personnel. Never give anything by mouth to an unconscious

person. Loosen tight clothing such as a collar, tie, belt or

waistband. Get medical attention if symptoms appear.

Serious Ingestion Not available.

Fire and Explosion Data

Flammability of the

Product

Flammable

Auto-Ignition

Temperature

477.78°C (892°F)

Flash Points CLOSED CUP: 11.1°C (52°F). OPEN CUP: 16.2°C (61.2°F)

(Cleveland).

Flammable Limits LOWER: 2.4% UPPER: 8%

Products of

Combustion

These products are carbon oxides (CO, CO2).

Fire Hazards in

Presence of Various

Substances

Highly flammable in presence of open flames and sparks, of heat.

Non-flammable in presence of shocks.

Explosion Hazards in

Presence of Various

Substances

Risks of explosion of the product in presence of mechanical

impact: Not available. Risks of explosion of the product in

presence of static discharge: Not available.

Fire Fighting Media

and Instructions

Flammable liquid, soluble or dispersed in water. SMALL FIRE:

Use DRY chemical powder. LARGE FIRE: Use alcohol foam,

204

water spray or fog.

Special Remarks on

Fire Hazards

May form explosive mixtures with air. CAUTION: MAY BURN

WITH NEAR INVISIBLE FLAME. Potassium sodium alloy +

tert-butyl alcohol caused ignition

Special Remarks on

Explosion Hazards

tert-butyl alcohol and hydrogen + sulfuric acid caused explosion

Accidental Release Measures

Small Spill Dilute with water and mop up, or absorb with an inert dry

material and place in an appropriate waste disposal container

Large Spill Flammable liquid. Keep away from heat. Keep away from

sources of ignition. Stop leak if without risk. If the product is in

its solid form: Use a shovel to put the material into a convenient

waste disposal container. If the product is in its liquid form:

Absorb with DRY earth, sand or other non-combustible material.

Absorb with an inert material and put the spilled material in an

appropriate waste disposal. Do not touch spilled material. Prevent

entry into sewers, basements or confined areas; dike if p. 3

needed. Be careful that the product is not present at a

concentration level above TLV. Check TLV on the MSDS and

with local authorities

Handling and Storage

Precautions Keep locked up. Keep away from heat. Keep away from sources

of ignition. Ground all equipment containing material. Do not

ingest. Do not breathe gas/fumes/ vapor/spray. Wear suitable

protective clothing. In case of insufficient ventilation, wear

suitable respiratory equipment. If ingested, seek medical advice

immediately and show the container or the label. Avoid contact

205

with skin and eyes. Keep away from incompatibles such as

oxidizing agents, acids.

Storage Store in a segregated and approved area. Keep container in a cool,

well-ventilated area. Keep container tightly closed and sealed

until ready for use. Avoid all possible sources of ignition (spark

or flame).

Exposure Controls/Personal Protection

Engineering Controls Provide exhaust ventilation or other engineering controls to keep

the airborne concentrations of vapors below their respective

threshold limit value. Ensure that eyewash stations and safety

showers are proximal to the work-station location.

Personal Protection Splash goggles. Lab coat. Vapor respirator. Be sure to use an

approved/certified respirator or equivalent. Gloves.

Personal Protection in

Case of a Large Spill

Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self-

contained breathing apparatus should be used to avoid inhalation

of the product. Suggested protective clothing might not be

sufficient; consult a specialist BEFORE handling this product.

Exposure Limits TWA: 300 (mg/m3) from ACGIH (TLV) [United States] TWA:

100 (ppm) from ACGIH (TLV) [United States] TWA: 100 STEL:

150 from NIOSH [United States] TWA: 300 STEL: 450 (mg/m3)

from NIOSH [United States] TWA: 100 STEL: 150 (ppm)

[United Kingdom (UK)] TWA: 308 STEL: 462 (mg/m3) [United

Kingdom (UK)] TWA: 100 STEL: 150 (ppm) [Canada] TWA:

303 STEL: 455 (mg/m3) [Canada] TWA: 100 from OSHA (PEL)

[United States] TWA: 300 from OSHA (PEL) [United States]3

Consult local authorities for acceptable exposure limits.

Physical and Chemical Properties

Physical state and

appearance

Liquid. (Colourless liquid (above 78 F) which forms white

rhombic crystals.)

206

Odour Camphor

Taste Not available

Molecular Weight 74.12g/mole

Colour Colourless

pH (1% soln/water) Not available

Boiling Point 82.41°C (180.3°F)

Melting Point 25.7°C (78.3°F)

Critical Temperature Not available

Specific Gravity 0.78581 (Water = 1)

Vapor Pressure 4.1 kPa (@ 20°C)

Vapor Density 2.55 (Air = 1)

Volatility Not available

Odor Threshold 219 ppm

Water/Oil Dist. Coeff The product is more soluble in oil; log(oil/water) = 0.4

Ionicity (in Water) Not available

Dispersion Properties See solubility in water

Solubility Soluble in cold water, hot water. Miscible in esters, aliphatic and

aromatic hydrocarbons, alcohol, and ether.

Stability and Reactivity Data

Stability The product is stable.

Instability

Temperature

Not available.

Conditions of

Instability

Heat, ignition sources, incompatibles

207

Incompatibility with

various substances

Reactive with oxidizing agents, acids.

Corrosivity Non-corrosive in presence of glass.

Special Remarks on

Reactivity

Strong mineral acids can cuse composition to flammable

isobutylene gas. Incompatible with mineral acids, sulfuric acid,

and oxidizing materials.

Special Remarks on

Corrosivity

Not available

Polymerization Will not occur

Toxicological Information

Routes of Entry Absorbed through skin. Dermal contact. Eye contact. Inhalation.

Toxicity to Animals WARNING: THE LC50 VALUES HEREUNDER ARE

ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE.

Acute oral toxicity (LD50): 2743 mg/kg [Rat]. Acute dermal

toxicity (LD50): 2000 mg/kg [Rabbit]. Acute toxicity of the vapor

(LC50): 10000 4 hours [Rat].

Chronic Effects on

Humans

CARCINOGENIC EFFECTS: A4 (Not classifiable for human or

animal.) by ACGIH. MUTAGENIC EFFECTS: Mutagenic for

bacteria and/or yeast.

Other Toxic Effects on

Humans

Hazardous in case of skin contact (irritant, permeator), of

ingestion, of inhalation.

Special Remarks on

Toxicity to Animals

Not available.

Special Remarks on

Chronic Effects on

Humans

May cause cancer (tumorigenic) based on animal data. May cause

adverse reproductive effects (fertility and fetotoxicity) and birth

defects based on animal data.

Special Remarks on

other Toxic Effects on

Humans

Acute Potential Health Effects: Skin: Causes skin irritation. Eyes:

Causes eye irritation. Inhalation: Causes respiratory tract and

mucous membrane irritation. May also affect behaviour/Central

Nervous system (ataxia, somnolence), respiration (dyspnoea), and

208

urinary system. Ingestion: Can cause gastrointestinal irritation.

Exposure can cause nausea, headache and vomiting. May also

affect behaviour/Central Nervous system (convulsions, seizures,

and withdrawal), heart, respiration (dyspnoea), urinary system,

metabolism, liver, sense organs.

Ecological Information

Ecotoxicity Not available

BOD5 and COD Not available.

Products of

Biodegradation

Possibly hazardous short term degradation products are not likely.

However, long term degradation products may arise.

Toxicity of the

Products of

Biodegradation

The products of degradation are less toxic than the product itself.

Special Remarks on

the Products of

Biodegradation

Not available

Disposal Considerations

Waste Disposal Waste must be disposed of in accordance with federal, state and

local environmental control regulations.

Transport Information

DOT Classification CLASS 3: Flammable liquid

Identification Butanol UNNA: 1120 PG: II

Special Provisions for

Transport

Not available

Other Regulatory Information

Federal and State Illinois toxic substances disclosure to employee act: tert-Butyl

209

Regulations alcohol Rhode Island RTK hazardous substances: tertButyl

alcohol Pennsylvania RTK: tert-Butyl alcohol Minnesota: tert-

Butyl alcohol Massachusetts RTK: tert-Butyl alcohol

Massachusetts spill list: tert-Butyl alcohol New Jersey: tert-Butyl

alcohol New Jersey spill list: tert-Butyl alcohol New Jersey toxic

catastrophe prevention act: tert-Butyl alcohol California Director's

list of Hazardous Substances: tert-Butyl alcohol TSCA 8(b)

inventory: tert-Butyl alcohol SARA 313 toxic chemical

notification and release reporting: tert-Butyl alcohol

Other Regulations OSHA: Hazardous by definition of Hazard Communication

Standard (29 CFR 1910.1200). EINECS: This product is on the

European Inventory of Existing Commercial Chemical

Substances.

WHMIS (Canada) CLASS B-2: Flammable liquid with a flash point lower than

37.8°C (100°F).

DSCL (EEC) R11- Highly flammable. R21- Harmful in contact with skin.

R36/38- Irritating to eyes and skin. S2- Keep out of the reach of

children. S36/37- Wear suitable protective clothing and gloves.

S46- If swallowed, seek medical advice immediately and show

this container or label.

HMIS (U.S.A.) Health Hazard: 2, Fire Hazard: 3, Reactivity: 0, Personal

Protection: h

National Fire

Protection Association

(U.S.A.)

Health: 1, Flammability: 3, Reactivity: 0

Protective Equipment Gloves. Lab coat. Vapour respirator. Be sure to use an

approved/certified respirator or equivalent. Wear appropriate

respirator when ventilation is inadequate. Splash goggles.

Other Information

References References: -Hawley, G.G... The Condensed Chemical

Dictionary, 11e ed., New York N.Y., Van Nostrand Reinold,

210

1987. -Material safety data sheet emitted by: la Commission de la

Santé et de la Sécurité du Travail du Québec. -SAX, N.I.

Dangerous Properties of Indutrial Materials. Toronto, Van

Nostrand Reinold, 6e ed. 1984. -The Sigma-Aldrich Library of

Chemical Safety Data, Edition II. -Guide de la loi et du règlement

sur le transport des marchandises dangeureuses au canada. Centre

de conformité internatinal Ltée. 1986.

Other Special

Considerations

Not available.

Created 10/09/2005 04:27 PM

Last Updated 05/21/2013 12:00 PM

7) Water [74]

Table 48: MSDS of Water

Identification

Name Water

Hazards Identification

Potential Acute Health

Effects

Non-corrosive for skin. Non-irritant for skin. Non-sensitizer for

skin. Non-permeator by skin. Non-irritating to the eyes. Non-

hazardous in case of ingestion. Non-hazardous in case of

inhalation. Non-irritant for lungs. Non-sensitizer for lungs.

Noncorrosive to the eyes. Non-corrosive for lungs.

Potential Chronic

Health Effects

Non-corrosive for skin. Non-irritant for skin. Non-sensitizer for

skin. Non-permeator by skin. Non-irritating to the eyes. Non-

hazardous in case of ingestion. Non-hazardous in case of

inhalation. Non-irritant for lungs. Non-sensitizer for lungs.

CARCINOGENIC EFFECTS: Not available. MUTAGENIC

EFFECTS: Not available. TERATOGENIC EFFECTS: Not

available. DEVELOPMENTAL TOXICITY: Not available.

211

First Aid Measures

Eye Contact Not applicable

Skin Contact Not applicable

Serious Skin Contact Not available

Inhalation Not applicable

Serious Inhalation Not available

Ingestion Not Applicable

Serious Ingestion Not available

Fire and Explosion Data

Flammability of the

Product

Non-flammable

Auto-Ignition

Temperature

Not applicable

Flash Points Not applicable

Flammable Limits Not applicable

Products of

Combustion

Not available

Fire Hazards in

Presence of Various

Substances

Not applicable

Explosion Hazards in

Presence of Various

Substances

Not available

Fire Fighting Media

and Instructions

Not available

Special Remarks on

Fire Hazards

Not available

212

Special Remarks on

Explosion Hazards

Not available

Accidental Release Measures

Small Spill Mop up, or absorb with an inert dry material and place in an

appropriate waste disposal container.

Large Spill Absorb with an inert material and put the spilled material in an

appropriate waste disposal.

Handling and Storage

Precautions No specific safety phrase has been found applicable for this

product.

Storage Not applicable

Exposure Controls/Personal Protection

Engineering Controls Not Applicable

Personal Protection Safety glasses. Lab coat.

Personal Protection in

Case of a Large Spill

Not Applicable

Exposure Limits Not available.

Physical and Chemical Properties

Physical state and

appearance

Liquid

odour Odourless

Taste Not available

Molecular Weight 18.02 g/mole

Colour Colourless

pH (1% soln/water) 7

213

Boiling Point 100°C (212°F)

Melting Point Not available

Critical Temperature Not available

Specific Gravity 1 (Water = 1)

Vapour Pressure 2.3 kPa (@ 20°C)

Vapour Density 0.62 (Air = 1)

Volatility Not available

Odour Threshold Not available

Water/Oil Dist. Coeff Not available

Ionicity (in Water) Not available

Dispersion Properties Not applicable

Solubility Not applicable

Stability and Reactivity Data

Stability The product is stable.

Instability

Temperature

Not available

Conditions of

Instability

Not available

Incompatibility with

various substances

Not available

Corrosivity Not available

Special Remarks on

Reactivity

Not available

Special Remarks on

Corrosivity

Not available

Polymerization Will not occur

214

Toxicological Information

Routes of Entry Absorbed through skin. Eye contact.

Toxicity to Animals LD50: [Rat] - Route: oral; Dose: > 90 ml/kg LC50: Not available.

Chronic Effects on

Humans

Not available

Other Toxic Effects on

Humans

Non-corrosive for skin. Non-irritant for skin. Non-sensitizer for

skin. Non-permeator by skin. Non-hazardous in case of ingestion.

Non-hazardous in case of inhalation. Non-irritant for lungs. Non-

sensitizer for lungs. Non-corrosive to the eyes. Noncorrosive for

lungs.

Special Remarks on

Toxicity to Animals

Not available.

Special Remarks on

Chronic Effects on

Humans

Not available

Special Remarks on

other Toxic Effects on

Humans

Not available

Ecological Information

Ecotoxicity Not available

BOD5 and COD Not available

Products of

Biodegradation

Possibly hazardous short term degradation products are not likely.

However, long term degradation products may arise.

Toxicity of the

Products of

Biodegradation

The product itself and its products of degradation are not toxic.

Special Remarks on

the Products of

Not available

215

Biodegradation

Disposal Considerations

DOT Classification Not a DOT controlled material (United States).

Identification Not applicable

Special Provisions for

Transport

Not applicable

Other Regulatory Information

Federal and State

Regulations

TSCA 8(b) inventory: Water

Other Regulations EINECS: This product is on the European Inventory of Existing

Commercial Chemical Substances.

WHMIS(Canada) Not controlled under WHMIS (Canada).

DSCL (EEC) This product is not classified according to the EU regulations. Not

applicable.

HMIS (U.S.A.) Health Hazard: 0, Fire Hazard: 0, Reactivity: 0, Personal

Protection: a

National Fire

Protection Association

(U.S.A.)

Health: 0, Flammability: 0, Reactivity: 0

Protective Equipment Not applicable. Lab coat. Not applicable. Safety glasses.

Other Information

References Not available

Special Considerations Not available

Created 10/10/2005 08:33 PM

Last Updated 05/21/2013 12:00 PM

216

Appendix B

Economic Potential Economic Potential by Design Variable

Economic potential and evaluation are an action to make sure the development of the

company especially in terms of company profit. The purpose of invest huge amount of money in a

chemical plant is to earn profit by some means of the economic performance of a project. Before

the company making the decision to invest large amount capital to build a chemical plant, the

management must be convinced that the project can earn profit to the company. Economic

potential depends on a lot of factor that can contribute to it. One of them is the absolute

production capacity of the economic branches. For calculation, economic potential will be based

on the actual output and total use of the production capacities. The pilot design will be tested

before the scale up to the desired plant capacity. The engineer must be understood all the process

limitation and can predict what will be happen when the scale up is done whether the process will

deviation much more than a pilot scale. Therefore, safety must be taken as one of the importance

factors to build full capacity plant. More than that, engineers must have the ability to anticipate

the future which means he/she must can predict the price of product so that the company will not

fall into trap of bankruptcy after putting large investment to build the plant.

The design variables play an importance role in controlling the economic potential of one

company. The project is initiated by considering normal operation and expected production rate.

Some of the costs found to be reducing and some cost increases when one of the design variables

is changed. In Petronas Sdn. Bhd petrochemical plant in Gebeng, the chosen design variable is

only the conversion of our final product which MTBE, since there will be no side reaction will

occur in the production. The production cost can be altered by the conversion of MTBE. By

making a hypothesis, the higher the conversion of MTBE will give higher economic potential for

one industry. An economic potential plot will be based on the conversion is made in order to

evaluate the effect of conversion of product toward the economic potential. For a company,

maximum profit is a must. Therefore, suitable design variable must be chosen properly. Input and

output structure, recycle structure are considered besides economic potential.

Economic Potential of Input-Output Structure

Level 1: Economics Potential: Input-Output Structure

Methyl

Tertiary Butyl

Ether (MTBE)

Isobutylene

Methanol REACTOR

217

Figure 34: Input-output structure for MTBE production from isobutylene and methanol

The economics potential is done based on the assumptions as stated below:

1. Methanol to isobutylene ratio – 1.1

2. Isobutylene conversion in the reactor – 0.92

3. Selectivity of MTBE in the reactor – 0.965

4. Selectivity of TBA in the reactor – 0.0064

5. Selectivity of DIB in the reactor – 1.0

6. Total working days per year: 350 days

Annual Cost of Product (MTBE)

= (𝑅𝑀 4663

𝑇𝑜𝑛𝑛𝑒𝑠 𝑀𝑇𝐵𝐸×

300,000 𝑇𝑜𝑛𝑛𝑒𝑠 𝑀𝑇𝐵𝐸

𝑦𝑒𝑎𝑟)

= 𝑅𝑀 1,398,900,000/𝑦𝑒𝑎𝑟

= 𝑹𝑴 𝟏𝟑𝟗𝟖. 𝟗𝟎 𝒎𝒊𝒍𝒍𝒊𝒐𝒏/𝒚𝒆𝒂𝒓

Annual Cost of Raw Material (Isobutylene, Methanol)

= (𝑅𝑀 2963

𝑇𝑜𝑛𝑛𝑒𝑠 𝐼𝑠𝑜𝑏𝑢𝑡𝑦𝑙𝑒𝑛𝑒×

190909.0909 𝑇𝑜𝑛𝑛𝑒𝑠 𝐼𝑠𝑜𝑏𝑢𝑡𝑦𝑙𝑒𝑛𝑒

𝑦𝑒𝑎𝑟) +

(𝑅𝑀 2323

𝑇𝑜𝑛𝑛𝑒𝑠 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙×

119999.9999 𝑇𝑜𝑛𝑛𝑒𝑠 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙

𝑦𝑒𝑎𝑟)

= 𝑅𝑀 565,663,636.30/𝑦𝑒𝑎𝑟 + 𝑅𝑀 278,759,999.80/𝑦𝑒𝑎𝑟

= 𝑅𝑀 844,423,636.10/𝑦𝑒𝑎𝑟

= 𝑹𝑴 𝟖𝟒𝟒. 𝟒𝟐𝟑𝟔 𝒎𝒊𝒍𝒍𝒊𝒐𝒏/𝒚𝒆𝒂𝒓

Economics Potential

= Annual Cost of Products – Annual Cost of Raw Materials

= 𝑅𝑀 1398.90 𝑚𝑖𝑙𝑙𝑖𝑜𝑛/𝑦𝑒𝑎𝑟 − 𝑅𝑀 844.4236 𝑚𝑖𝑙𝑙𝑖𝑜𝑛/𝑦𝑒𝑎𝑟

= 𝑹𝑴 𝟓𝟓𝟒. 𝟒𝟕𝟔𝟒 𝒎𝒊𝒍𝒍𝒊𝒐𝒏/𝒚𝒆𝒂𝒓

218

At Recycle Structure

Level 2: Economics Potential: Varying Recycle Ratio to the Reactor

Recycle unreacted methanol

Figure 35: Recycle structure for MTBE production from isobutylene and methanol

The recycle ratio is varied from 0 to 0.99. Assumptions for other calculation are stated below:

1. Methanol to isobutylene ratio – 1.1

2. Isobutylene conversion in the reactor – 0.92

3. Selectivity of MTBE in the reactor – 0.965

4. Selectivity of TBA in the reactor – 0.0286

5. Selectivity of DIB in the reactor – 0.0064

6. Total working days per year: 350 days

Table 49: Economics potential of MTBE production with varying methanol recycle ratio

Recycle

Ratio

Price of Product

Formed

Flow Rate of

Fresh Methanol

Price of Fresh

Methanol

Total Reactant

Price

Economic

Potential

(RM/year) (tonnes/year) (RM/year) (RM/year) (RM/year)

0.0 1398900000.00 119999.9999 158759999.87 724423636.17 674476363.83

0.1 1398900000.00 117626.0927 155619320.64 721282956.94 677617043.06

0.2 1398900000.00 115252.1855 152478641.42 718142277.72 680757722.28

0.3 1398900000.00 112878.2783 149337962.19 715001598.49 683898401.51

0.4 1398900000.00 110504.3711 146197282.97 711860919.27 687039080.73

0.5 1398900000.00 108130.4639 143056603.74 708720240.04 690179759.96

0.6 1398900000.00 105756.5567 139915924.51 705579560.81 693320439.19

0.7 1398900000.00 103382.6495 136775245.29 702438881.59 696461118.41

0.8 1398900000.00 101008.7423 133634566.06 699298202.36 699601797.64

0.9 1398900000.00 98634.8351 130493886.84 696157523.14 702742476.86

1.0 1398900000.00 96260.9279 127353207.61 693016843.91 705883156.09

REACTOR Isobutylene

MTBE Methanol

219

Figure 36: Graph of economics potential vs recycle ratio

In this level 2 economic potential analysis, the recycle ratio of unreacted methanol back to

the reactor is varied. From table 36, the amount of methanol needed can be decreased with

increasing of recycle ratio and vice versa. Therefore, the cost required to buy methanol as the

reactant of the reaction can be reduced. In other words, the operational cost allocated to buy the

methanol can be decreased with the increase of methanol recycle amount hence higher economics

potential as depicted by Figure 31 especially towards full recycling. The economic potential here

indicates that the profit of the plant corresponding to the different recycle ratio. Hence, for our

plant design, we set recycle ratio of methanol at the highest possible percentage (100%) to

minimize the operational cost.

Level 3: Economics Potential: Varying CO conversion in methanol reactor

Figure 37: Reactor structure for MTBE production from isobutylene and methanol

The isobutylene conversion is varied from 0.1 to 1. Assumptions for other calculation are stated

below:

1. Methanol to isobutylene ratio – 1.1

2. Isobutylene conversion in the reactor – 0.92

3. Selectivity of MTBE in the reactor – 0.965

4. Selectivity of TBA in the reactor – 0.0286

5. Selectivity of DIB in the reactor – 0.0064

6. Total working days per year: 350 days

6.70E+08

6.75E+08

6.80E+08

6.85E+08

6.90E+08

6.95E+08

7.00E+08

7.05E+08

7.10E+08

0.0 0.2 0.4 0.6 0.8 1.0 1.2

Eco

no

mic

Po

ten

tia

l (R

M/y

ear)

Recycle Ratio

Economic Potential vs Recycle Ratio

REACTOR Isobutylene

MTBE Methanol

220

Table 50: Economics potential of methanol production with varying isobutylene conversion

Isobutylene

conversion

Total

Reactant

Price

Flow Rate of

Product

Formed

Price of

product

formed

Economic

Potential

(RM/year) (tonnes/year) (RM/year) (RM/year)

0.1 693016843.91 30000 139890000 -553126843.91

0.2 693016843.91 60000 279780000 -413236843.91

0.3 693016843.91 90000 419670000 -273346843.91

0.4 693016843.91 120000 559560000 -133456843.91

0.5 693016843.91 150000 699450000 6433156.09

0.6 693016843.91 180000 839340000 146323156.09

0.7 693016843.91 210000 979230000 286213156.09

0.8 693016843.91 240000 1119120000 426103156.09

0.9 693016843.91 270000 1259010000 565993156.09

1.0 693016843.91 300000 1398900000 705883156.09

Figure 38: Graph of economics potential vs isobutylene conversion

In this level 3 economic potential analysis, the isobutylene conversion in the reactor is

manipulated from 0.1 to 1.0. From the table above, the amount of MTBE (desired product)

produced increases with increasing of isobutylene conversion and vice versa. Therefore, the profit

of methanol per year increases with increase of isobutylene conversion hence higher economics

potential as depicted by Figure 33. Based on the figure, the conversion of isobutylene must be at

least equal to 0.495 in order to get positive economic potential. However, for our plant design, we

set the isobutylene conversion at 0.92 as this value is obtained from literature, which researchers

have carried out the extensive number of experiments in laboratory to prove this value.

-8.00E+08

-6.00E+08

-4.00E+08

-2.00E+08

0.00E+00

2.00E+08

4.00E+08

6.00E+08

8.00E+08

0.0 0.2 0.4 0.6 0.8 1.0 1.2

Eco

nom

ic P

ote

nti

al

(RM

/yea

r)

Conversion

Economic Potential vs Conversion

221

Appendix C

Mass Transfer Equipment Design Distillation Column, T-101

Design Criteria:

This distillation column is used to separate desired product, MTBE from mixture of unreacted methanol,

C4 mixture and by-product.

Design Parameters:

Component

Distribution

Column Sizing Plate Hydraulic

Design

Mechanical Design

Number of Stages Tray Spacing Active Area Design Pressure

Reflux Ratio Flooding Velocity Hole Area Design Temperature

Number of Actual

Stages

Net Area Tray Thickness Material of

Construction

Tray Efficiency Downcomer Area Hole Diameter Column Wall

Thickness

Location of Feed

Stage

Column Diameter Liquid Flow

Arrangement

Column Head Design

Column Height Column Pressure Drop Insulation

Weeping Checking Stress Analysis

Downcomer Liquid

Backup

Column Support

Residence Time Nozzle Size

Entrainment Checking

Number of Holes

Design Basic:

Feed stream into the distillation column T-101 consist of a mixture of unreacted methanol, C4 mixture and

by product, TBA and diisobutylene. The total mass flow rate of feed is 43011.388 kg/hr at 75 oC and

1000kPa. Distillate is carried out from the top of the column operating at 67 oC and 750kPa. On the other

hand, the bottom of column operate at 120 oC and 750kPa.

Design Method:

Fenske-Underwood-Gilliland method is used for component distribution calculation. The column sizing,

plate hydraulic design and mechanical design of the distillation column is based on Coulson and

Richardson’s Chemical Engineering Design and Ray Sinnott and Gavin Towler’s Chemical Engineering

Design.

1. Component Distribution:

Step 1: Identification of Light Key (LK) and Heavy Key (HK) Component

222

Butane is light key component, MTBE is heavy key component. On the other hands, methanol, isobutylene,

1,3-butadiene and butene are light non-key components. TBA and diisobutylene are heavy non-key

components.

Step 2: Relative Volatility Calculation

Relative volatility is calculated from the volatility of respective component, which is determined from the

partial pressure of component and the system pressure. Partial pressure of component is determined from

Antoine’s equation. The Antoine Equation is stated as

log10 𝑝 = 𝐴 −𝐵

𝑇 + 𝐶

Where p= vapour pressure(mmHg)

A,B,C= regression coefficients for chemical compound

T= temperature(oC)

The constant for each component as stated below which get from Richard M.Felder and Ronald’s

Elementary Principles of Chemical Processes:

Components A B C

Methanol 7.87863 1473.110 230.0

MTBE 5.89600 708.690 179.9

Isobutylene 6.84134 923.200 240.0

1,3-butadiene 7.00613 999.04 245.866

Butene 6.53101 810.261 228.066

Butane 6.82485 943.453 239.711

Diisobutylene 6.81189 1257.840 220.735

TBA 7.31990 1154.480 177.660

TF =75 oC TD =67 oC TB =120 oC

Component vapor pressure α vapor pressure α vapor pressure α

Butane(LK) 8.951654612 5.143597754 7.476698096 5.286389071 21.2292967 4.66788569

MTBE(HK) 1.740348884 1 1.414329894 1 4.547947 1

Methanol(LNK) 1.491640745 0.857092942 1.105520399 0.781656672 6.23228602 1.37035151

Isobutylene(LNK) 10.85049221 6.234664964 9.100745438 6.434669503 25.2231107 5.54604324

1,3-butadiene(LNK) 10.41020303 5.981675932 8.666524166 6.127653952 25.1429291 5.52841295

Butene(LNK) 9.602111267 5.517348478 8.126059529 5.745519176 21.2822912 4.67953809

Diisobutylen(HNK) 0.482531653 0.277261449 0.367511288 0.259848349 1.7589113 0.38674842

TBA(HNK) 0.750758867 0.431384117 0.532220267 0.376305606 3.68369763 0.80996934

𝑊ℎ𝑒𝑟𝑒 𝛼𝐿𝐾/𝐻𝐾 =𝑃𝐿𝐾

𝑠𝑎𝑡

𝑃𝐻𝐾𝑠𝑎𝑡

𝛼𝑎𝑣𝑔 = (5.14 × 5.29 × 4.67)13

= 5.027

223

Step 3: Minimum number of stages, Nmin

Component XB XD 𝛼𝐿𝐾/𝐻𝐾

Butane (LK) 0.000005 0.0016 5.027

MTBE (HK) 0.9679 0.0296

𝑁𝑚𝑖𝑛 =ln[(

𝑥𝐿𝐾𝑥𝐻𝐾

)𝐷 × (𝑥𝐻𝐾𝑥𝐿𝐾

)𝐵

ln[𝛼𝐿𝐾𝛼𝐻𝐾

]

=ln [(

0.00160.0296

) × (0.9679

0.000005)]

ln 5.027 = 5.73 𝑠𝑡𝑎𝑔𝑒𝑠

Step 4: Minimum reflux ratio, Rmin

Before calculating R, minimum reflux ratio, Rmin is determined by using the Underwood equation:

∑𝛼𝑖𝑥𝐹,𝑖

𝛼𝑖 − 𝜃= 1 − 𝑞

𝑛

𝑖=1

At feed condition (85 oC, 100kPa), the feed exist as saturated liquid. Thus q=1 since vapor

fraction=0.

Component XB XD α(TF) XF

Butane(LK) 0.000005 0.0016 5.14 0.0004

MTBE(HK) 0.967900 0.0296 1.00 0.7347

Methanol(LNK) 0.000000 0.7003 0.86 0.1740

Isobutylene(LNK) 0.000000 0.2636 6.23 0.0655

1,3-butadiene(LNK) 0.000000 0.0017 5.98 0.0004

Butene(LNK) 0.000000 0.0033 5.52 0.0008

Diisobutylen(HNK) 0.003200 0.0000 0.28 0.0024

TBA(HNK) 0.028900 0.0000 0.43 0.0217

5.14 × 0.0004

5.14 − 𝜃+

1.00 × 0.7347

1.00 − 𝜃+

0.86 × 0.174

0.86 − 𝜃+

6.23 × 0.0655

6.23 − 𝜃+

5.98 × 0.0004

5.98 − 𝜃

+5.52 × 0.0008

5.52 − 𝜃+

0.28 × 0.0024

0.28 − 𝜃+

0.43 × 0.0217

0.43 − 𝜃= 0

By using SOLVER in Excel, we get the value of θ=0.280476

Minimum reflux ratio, Rmin can be determined by using θ value through the equations:

𝑅𝑚𝑖𝑛 + 1 = ∑𝛼𝑖𝑥𝐷,𝑖

𝛼𝑖 − 𝜃𝑖

For θ=3.305,

224

𝑅𝑚𝑖𝑛 + 1 =𝛼𝐿𝐾𝑥𝐷,𝐿𝐾

𝛼𝐿𝐾 − 𝜃+

𝛼𝐻𝐾𝑥𝐷,𝐻𝐾

𝛼𝐻𝐾 − 𝜃+

𝛼𝑁𝐾𝑥𝐷,𝑁𝐾

𝛼𝑁𝐾 − 𝜃

𝑅𝑚𝑖𝑛 + 1 =5.14 × 0.0016

5.14 − 0.280476+

1.00 × 0.0296

1.00 − 0.280476+

0.86 × 0.7003

0.86 − 0.280476+

6.23 × 0.2636

6.23 − 0.280476

+5.98 × 0.0017

5.98 − 0.280476+

5.52 × 0.0033

5.52 − 0.280476+

0.28 × 0.00

0.28 − 0.280476+

0.43 × 0.00

0.43 − 0.280476

Rmin = 0.363

Step 5: Determination of reflux ratio, R

According to rule of thumb, actual reflux ratio is R=1.2Rmin

R=1.2(0.363) =0.4356

Step 6: Determination of number of theoretical stages, N

𝑋 =𝑅−𝑅𝑚𝑖𝑛

𝑅+1=

0.4356−0.363

0.4356+1= 0.0506

𝑌 = 1 − exp [(1+54.4𝑋

11+117.2𝑋) (

𝑋−1

𝑋0.5)]

= 1 − exp [(1+54.4(0.0506)

11+117.2(0.0506)) (

0.0506−1

(0.0506)0.5)] = 0.6076

𝑌 =𝑁−𝑁𝑚𝑖𝑛

𝑁+1

0.6076 =𝑁−5.73

𝑁+1

𝑁 = 16.15 𝑠𝑡𝑎𝑔𝑒𝑠

Step 7: Overall Tray Efficiency

The tray efficiency is determined through the equation shown below:

𝐸0 =0.492

[(𝛼𝐿𝐾 𝐻𝐾⁄ )𝑎𝑣𝑒𝜇𝐹]0.245

Where μF = viscosity of feed mixture, by which μF can be estimated by using the equation:

1

𝜇𝐹= ∑

𝑥𝑖

𝜇𝑖

Below is the table of viscosity of each component in the feed at T=75 oC

Component μi (Pa.s) XF Xi/ μi

Butane(LK) 1.00272 0.0004 0.0004

MTBE(HK) 0.00021 0.7347 3529.714

Methanol(LNK) 0.00031 0.1740 555.5937

Isobutylene(LNK) 0.000129 0.0655 507.752

1,3-butadiene(LNK) 0.0000829 0.0004 4.825

225

Butene(LNK) 0.000116 0.0008 6.8966

Diisobutylen(HNK) 0.000104 0.0024 23.077

TBA(HNK) 0.000632 0.0217 34.335

Total 4662.1937

𝜇𝐹 = 0.2145𝑚𝑃𝑎. 𝑠

𝐸0 =0.492

(5.027×0.2145)0.245 = 0.483

Step 8: Actual number of stages

𝑁𝑎𝑐𝑡𝑢𝑎𝑙 =𝑁

𝐸0=

16.15

0.483= 33.44 𝑠𝑡𝑎𝑔𝑒𝑠

Number of theoretical stages, N= Nactual -1= 33.44-1 = 32.44

≈ 33 stages

Step 9: Determination of location of feed tray

By using Kirkbride equation, the location of the feed point calculated from bottom is determined.

log𝑁𝑟

𝑁𝑠= 0.206 log{

𝐵

𝐷(𝑥𝐻𝐾

𝑥𝐿𝐾)𝐹[

(𝑥𝐿𝐾)𝐵

(𝑥𝐻𝐾)𝐷]2} ………….. (1)

𝑁𝑟 + 𝑁𝑠 = 𝑁𝑎𝑐𝑡 ………(2)

Bottom, B 25452.59 XF,HK 0.1740 XB,LK 0.000005

Distillate, D 74747.29 XF,LK 0.0004 XD,HK 0.0296

Subsitute the values in the table into equation (1). We will get:

𝑁𝑟 = 0.07815𝑁𝑠 ……..(3)

𝑁𝑟 + 𝑁𝑠 = 33 ……..(4)

Solve equation (3) & (4) simultaneously, thus we will get:

Ns=31

Nr=2

Thus, the feed enter the column at 31st stages from the bottom of column

Number of stages/trays in rectifying section = 2

Number of stages in stripping section =31

Number of trays in stripping section =30 (excluding partial reboiler)

1. Column Sizing

226

The distillation column is sized based on the top condition and the bottom condition. Besides,

the size of distillation column is decided based on the larger diameter calculated from the top

or bottom condition. For column sizing, the important information is the flow rate of each

stream related to distillation column and their respective density.

Step 1: Determination of column height

Tray spacing of 0.3-0.6m are normally employed in industry. Hence, tray spacing, Hs=0.6m is

chosen.

Column height is calculated with tray spacing and the additional space for vapor-liquid

disengagement at column top and for liquid sump at column bottom. An approximation of 15%

allowance for the additional space for phase disengagement and required internal hardware.

Column height, HC = 1.15NHS

HC= 1.15(33)(0.6)

= 22.77 m

Step 2: Determination of physical properties of distillate and bottom product

To determine the diameter of a column, the surface tension (σ) of liquid-vapor interaction is

prerequiste. According to Sugden (1924), a method was developed to estimate the surface tension

of pure component as well as mixture of components, known as contribution to Sudgens’ parachor

for organic compounds as shown in Table 8.7 (pg. 335) in Coulson & Richardson Chemical

Engineering, vol. 6, 4th

edition.

For pure component: 𝜎 = [𝑃𝑐ℎ(𝜌𝐿−𝜌𝑉)

𝑀]4 × 10−12

Where σ= Surface tension (mJ/m2)

Pch= Sudgen’s parachor (Refer Table 8.7)

ρL= Liquid density (kg/m3)

ρV= Density of saturated vapour (kg/m3)

M= Molecular weight

For mixture of liquid: 𝜎𝑚 = 𝜎1𝑥1 + 𝜎2𝑥2 + ⋯

227

Where x1,x2 is the component mole fractions

Pch estimation:

For methanol:

Atom, Group or

Bond

Contribution Value Total Contribution

C 1 4.8 4.8

H-O 1 11.3 11.3

H-C 3 51.3 51.3

O 1 20 20

87.4

For MTBE:

Atom, Group or

Bond

Contribution Value Total Contribution

C 5 4.8 24

H-O 0 11.3 0

H-C 12 17.1 205.2

O 1 20 20

249.2

For isobutylene:

Atom, Group or

Bond

Contribution Value Total Contribution

H-C 8 17.1 136.8

C 4 4.8 19.2

= Bond 1 23.2 23.2

179.2

For butene:

Atom, Group or

Bond

Contribution Value Total Contribution

C 4 4.8 19.2

H-C 8 17.1 136.8

= Bond 1 23.2 23.2

228

179.2

For diisobutylene:

Atom, Group or

Bond

Contribution Value Total Contribution

C 8 4.8 38.4

H-C 16 17.1 273.6

= Bond 1 23.2 23.2

335.2

For butane:

Atom, Group or

Bond

Contribution Value Total Contribution

H-C 10 17.1 171

C 4 4.8 19.2

190.2

For TBA:

Atom, Group or

Bond

Contribution Value Total Contribution

C 4 4.8 19.2

H-O 1 11.3 11.3

H-C 9 51.3 461.7

O 1 20 20

512.2

For 1,3-butadiene:

Atom, Group or

Bond

Contribution Value Total Contribution

C 4 4.8 19.2

H-C 6 17.1 102.6

= Bond 2 23.2 46.4

168.2

229

To determine the density of vapour at particular pressure, the ideal gas behaviour can be assumed

for pure component and non-ideal for mixture to account for the molecular interaction of

individual component.

For pure component: 𝜌𝑉 =𝑃𝑀

𝑅𝑇

For mixture: 𝜌𝑣,𝑚 =𝑃𝑟

′𝑀𝑟,𝑚𝑖𝑥

𝑧𝑅𝑇𝑟′

Where Pr’= Pseudoreduced pressure = P/Pc’

Mr,mix= Molecular weight of mixture

Tr’= Pseudoreduced temperature = T/Tc’

Z= Compressibility factor

P= Pressure of system

Pc’= Preudocritical pressure= yAPcA + yBPcB+….

Tc’= Pseudocritical temperature= yATcA + yBTcB+….

yA, yB= component mole fraction

PcA, PcB= component critical pressure

TcA, TcB= component critical temperature

The physical properties of pure component in distillate and bottom product:

Pure Components Butane MTBE Methanol Isobutylene 1,3-

butadiene

Butene DIB TBA

ρv

(kg/m3)

Top 15.414 23.338 8.487 14.881 14.345 14.881 30.294 19.657

Bottom 13.336 20.192 7.342 12.875 12.411 12.875 26.210 17.007

ρL

(kg/m3)

Top 518.548 689.946 746.175 529.848 556.806 528.168 654.247 734.294

Bottom 424.266 624.771 684.241 423.854 455.455 422.659 603.678 663.570

Pch 190.2 249.2 87.4 179.2 168.2 179.2 335.2 512.2

σ

(J/m2)

Top 0.0073 0.0127 0.0165 0.0073 0.0081 0.0072 0.0112 0.5948

Bottom 0.0033 0.0086 0.0117 0.0030 0.0036 0.0029 0.0082 0.3985

Molecular mass

(kg/kmol)

58.12 88 32 56.11 54.09 56.11 114.229 74.12

PC (bar) 37.94 35.87 79.54 40.10 43.20 40.23 26.19 39.72

TC (K) 424.90 497.25 786.35 418.09 425.00 692.60 559.70 506.20

XD 0.0016 0.0296 0.7003 0.2636 0.0017 0.0033 0.0000 0.0000

XB 0.000005 0.9679 0.0000 0.0000 0.0000 0.0000 0.0032 0.0289

230

For mixture:

properties

mixture

top bottom

Pc’ (bar) 67.600877 35.950

Pr’ (bar) 0.110945306 0.210000

Tc’ (K) 679.295949 497.7106195

Tr’ (K) 0.500739038 0.78991684

Z 0.92 0.85

Mr (kg/kmol) 36.98713886 87.58966689

ρL (kg/m3) 670.5516921 625.7535308

ρv (kg/m3) 9.809152936 20.09767588

L (kmol/hr) 306.906336 1300.376336

V (kmol/hr) 2853.450 1933.770

FLV 0.036698984 0.520415338

Compressibility factor,z is obtained by interpolation from Figure 3.8 based on the value of Pr’ and

Tr’ in Coulson, Chemical Engineering Design.

For mixture in both liquid and vapour in overhead and bottom product, the methods used to

estimate the physical properties (ρL, ρV and Mr) are stated as below:

Molecular weight, Mr: 1

𝑀𝑟=

𝑥𝐴

𝑀𝐴+

𝑥𝐵

𝑀𝐵+ ⋯

Where xA, xB= component mass fraction

MA,MB= component molecular weight

Liquid density, ρL: 1

𝜌𝐿=

𝑥𝐴

𝜌𝐴+

𝑥𝐵

𝜌𝐵+ ⋯

Where xA, xB= component mass fraction

ρA,ρB= component density

Step 3: Determination of K value

231

From the value of FLV get previously, we can get the value of K1 from Coulson & Richardson

Chemical Engineering, Vol. 6, 4th

edition Figure 11.27 (pg. 568).

Top Bottom

K1 0.12 0.053

Step 4: Determination of vapour flooding velocity, uf

Assuming column diameter is larger than 1m, tray spacing of 0.5m is typically chosen.

𝑢𝑓 = 𝐾1(𝜌𝐿 − 𝜌𝑉

𝜌𝑉)0.5

Top Bottom

Uf

0.12 (670.55 − 9.809

9.809)0.5

=0.985 m/s

0.053 (625.754 − 20.098

20.098)

0.5

=0.291 m/s

Step 5: Determination of actual vapour velocity, uV

232

Assume 50% flooding for column operation

𝑢𝑉 = 0.5𝑢𝑓

Top Bottom

UV 0.5(0.985 m/s)= 0.493 m/s 0.5(0.291 m/s)= 0.146 m/s

Step 6: Determination of volumetric flow rate, �̇�

�̇� =𝑣 (

𝑘𝑚𝑜𝑙ℎ𝑟

) × 𝑀𝑟 (𝑘𝑔

𝑘𝑚𝑜𝑙)

𝜌𝑉 (𝑘𝑔𝑚3) ×

3600𝑠ℎ𝑟

Top Bottom

�̇� 2853.45×36.987

9.809×3600

=2.99 m3/s

1933.77×87.59

20.098×3600

=2.34 m3/s

Step 7: Determination of net column area, An

𝐴𝑛 =�̇�

𝑢𝑣

Top Bottom

An 2.99/0.493

=6.06 m2

2.34/0.146

=16.03 m2

Step 8: Determination of cross sectional area, Ac

Assume downcomer occupies 20% of column cross sectional area, 𝐴𝑐 =𝐴𝑛

0.8

Top Bottom

Ac 6.06/0.8

=7.58 m2

16.03/0.8

=20.04 m2

Step 9: Determination of cross sectional area of downcomer, Ad

233

𝐴𝑑 = 𝐴𝑐 − 𝐴𝑛

Top Bottom

Ad 7.58-6.06

=1.52 m2

20.04-16.03

=4.01 m2

Step 10: Determination of column diameter, Dc

𝐷𝑐 = √4𝐴𝑐

𝜋

Top Bottom

Dc √

4𝐴𝑐

𝜋

=√4(7.58)

𝜋

=3.11 m

√4𝐴𝑐

𝜋

=√4(20.04)

𝜋

=5.05 m

Since limiting vapour condition occurs at the bottom of column, so the column inner diameter is

taken as 5.05 m. Since the column diameter is larger than 1m, the tray spacing of 0.6 m is justified.

There are two limitations on the design conditions of distillation column, which are the column

height and height-to-diameter ratio. The general guidelines are column height, Hc < 54m and the

height-to-diameter ratio, Hc/Dc < 30 [James M.Douglas, 1988. “Conceptual Design of Chemical

Processes”, McGraw Hill, pg 457]

Previously, we calculated Hc = 22.77 m which is less than 54m. Thus, it is acceptable. On the

other hands, ratio Hc/Dc = 22.77/ 5.05= 4.51 (<30). Hence, it is acceptable.

2. Plate hydraulic design

Consider the preliminary specification of column T-101 on the basis of bottom section.

Column diameter, Dc= 5.05 m

Column area, Ac=20.04 m2

Net area, An= 16.03 m2

Downcomer area, Ad= 4.01 m

2

Step 1: Provisional plate design

Active area, 𝐴𝑎 = 𝐴𝑐 − 2𝐴𝑑 = 20.04 − 2(4.01) = 12.02 𝑚2

Assume all active holes take 6% of active area.

Hole area, 𝐴ℎ = 0.06𝐴𝑎 = 0.06(12.02) = 0.7212 𝑚2

Hole size/diameter:

234

The optimum size of hole that can be punched is twice the plate thickness. Due to handling

of heavy hydrocarbons in the column, large-sized hole will not susceptible to fouling. Thus,

hole size or diameter = 5 mm

Plate thickness = 2mm

Weir height, hw = 0.05m (suggestion from Coulson & Richardson)

Weir length, lw:

From figure 11.31 in Coulson & Richardson Chemical Engineering, Vol.6, 4th

edition,

when Ad/Ac X 100% = 20%; lw/Dc = 0.86

Thus, lw = 4.34m

Hole pitch, lp:

The normal range of hole pitch to diameter ratio is 2.5 to 4. Taking average value of the

range, assume hole pitch is 3.25 times of hole diameter.

𝑙𝑝 = 3.25(5) = 16.25𝑚𝑚 = 0.01625𝑚

Area of active hole:

𝐴ℎ = 𝜋(𝐷ℎ

2)2

= 𝜋(0.005

2)2

= 1.9635 × 10−5𝑚2

Number of holes per tray: 𝐴ℎ,𝑡𝑜𝑡𝑎𝑙

𝐴ℎ=

0.7212

1.9635×10−5 = 36730.3 ≈ 36731 ℎ𝑜𝑙𝑒𝑠

Step 3: Check weeping

The height of the liquid crest over the weir, how can be determined by using Francis weir formula:

ℎ𝑜𝑤 = 750[𝐿𝑤

𝑙𝑤 × 𝜌]2 3⁄

235

Maximum liquid rate = 31.64 kg/s

Minimum liquid rate at 70% Turndown Ratio = (0.70)(31.64) = 22.15 kg/s

Maximum how = 750 (31.64

625.754×4.34)

2

3= 38.54 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Minimum how= 750 (22.15

625.754×4.34)

2

3= 30.39 mm liquid

To ensure an even flow of liquid along the wier, the crest should be at least 10mm at the

lowest liquid rate. Thus, we chosen crest at 10mm at the lowest liquid rate.

At minimum liquid flow rate, how+hw= 30.39 + 40 =70.39mm

From Coulson and Richardson’s Chemical Engineering Design, Figure 11.30,

we get K2= 30.5

Minimum design vapour velocity,

𝑢ℎ =[𝐾2−0.90(25.4−𝑑ℎ)]

(𝜌𝑣)0.5

𝑢ℎ =[30.5−0.90(25.4−5)]

(20.098)0.5

= 2.71 𝑚/𝑠

Maximum vapour flowrate = 2.99 m3/s

Minimum vapour rate at 70% turndown ratio: 0.70(𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒)

𝐴ℎ=

0.7(2.99)

0.7212= 2.90 𝑚/𝑠

Actual minimum vapour velocity > weeping velocity, so minimum operating rate will be

well below weep point

Step 4: Determination of plate pressure drop

Maximum vapour flowrate, �̇�= 2.99 m3/s

Maximum vapour velocity through holes, 𝑢ℎ =�̇�

𝐴ℎ,𝑡𝑜𝑡𝑎𝑙=

2.99

0.7212= 4.15 𝑚/𝑠

Percentage of perforated area, 𝐴ℎ

𝐴𝑝× 100% ≈

𝐴ℎ

𝐴𝑎× 100% = 6%

Plate thickness/ hole diameter =2

5=0.4

236

From figure 11.34 (pg 576), Coulson & Richardson’s Chemical Engineering, vol.6, 4th

edition, the orifice coefficient Co can be estimated.

Thus, C0=0.69

Dry plate drop, hd:

ℎ𝑑 = 51[𝑢ℎ

𝐶𝑜]2

𝜌𝑉

𝜌𝐿

= 51(4.15

0.69)2 20.098

625.754

= 59.25 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Residual head, ℎ𝑟 =12500

𝜌𝐿,𝐵𝑜𝑡𝑡𝑜𝑚=

12500

625.754= 19.98 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Total pressure drop, ℎ𝑇 = ℎ𝑑 + (ℎ𝑤 + ℎ𝑜𝑤) + ℎ𝑟 = 149.62 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Step 5: Downcomer liquid backup

Height of the bottom edge of the apron above the plate, hap:

ℎ𝑎𝑝 = ℎ𝑤 − 10 = 40 − 10 = 30 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Clearance area under downcomer apron, Aap:

𝐴𝑎𝑝 = 𝑙𝑤ℎ𝑎𝑝 = 4.34 × 0.03 = 0.1302 𝑚2

237

As this is less than Ad, Aap is used

ℎ𝑑𝑐 = 166(𝐿𝑤𝑑

𝜌𝐿𝐴𝑚)2

= 166(31.64

625.754×0.1302)2

=25.04 mm

Back-up in downcomer

ℎ𝑏 = ℎ𝑑𝑐 + (ℎ𝑤 + ℎ𝑜𝑤) + ℎ𝑡

= 25.04 + (40 + 30.39) + 149.62

= 245.05 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

To avoid flooding, hb < (0.5)(tray spacing + weir height)

0.5(0.6+0.05)= 0.325 m

hb < 0.325 m. Thus, it can avoid flooding.

Contact/residence time, tr:

𝑡𝑟 =𝐴𝑑ℎ𝑏𝜌𝐿

𝐿𝑤𝑑

=4.01×(245.05×10−3)×625.754

31.64

= 19.43𝑠

A residence time of at least 3s is recommended. Since tr > 3s, thus it is acceptable.

Step 6: Check Entrainment

𝑢𝑣 =max𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒

𝐴𝑛

=2.99

16.03= 0.187 𝑚/𝑠

Percentage of flooding =𝑢𝑣

𝑉𝑛𝑓,𝑡𝑜𝑝=

0.187

0.291= 0.64 = 64%

Fractional entrainment

From figure 11.29 (pg 570) in Coulson & Richardson’s Chemical Engineering, vol.6, 4th

edition, the fractional entrainment is determined by using flooding percentage and FLV

value.

With FLV = 0.52 and 64% flooding, the fractional entrainment Ψ=0.001

238

The entrainment is below 0.1, thus it is acceptable.

1. Mechanical Design

Step 1: Design Pressure

The operating pressure of the column is 1000kPa. However, there is quite a lot of number of

plates and lead to a significant of pressure drop. It is predicted that pressure at bottom of the

column will be higher. Therefore, an extra 10% of pressure will be considered in mechanical

design.

Design pressure, Pi = 1100kPa

Step 2: Design temperature

Feed temperature, TF =75 oC

239

Distillate temperature, TD =67 oC

Bottom temperature, TB =120 oC

For design temperature, 10 oC is added to the operating temperature.

Design temperature, Ti = 120+10= 130 oC

Step 3: Material of construction and corrosion allowance

Carbon steel is selected as material of construction since we do not have corrosive material to

handle. Besides, it is the most commonly used engineering material. It is cheap and is available in

a wide range of standard forms and sizes. It can be easily worked and welded. It has good tensile

strength and ductility.

From table 13.2 Coulson & Richardson 6th

volume 4th

edition (pg 812), by interpolation, at T

=130 oC, the design stress is 119 N/mm

2, which is much higher than the column design pressure.

Hence, it is a suitable material of construction for this distillation column.

Step 4: Welded joint efficiency

The strength of a welded joint will depend on the type of joint and the quality of the welding. A

double welded butt type of welding is used for this distillation column to balance the tradeoff

between higher cost and higher strength of weld joint. The welded joint efficiency, J of this weld

joint is 0.85.

Step 5: Minimum Column Thickness

Internal diameter of column, Di = 5.05m = 5050 mm

Wall thickness is calculated based on Coulson & Richardson’s Chemical Engineering Design.

240

Minimum wall thickness, 𝑡 =𝑃𝑖𝐷𝑖

2𝐽𝑓−𝑃𝑖=

1.1×5050

2(0.85)(119)−1.21= 27.61𝑚𝑚

Take corrosion allowance of 2mm.

Thus, fabrication thickness of tube wall = 27.61 + 2 =29.61mm ≈ 30mm

The maximum allowable working pressure (MAWP) for this wall thickness is given by:

𝑀𝐴𝑊𝑃 =2 × 𝑡𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ × 𝑤𝑒𝑙𝑑 𝑗𝑜𝑖𝑛𝑡 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 × 𝑡

𝐷𝑖 + 𝑡

=2 × 360 × 0.85 × 30

5050 + 30= 3.6142 𝑁/𝑚𝑚2

Since MAWP is greater than the operating pressure, thus the thickness of column is

acceptable.

Step 6: Column head design

The type of head chosen is torispherical head. It is often used as the end closure of cylindrical

vessels. The shape is close to that of an ellipse but is easier and cheaper to fabricate. For

torispherical head, the head thickness is designed as below:

Crown radius, Rc=Di=5.05m

Knuckle radius, Rk=0.06 Rc=0.303m

𝐶𝑠 =1

4(3 + √

𝑅𝑐

𝑅𝑘)

=1

4(3 + √

5.05

0.303)

= 1.77

𝑡 =𝑃𝑖𝑅𝑐𝐶𝑠

2𝑓𝐽+𝑃𝑖(𝐶𝑠−0.2)

=1.1×5050×1.77

2(0.85)(119)+1.1(1.77−0.2)

= 48.19 mm

Take corrosion allowance of 2mm.

Fabrication thickness of vessel head = 48.19+2 = 50.19mm ≈51mm

The maximum allowable working pressure (MAWP) for this wall thickness is given by

𝑀𝐴𝑊𝑃 =2 × 𝑡𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ × 𝑤𝑒𝑙𝑑 𝑗𝑜𝑖𝑛𝑡 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 × 𝑡

𝐷𝑖 + 𝑡

=2 × 360 × 0.85 × 51

5050 + 51= 6.119 𝑁/𝑚𝑚2

Since MAWP is greater than the operating pressure, thus the thickness of head is

acceptable.

Step 7: L/D ratio of reactor

Column outer diameter = column inner diameter + 2 x column thickness

241

Do = Di + 2 x t = 5050 + 2 x 30 = 5110 mm = 5.110m

𝐿

𝐷𝑟𝑎𝑡𝑖𝑜 =

𝐻

𝐷𝑜=

22.77

5.110= 4.456

Since the L/D ratio < 30 , the column size is acceptable.

Step 8: Insulation Design

Rock wool is chosen as the insulation material as it can be used up to the temperature of 659 oC.

Rock wool has the density of 130 kg/m3 and the insulation thickness of 75 mm.

Step 9: Weight of vessel

The total weight of vessel consists of the column weight, tray weight and weight of insulation.

Each weight is calculated separately and summed up to get the total weight of vessel which is

required for stress analysis of the column. The weight of column is calculated based on formula in

Coulson & Richardson’s Chemical Engineering Design.

a. Weight of column

Take Cv = 1.15 as a factor to account for the weight of nozzle, manway, internal support

Mean diameter, Dm = Di + t = 5050+30=5080 mm =5.080m

Weight of column, Wt = 240CvDm(Hv+0.8Dm)t

= 240(1.15)(5.080)(22.77+0.8x5.080)(30)

= 1128702.44N=1128.70kN

b. Weight of trays

Weight of single tray = (An-Ah) x Plate thickness x Carbon steel density x g

= (16.03-0.7212) x (0.002) x (7787.40) x (9.81)

= 2339.01N = 2.34kN

Weight of trays = Weight of single tray x Number of trays

= 2.34 x 33= 77.22 kN

c. Weight of insulation

Vessel diameter, Dt = Column outer diameter + 2 x Insulation thickness

= 5.05 + 2 x 0.075

= 5.2m

Volume of insulation =𝜋(𝐷𝑡

2−𝐷𝑜2)

4𝐻 =

𝜋(5.22−5.052)

4(22.77) = 27.50𝑚3

Weight of insulation = 2 x volume of insulation x insulation material density x g

= 2 x 27.50 x 130 x 9.81

= 70141.5N = 70.14 kN

Total weight of distillation column, W = 1128.70+77.22+70.14 =1276.06 kN

Step 10: Stress analysis

Stress analysis must be made to ensure that the reactor structure is strong and safe. Stress

analysis is solely based on Coulson and Richardson’s Chemical Engineering Design.

a. Wind loading

Typically, wind pressure = 1280 N/m2 for preliminary design

Effective column diameter = Vessel diameter = 5.2m

Wind loading per unit length of column, Fw = 1280(5.2) = 6656 N/m

Bending moment at bottom tangent line, Mx =𝐹𝑤𝐻2

2

=6656(22.77)2

2= 1725477.81𝑁𝑚

242

Longitudinal stress, 𝜎ℎ =𝑃𝐷𝑖

2𝑡=

1.1(5050)

2(30)= 92.58𝑁/𝑚𝑚2

Circumferential stress, 𝜎𝐿 =𝑃𝐷𝑖

4𝑡=

1.1(5050)

4(30)= 46.29𝑁/𝑚𝑚2

Dead weight stress, 𝜎𝑊 =𝑊

𝜋(𝐷𝑖+𝑡)𝑡=

1276.06 × 1000

𝜋(5050+30)30= 2.665

𝑁

𝑚𝑚2

Second moment area of the vessel about the plane of bending, 𝐼𝑣 =𝜋

64(𝐷𝑜

4 − 𝐷𝑖4)

𝐼𝑣 =𝜋

64(51104 − 50504) = 1.544 × 1012𝑚𝑚4

Bending stress, 𝜎𝑏 = ±𝑀𝑥

𝐼𝑣(𝐷𝑖

2+ 𝑡) = ±

1725477.81(1000)

1.544×1012 (5050

2+ 30) = ±2.855𝑁/𝑚𝑚2

Total longitudinal stress, 𝜎𝑧 = 𝜎𝐿 + 𝜎𝑤 ± 𝜎𝑏

Since the vessel is above the support, so stress is applied from top of support, thus,

comprehensive (negative value)

𝜎𝑧(𝑢𝑝𝑤𝑖𝑛𝑑) = 46.29 − 2.665 + 2.855 = 46.48𝑁/𝑚𝑚2

𝜎𝑧(𝑑𝑜𝑤𝑛𝑤𝑖𝑛𝑑) = 46.29 − 2.665 − 2.855 = 40.77𝑁/𝑚𝑚2

Torsional shear stress needs not be considered in preliminary design.

Under this condition, the 3 principal stresses and their difference are calculated as shown:

Principle stress (N/mm2) Upwind Downwind

𝜎1 = 𝜎ℎ 92.58 92.58

𝜎2 = 𝜎𝑧 46.48 40.77

𝜎3 = 0.5𝑃 0.55 0.55

𝜎1 − 𝜎2 46.10 51.81

𝜎1 − 𝜎3 92.03 92.03

𝜎2 − 𝜎3 45.93 40.22

The greatest difference between the principal stresses will be on the down-wind side which

is 92.03 N/mm2. It is well below the maximum allowable design stress (119N/mm

2).

Hence, the design is acceptable.

Critical buckling stress, 𝜎𝑐 = 2 × 104 (𝑡

𝐷𝑜) = 2 × 104 (

30

5050) = 118.81 𝑁/𝑚𝑚2

Maximum compressive where the vessel is not under pressure

= 𝜎𝑤 + 𝜎𝑏 = 2.665 + 2.855 = 5.52 𝑁/𝑚𝑚2

The maximum compressive when vessel is not under pressure is below the critical

buckling stress. Thus, the design is satisfactory.

Step 11: Vessel support

Type of support chosen: Conical skirt (used for tall, vertical column)

Take skirt bottom diameter, Ds = 6m

Take skirt height, Hs = 4m

Skirt base angle, 𝜃𝑠 = tan−1 𝐻𝑠1

2(𝐷𝑠−𝐷𝑖)

= tan−1 41

2(6−5.05)

= 83.23𝑜

This angle is between 80o and 90

0, hence the skirt base angle is satisfactory.

The maximum dead weight load on the skirt will occur when the vessel is full of water.

Approximate water weight, 𝑊𝑤 = (𝜋

4× 𝐷𝑖

2 × 𝐻) × 1000 × 9.81

243

= (𝜋

4× 5.052 × 22.77) × 1000 × 9.81

= 4474089.58𝑁 = 4474.09𝑘𝑁

Take skirt thickness, ts be 9mm,

Bending moment at bottom of skirt, 𝑀𝑠 =𝐹𝑤(𝐻+𝐻𝑠)

2

2

=6656(22.77 + 4)2

2

= 2384954.29 𝑁𝑚

Bending stress in skirt, 𝜎𝑏𝑠 =4𝑀𝑠

𝜋(𝐷𝑠+𝑡𝑠)𝐷𝑠𝑡𝑠=

4(2384954.29)(103)

𝜋(6000+9)6000×9= 9.358 𝑁/𝑚𝑚2

Dead weight stress in the skirt, 𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) =𝑊𝑤

𝜋(𝐷𝑠+𝑡𝑠)𝑡𝑠=

4474089.58

𝜋(6000+9)9= 26.33 𝑁/𝑚𝑚2

𝜎𝑤𝑠(𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔) =𝑊

𝜋(𝐷𝑠 + 𝑡𝑠)𝑡𝑠=

1276.06 × 103

𝜋(6000 + 9)9= 7.51 𝑁/𝑚𝑚2

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) = 9.358 + 26.33 = 35.688 𝑁/𝑚𝑚2

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) = 9.358 − 7.51 = 1.848 𝑁/𝑚𝑚2

The skirt thickness should be such that under the worst combination of wind and dead-

weight loading, 2 design criteria must be satisfied. Choosing the skirt material to be carbon

steel, maximum allowable design stress at 20 oC is 135 N/mm

2. The young modulus of

stainless steel type 304 is 210000 MPa.

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑓𝑠𝐽 sin 𝜃

1.848 < (0.85)(135) sin 83.23𝑜

1.848 < 113.95

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸(𝑡𝑠

𝐷𝑠) sin 𝜃

35.688 < 0.125(210000)(9

6000) sin 83.23𝑜

35.688 < 39.10

Since both design criteria are satisfied, the skirt thickness is acceptable.

Take corrosion allowance of 2mm, skirt thickness =9+2=11mm

Step 12: Base ring and anchor bolt design

Take pitch circle diameter, Db =5.2m

Circumference of bolt circle = 5.2 X 103(π)= 16336.28 mm

Minimum bolt spacing is recommended at 600mm

No of bolts required =16336.28

600= 27.23 ≈ 28 𝑏𝑜𝑙𝑡𝑠 (𝑚𝑢𝑠𝑡 𝑏𝑒 𝑚𝑢𝑙𝑡𝑖𝑝𝑙𝑒 𝑜𝑓 4)

Bolt stress, fb = 125 N/mm2 (from Coulson & Richardson’s Chemical Engineering Design)

Area of bolt, 𝐴𝑏 =1

𝑁𝑏𝑓𝑏[4𝑀𝑠

𝐷𝑏− 𝑊] =

1

28(125)[4(2384954.29)

5.2− 1276.06 × 103]

= 159.58 mm2

Diameter of bolt= √𝐴𝑏×4

𝜋= √

159.98×4

𝜋= 14.27𝑚𝑚

Referring to Figure 13.2 Coulson & Richardson 6th

volume 4th

edition, the bolt size of

M24 (root area 353) is used.

Total compressive load on base ring, Fb

244

=4𝑀𝑠

𝜋𝐷𝑠2+

𝑊

𝜋𝐷𝑠=

4(2384954.29)

𝜋(6)2+

1276.06 × 103

𝜋(6)= 152047.59 𝑁/𝑚2

From Coulson and Richardson’s Chemical Engineering Design, maximum allowable

bearing pressure on concrete foundation pad, fc = 7 N/mm2

Minimum base ring width, 𝐿𝑏 =𝐹𝑏

𝑓𝑐×

1

1000=

152047.59

1

1000= 21.72𝑚𝑚

From figure 13.30 Coulson & Richardson Chemical Engineering, vol.6, 4th

edition, for

M24 bolts, Lr =150mm.

Actual base ring width = Lr + ts +50=150+9+50= 209mm

Actual bearing pressure on concrete foundation pad, f’c =152047.59

209×1000= 0.728 𝑁/𝑚𝑚2

Allowable design stress in ring material, fr=140 N/mm2 (From Coulson and Richardson’s

Chemical Engineering Design)

Minimum base ring thickness, tb = 𝐿𝑟√3𝑓𝑐

𝑓𝑟= 150√

3(0.728)

140= 18.73𝑚𝑚

Step 13: Nozzles Design

The Harker equation (1978), modified for SI unit, for the optimum pipe and nozzle

diameter:

For feed opening, 𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where W is mass flow rate in kg/hr and ρ is density of fluid in kg/m3

a. For feed inlet

𝐷𝑜𝑝𝑡 = 8.4143011.3880.45

676.400.31= 135.68 𝑚𝑚 = 5.34 𝑖𝑛 ≈ 6.0 𝑖𝑛

b. For top outlet

𝐷𝑜𝑝𝑡 = 8.4128280.6550.45

9.810.31= 417.40 𝑚𝑚 = 16.40 𝑖𝑛 ≈ 18.0 𝑖𝑛

c. For bottom outlet

𝐷𝑜𝑝𝑡 = 8.4174747.2930.45

625.750.31= 178.25 𝑚𝑚 = 7.02 𝑖𝑛 ≈ 8.0 𝑖𝑛

d. For reflux inlet

𝐷𝑜𝑝𝑡 = 8.4122624.5240.45

677.010.31= 101.59 𝑚𝑚 = 3.99 𝑖𝑛 ≈ 4.0 𝑖𝑛

e. For reboiler inlet

𝐷𝑜𝑝𝑡 = 8.4137392.0360.45

24.200.31= 42.54 𝑚𝑚 = 1.67 𝑖𝑛 ≈ 2.0 𝑖𝑛

Summary of nozzle design:

Stream W (kg/hr) Ρ (kg/m3) Dopt (in)

Feed Inlet 43011.388 676.40 6.0

Top Outlet 28280.655 9.81 17.0

Bottom Outlet 74747.293 625.57 8.0

Reflux Inlet 22624.524 677.01 4.0

Reboiler Inlet 37392.036 24.20 2.0

245

Absorber/Methanol Scrubber (T-102)

Design basis

Feed stream that is channelled into the absorption tower (T-102) consists of a mixture of methanol,

isobutylene, MTBE, butene, 1,3-butadiene and also butane. The total mass flow rate of feed is

5656.13 kg/hr at 393.15K and 700 kPa. The exit gas will flow to stream 15, carried out from the

top of the column operating at 343.15K and 100kPa whereas the bottom of the column operating

at 358.15K and 100kPa will be remove as the exit liquid through stream 16. The solvent stream

will enter this column through stream 28 that carries out 27639.06 kg/hr component at 334.81K

and 100kPa.

Cornell et al. (1960) reviewed the previously published data and presented empirical equations for

predicting the height of the gas and liquid film transfer units. Their correlation takes into account

the physical properties of the system, the gas and liquid flow-rates; and the column diameter and

height. By referring the textbook (Coulson and Richardson's Chemical Engineering), the

following calculation is performed.

From Mass Balance Spreadsheet, STREAM 14

𝑃𝑀𝑒𝑂𝐻,𝑓𝑒𝑒𝑑 = 𝑦𝑀𝑒𝑂𝐻,𝑓𝑒𝑒𝑑𝑃𝑓𝑒𝑒𝑑 =3.9969 𝑚3𝑀𝑒𝑂𝐻

8.1011 𝑚3𝑡𝑜𝑡𝑎𝑙 𝑔𝑎𝑠 𝑖𝑛 𝑓𝑒𝑒𝑑 × 700 𝑘𝑃𝑎

𝑃𝑀𝑒𝑂𝐻,𝑓𝑒𝑒𝑑 = 0.4934 × 700𝑘𝑃𝑎

𝑃𝑀𝑒𝑂𝐻,𝑓𝑒𝑒𝑑 = 345.36 𝑘𝑃𝑎 𝑀𝑒𝑂𝐻

From Mass Balance Spreadsheet, STREAM 15

𝑃𝑀𝑒𝑂𝐻,𝑒𝑥𝑖𝑡 = 𝑦𝑀𝑒𝑂𝐻,𝑒𝑥𝑖𝑡𝑃𝑒𝑥𝑖𝑡 =3.5379 𝑚3𝑀𝑒𝑂𝐻

4.2563 𝑚3𝑡𝑜𝑡𝑎𝑙 𝑔𝑎𝑠 𝑖𝑛 𝑒𝑥𝑖𝑡 × 100 𝑘𝑃𝑎

𝑃𝑀𝑒𝑂𝐻,𝑒𝑥𝑖𝑡 = 0.8312 × 100𝑘𝑃𝑎

𝑃𝑀𝑒𝑂𝐻,𝑒𝑥𝑖𝑡 = 9.4330 𝑘𝑃𝑎 𝑀𝑒𝑂𝐻

𝐹𝑒𝑒𝑑 𝑖𝑛𝑙𝑒𝑡 𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 =5656.131𝑘𝑔

ℎ×

1ℎ

3600𝑠= 1.5711𝑘𝑔/𝑠

𝐹𝑒𝑒𝑑 𝑖𝑛𝑙𝑒𝑡 𝑚𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 140.91𝑘𝑚𝑜𝑙/ℎ

Solubility data

Since methanol is soluble in water (solvent), operation at atmospheric pressure should be

satisfactory. (Source: Bayer R.: Die Dampfdrücke des binären Systems Methylalkohol-Wasser.

Z.Phys.Chem.(Leipzig) 130 (1927) 1-14)

MeOH

Partial

Pressure

gas, kPa 9.079 11.412 11.506 13.012 13.786 14.639 15.785 15.879 16.319 17.599 18.425

per cent

w/w

solution 0.0820 0.1535 0.1535 0.2151 0.2422 0.2820 0.3120 0.3114 0.3377 0.3793 0.4168

246

MeOH

Partial Pressure

gas, kPa 19.025 20.705 21.532 22.318 23.385 25.091 26.998 27.518 29.744 32.571

per cent w/w

solution 0.4401 0.5126 0.5601 0.5791 0.6431 0.7218 0.7996 0.8020 0.8769 0.9576

From the data, a linear graph can be approximated and its equation is shown in the graph (Figure 1)

below as well.

Figure 1: Graph of Partial Pressure of MeOH vs Solubility of MeOH in H2O

Slope of equilibrium line

Based on the equation, when solubility of MeOH in water is 1.5% w/w MeOH, the partial

pressure need to be exerted is 45.301 kPa.

Mole fraction in vapour =45.301

700= 0.06472

Mole fraction in liquid =1.5

32.042⁄

1.532.042⁄ + 98.5

18.015⁄= 0.008489

𝑚 =0.06472

0.008489= 7.6240

To decide the most economic water flow-rate, absorption design must be taken into our

consideration. Using Figure 2, the number of stages required at different water rates will be

determined and the “optimum” rate chosen: 𝑦1

𝑦2=

𝑝1

𝑝2=

345.36 𝑘𝑃𝑎

9.43 𝑘𝑃𝑎= 34.62

𝑚𝐺𝑚

𝐿𝑚 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

NOG 3.9 4.2 4.6 5 5.8 7.1 8 10.1 13.8

y = 25.09x + 7.666 R² = 0.9962

0

5

10

15

20

25

30

35

0.00 0.20 0.40 0.60 0.80 1.00 1.20Par

tial

Prs

sure

of

MeO

H (

kPa)

Solubility of MeOH in H2O (wt./wt.)

Partial Pressure of MeOH vs Solubility of MeOH in H2O

247

It can be seen that the “optimum” will be between the value of m(Gm/Lm) ranged from 0.5 to 0.7,

as would be expected. Below 0.5 there is only a small decrease in the number of stages required

with increasing liquid rate; and above 0.7 the number of stages increases rapidly with decreasing

liquid rate. For this case, to ensure better efficiency for the absorption to occur, 0.7 is chosen.

Thus:

NOG = 8

𝑚𝐺𝑚

𝐿𝑚= 0.7

𝐿𝑚 =7.6240 × 140.91𝑘𝑚𝑜𝑙/ℎ𝑟

0.7= 1534.71𝑘𝑚𝑜𝑙/ℎ𝑟

Since 𝐿𝑚 assume to consist of only pure water (𝑀𝑊𝐻2𝑂 ≈ 18),

𝐿𝑚 = 27624.78 𝑘𝑔 𝐻2𝑂/ℎ𝑟 = 7.67355 𝑘𝑚𝑜𝑙 𝐻2𝑂/𝑠

Figure 2: Number of transfer units NOG as a function of y1/y2 with 𝑚𝐺𝑚

𝐿𝑚 as parameter

Column diameter

The physical properties of the gas inlet are calculated based on the fraction of each of the gas

components exists in the gas stream.

𝐺𝑎𝑠 𝑖𝑛𝑙𝑒𝑡 𝑀𝐴𝑆𝑆 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 5656.131𝑘𝑔

ℎ= 1.5711

𝑘𝑔

𝑠

248

𝐺𝑎𝑠 𝑖𝑛𝑙𝑒𝑡 𝑀𝑂𝐿𝐴𝑅 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒

=

2079.954𝑘𝑔ℎ

56𝑘𝑔𝑘𝑚𝑜𝑙

+

3257.536𝑘𝑔ℎ

32𝑘𝑔𝑘𝑚𝑜𝑙

+

366.587𝑘𝑔ℎ

88𝑘𝑔𝑘𝑚𝑜𝑙

+

26.092𝑘𝑔ℎ

56𝑘𝑔𝑘𝑚𝑜𝑙

+

13.046𝑘𝑔ℎ

54𝑘𝑔𝑘𝑚𝑜𝑙

+

12.916𝑘𝑔ℎ

58𝑘𝑔𝑘𝑚𝑜𝑙

= 140.91𝑘𝑚𝑜𝑙

ℎ= 0.0391

𝑘𝑚𝑜𝑙

𝑠

Select 38 mm (1.5 in.) ceramic Intalox saddles.

From Table 1 below, Fp = 170 m-1

Table 1: Design data for various packings

By considering all the components present in both the gas and liquid stream, the representative

density can be obtained:

Gas density, 𝜌𝑉 = 3.01 kg/m3

Liquid density, 𝜌𝐿 = 999.85 kg/m3

Liquid viscosity, 𝜇𝐿= 0.315 x 10-3

N s/m2

𝐿𝑤∗

𝑉𝑤∗

=𝐿𝑚

𝐺𝑚=

27624.78 𝑘𝑔/ℎ𝑟

5656.13𝑘𝑔/ℎ𝑟

𝐿𝑤∗

𝑉𝑤∗ √

𝜌𝑉

𝜌𝐿=

27624.78

5656.13∙ √

3.01

999.85= 0.2680

Design for a pressure drop of 20 mm H2O/m (0.1kPa/m) packing, and from Figure 3,

K4 = 0.65

At flooding K4 = 2.0

Percentage flooding = √0.65

2.0× 100 = 57.01%

249

Figure 3: Generalised pressure drop correlation, adapted from a figure by the Norton Co. with

permission

Based on equation below,

Gas mass flow-rate can be calculated by rearranging,

(𝑉𝑤∗)2 =

𝐾4 × 𝜌𝑉(𝜌𝐿 − 𝜌𝑉)

13.1 × 𝐹𝑝 × (𝜇𝐿

𝜌𝐿)0.1

𝑉𝑤∗ =

0.65 × 3.01(999.85 − 3.01)

13.1 × 170 × (0.315 × 10−3

999.85)0.1 = 1.9782

𝑘𝑔

𝑚2 ∙ 𝑠

250

The area of the absorption column,

𝐶𝑜𝑙𝑢𝑚𝑛 𝑎𝑟𝑒𝑎 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 =𝑉𝑤

𝑉𝑤∗=

5656.13𝑘𝑔ℎ𝑟

×ℎ𝑟

3600𝑠

1.9782 𝑘𝑔

𝑚2 ∙ 𝑠

= 0.7942𝑚2

𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 = √4

𝜋× 0.7942 = 1.0056 𝑚

Round off to 1.10 m

𝐶𝑜𝑙𝑢𝑚𝑛 𝑎𝑟𝑒𝑎 =𝜋𝐷2

4=

𝜋(1.12)

4= 0.9503𝑚2

Percentage flooding at selected diameter,

57.01% ×0.8068𝑚2

0.9503𝑚2= 48.01% 𝑓𝑙𝑜𝑜𝑑𝑖𝑛𝑔 (𝑠𝑎𝑡𝑖𝑠𝑓𝑎𝑐𝑡𝑜𝑟𝑦)

Estimation of HOG

Cornell’s method

At operating temperature,

Gas viscosity, 𝜇𝑉 = 0.1144 x 10-5

N s/m2

Diffusivity of MeOH, Dv = 1.64 x 10-5

m2 /s

Diffusivity of Water, DL= 1.7 x 10-9

m2 /s

Schmidt number, Sc = 𝑣𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦,𝑣

(𝑑𝑒𝑛𝑠𝑖𝑡𝑦,𝜌)×(𝐷𝑖𝑓𝑓𝑢𝑠𝑖𝑣𝑖𝑡𝑦,𝐷)

Gas Schmidt number, (Sc)v = 0.315 x 10−3

3.01×1.64 x 10−5= 6.38

Liquid Schmidt number, (Sc)L = 0.1144x 10−4

999.85×1.7 x 10−9 = 6.73

𝐿𝑖𝑞𝑢𝑖𝑑 𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑝𝑒𝑟 𝑢𝑛𝑖𝑡 𝑎𝑟𝑒𝑎, 𝐿𝑊∗ =

27624.78 3600⁄

0.9503= 8.0749 𝑘𝑔/𝑚2 ∙ 𝑠

Based on Figure 4, at 47.65% flooding, K3 = 0.97

From Figure 5, at 47.65% flooding, ψh = 80

From Figure 6, at 𝐿𝑊∗ = 8.0749, ϕh = 0.07

251

Cornell’s equations are,

As the solvent used considered as pure water in this design calculation,

f1= f2= f3= 1

1) HG = [0.0011(80)(6.38)0.5

(1.1/0.305)1.11

(Z/3.05)0.33

]/[7.6119(1)(1)(1)]0.5

i. HG = 0.3346(Z/3.05)0.33

2) HL= 0.305(0.07)(6.73)0.5

(0.97)(Z/3.05)0.15

i. HL=0.0537(Z/3.05)0.15

3) HOG = HG + 𝑚𝐺𝑚

𝐿𝑚 HL ; 𝑚

𝐺𝑚

𝐿𝑚= 0.7

4) Z = HOG NOG ; NOG = 8

By using goalseek tool in Microsoft Excel, Equation (1) to Equation (4) above can be solved

to obtain the height of the column. HOG is calculated to be around 0.375 m, and the obtained

column height, Z is 3.002 m.

∴ 𝑃𝑎𝑐𝑘𝑒𝑑 𝑏𝑒𝑑 ℎ𝑒𝑖𝑔ℎ𝑡, 𝑍 = 3.002 𝑚

252

Figure 4: Percentage flooding correction factor

Figure 5: Factor for HG for Berl saddles

Figure 6: Factor for HL for Berl saddles

253

Mechanical Design

Design pressure

The operating pressure of the column is 700 kPa. However since ceramic Intalox saddles are

chosen as the packings in the column, there is significant pressure drop. It is predicted that

pressure at bottom of the column will be lower. Anyway, for the safety purpose, an extra 10% of

pressure will be considered in mechanical design.

Design Pressure, Pi = 770kPa

Design temperature

Feed temperature, TF = 383.15 K

Exit gas temperature, Tg = 343.15 K

Exit liquid temperature, Tl = 358.15 K

Solvent temperature, Ts = 335.15 K

For design temperature, 10oC is added to the operating temperature

Design temperature, Ti = 110 oC + 10

oC = 120

oC =393.15K

Material of construction and corrosion allowance

Stainless steel type 304 is selected as material of construction since it is corrosion resistance to

most chemical substances. Referring to Table 13.2 Coulson & Richardson 4th edition page 812:

By interpolation, at temperature of 120oC,

Design stress, f = 141 N/mm2

Welded joint factor

The strength of a welded joint will depend on the type of joint and the quality of the welding

From the Coulsons & Richardsons Chemical Engineering Design, 4th edition, page 813

254

A double welded butt type of welding is used for this reactor to balance the trade-off between

higher cost and higher strength of weld joint. Thus:

Type of joint chosen = double welded butt or equivalent

Joint factor, J = 0.85

Wall thickness

Cylindrical section

From calculation above (Cornell’s method),

Internal diameter, Di = 1.1 m

𝑀𝑖𝑛𝑖𝑚𝑢𝑛 𝑤𝑎𝑙𝑙 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠, 𝑡𝑚𝑖𝑛 =𝐷𝑒𝑠𝑖𝑔𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 × 𝐼𝑛𝑡𝑒𝑟𝑛𝑎𝑙 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟

(2 × 𝐷𝑒𝑠𝑖𝑔𝑛 𝑆𝑡𝑟𝑒𝑠𝑠 × 𝐽) − 𝐷𝑒𝑠𝑖𝑔𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒

𝑀𝑖𝑛𝑖𝑚𝑢𝑛 𝑤𝑎𝑙𝑙 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠, 𝑡𝑚𝑖𝑛 =(770 × 0.001)𝑁/𝑚𝑚2 × (1.1 × 1000)𝑚𝑚

(2 × 141 𝑁/𝑚𝑚2 × 0.85) − (770 × 0.001)𝑁/𝑚𝑚2

𝑀𝑖𝑛𝑖𝑚𝑢𝑛 𝑤𝑎𝑙𝑙 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠, 𝑡𝑚𝑖𝑛 = 3.54𝑚𝑚 ≈ 4𝑚𝑚

Setting corrosion allowance which makes the wall thicker by 2 mm, the effective wall thickness is:

Effective thickness, teff = tmin + corrosion allowance = (4 + 2) mm = 6mm

Head and closures

Torispherical heads is in torispherical shape, which is extensively used as the end closure for a

large variety of cylindrical pressure vessels. These are formed from part of a torus and part of a

sphere. The shape is close to that of an ellipse but is easier and cheaper to fabricate. Since crown

radius should not be greater than the diameter of the cylindrical section, so we fix the radius less

than diameter of column. Figure below shows a typical torispherical head.

255

Crown radius, Rc = Di/2 = 0.60 m

To avoid buckling, The ratio of the knuckle to crown radii should not be less than 0.06. So:

Knuckle radius, Rk = 0.06 x Rc = 0.036 m

Minimum thickness of head:

Stress concentration factor, Cs:

𝐶𝑠 =1

4× (3 + √

𝑅𝑐

𝑅𝑘)

𝐶𝑠 =1

4× (3 + √

0.55

0.033) = 1.7706

Minimum thickness of head:

𝑒 =(770×0.001)𝑁/𝑚𝑚2×0.60×1.7706

(2×141 𝑁/𝑚𝑚2×0.85)+[(770×0.001)𝑁/𝑚𝑚2]∙(1.7706−0.2)= 3.3954 mm

Stress analysis

Preliminary specifications:

Density stress 141 N/mm2

Density of material (Stainless Steel 304) 8000 kg/m3

Density of packing (1.5in Intalox saddlers ceramic) 625 kg/m3

Design pressure 770 kPa

Corrosion allowance 2 mm

Inner column diameter 1.19994 m

Height of column 4.3975 m

Joint factor 0.85

Wind pressure 1280 N/m2

Insulation 75 mm

Mineral wool density (as insulation material) 130 kg/m3

256

Deadweight of vessel

For vessel

Mean diameter, Dm = Di + 2 x teff = 1.19994m + 2 (9.53/1000) m = 1.219 m

Shell weight, Wv = Cv 𝜋 𝜌m Dm g (Hv+0.8Dm) ts

Wv = 1.15 x 3.142 x 8000 kg/m3 x 1.19994m x 9.81m

2/s x [4.3975m + 0.8(1.219m)] x

[(9.53/1000) m]

Wv = 17420.21 N = 17.4202 kN

For insulation layer

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛, 𝑉𝑖 = 𝜋𝐷𝑖𝑡𝑖𝐻𝑣 = 3.142 × 1.19994𝑚 × 0.075𝑚 × 4.3975𝑚

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛, 𝑉𝑖 =1.2433 m3

𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛 = 𝜌𝑖𝑉𝑖𝑔 = 130𝑘𝑔

𝑚3× 1.2433𝑚3 × 9.81

𝑚2

𝑠

𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛 = 1585.59 N = 1.5856 kN

To consider the fitting weight, the weight of insulation is doubled as suggested in the

textbook.

𝑇𝑜𝑡𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛,𝑊𝑖 = 2𝜌𝑖𝑉𝑖𝑔 = 3171.18 𝑁 = 3.1712 𝑘𝑁

For packing

Volume of packed bed in the column = 3.3948 m3

257

Mass/Weight of packing in the column, Wp = 2121.78 kg = 20814.63 N = 20.8146 kN

Total dead weight, Wtotal = Wv +Wp +Wi

Wtotal = 17.4203 kN + 1.5856 kN + 20.8146 kN

Wtotal = 38.8204 kN

Wind loading

Take dynamic wind pressure as 1280 N/m2.

Mean diameter (including insulation) = 1.219m + 2(0.075m) = 1.369m

Loading, Fw = 1280 N/m x 1.369m = 1752.32 N/m

Bending moment, Mx = 𝐹𝑊𝐻𝑉

2

2=

1752.32𝑁

𝑚×(4.3975𝑚)2

2= 16943.34 𝑁𝑚

Analysis of stresses

The longitudinal and circumferential stresses due to pressure (internal or external) given by:

Longitudinal, 𝜎𝐿 =𝑃𝑑𝐷𝑖

4𝑡𝑠=

(770×0.001)𝑁/𝑚𝑚2×(1.19994×1000)𝑚𝑚

4×9.53𝑚𝑚= 24.2380𝑁/𝑚𝑚2

Circumferential, 𝜎ℎ =𝑃𝑑𝐷𝑖

2𝑡𝑠=

(770×0.001)𝑁/𝑚𝑚2×(1.19994×1000)𝑚𝑚

2×9,53𝑚𝑚= 76.9962𝑁/𝑚𝑚2

Direct (due to weight),𝜎𝑊 =𝑊𝑇𝑜𝑡𝑎𝑙

𝜋(𝐷𝑖+𝑡𝑠)𝑡𝑠=

26702.3𝑁

𝜋[(1.19994×1000)𝑚𝑚+9,53𝑚𝑚](9,53𝑚𝑚) 1.7518N/mm

2

Bending Stress

Do = Di + 2 x t = 1199.94 mm + 2(9.53 mm) =1219 mm

Second moment of area of the vessel, 𝐼𝑣 =𝜋

64(𝐷4 − 𝐷𝑠

4) = 6621632147.69

𝜎𝑏 = ±𝑀𝑥

𝐼𝑣(𝐷𝑠

2+ 𝑡𝑠) = ± 1.5596 N/mm

2

Resultant longitudinal stress, 𝜎𝑧 = 𝜎𝐿−𝜎𝑤 ± 𝜎𝑏

Upwind: 𝜎𝑧 = 𝜎𝐿−𝜎𝑤 + 𝜎𝑏 = 24.04583 N/mm2

Downwind: 𝜎𝑧 = 𝜎𝐿−𝜎𝑤 − 𝜎𝑏= 20.92667 N/mm2

The greatest difference between the principal stresses will be on the up-wind side.

Stress difference = 𝜎ℎ − 𝜎𝑧(𝑑𝑜𝑤𝑛𝑤𝑖𝑛𝑑) =76.9962N/mm2 – 20.9267 N/mm

2

Stress difference = 56.06948 N/mm2 (well below the maximum allowable design stress)

Vessel Support

Type of Support Chosen: Skirt

After trial and error, we decided that a conical skirt support would be used.

By assuming the skirt's diameter bottom, Ds = 1.3659 m and skirt height = 2 m

𝑡𝑎𝑛 𝜃𝑠𝑘𝑖𝑟𝑡 =𝐻𝑠𝑘𝑖𝑟𝑡

12

(𝐷𝑠𝑘𝑖𝑟𝑡 − 𝐼𝐷𝑠)

258

The skirt base angle,𝜃𝑠 = 87.62° is acceptable which is within common range of 80° 𝑡𝑜 90°

From Coulson & Richardson's chemical engineering, at 120oC (design temperature)

Design Stress = 141N/mm2

Young's Modulus, E = 200000 N/mm2

The maximum dead weight load on the skirt will occur when the vessel is full of water.

𝑊𝑒𝑖𝑔ℎ𝑡 𝐸𝑠𝑡𝑖𝑚𝑎𝑡𝑒𝑑 =𝜋 × 𝐷𝑖

2 × 𝐻𝑉

4× 1000 × 9.81

Weight Estimated = 48784.94 N = 48.7849 kN

Weight of vessel = 39.8204 kN

Total weight (include hydraulic loading), Whydraulic = 48.7849 kN + 39.8204 kN = 88.6053 kN

From previous,

Wind Loading = 1280 N/m2

𝐵𝑒𝑛𝑑𝑖𝑛𝑔 𝑚𝑜𝑚𝑒𝑛𝑡 𝑜𝑓 𝑏𝑎𝑠𝑒 𝑠𝑘𝑖𝑟𝑡,𝑀𝑠 =1

2𝐹𝑊(𝐻𝑉 + 𝐻𝑠𝑘𝑖𝑟𝑡)

2

=1

2(1752.32

𝑁

𝑚) (4.3975𝑚 + 2𝑚)2 = 35859.71 𝑁𝑚

Take the skirt thickness as the same as that of the thickness of the vessel = 9.53 mm

𝐵𝑒𝑛𝑑𝑖𝑛𝑔 𝑠𝑡𝑟𝑒𝑠𝑠 𝑖𝑛 𝑡ℎ𝑒 𝑠𝑘𝑖𝑟𝑡, 𝜎𝑏𝑠 =4𝑀𝑠

𝜋(𝐷𝑖 + 𝑡𝑠)𝑡𝑠𝐷𝑖

𝜎𝑏𝑠 = 35859.71×1000 𝑁𝑚𝑚

𝜋[(1.19994×1000)𝑚𝑚+6𝑚𝑚](9.53𝑚𝑚)(1.19994×1000𝑚𝑚)= 3.3012 N/mm

2

𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 𝑠𝑡𝑟𝑒𝑠𝑠 𝑖𝑛 𝑡ℎ𝑒 𝑠𝑘𝑖𝑟𝑡, 𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) =𝑊ℎ𝑦𝑑𝑟𝑎𝑢𝑙𝑖𝑐

𝜋(𝐷𝑖 + 𝑡𝑠)𝑡𝑠

𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) = 88605.37𝑁

𝜋[(1.19994×1000)𝑚𝑚+9.53𝑚𝑚](9.53𝑚𝑚)= 2.4469 N/mm

2

***the "test" condition is with the vessel full of water for the hydraulic test. In estimating total

weight, the weight of liquid on the plates has been counted twice. The weight has not been

adjusted to allow for this as the error is small, and on the "safe side".

𝜎𝑤𝑠(𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔) =𝑊𝑣𝑒𝑠𝑠𝑒𝑙

𝜋(𝐷𝑖+𝑡𝑠)𝑡𝑠=

26702.3𝑁

𝜋[(1.1×1000)𝑚𝑚+6𝑚𝑚](6𝑚𝑚)=1.2808 N/mm

2

Maximum σ̂s(compressive) = 𝜎𝑏𝑠 + 𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) = 3.3012 N/mm2 + 2.4469 N/mm

2

Maximum σ̂s(compressive) = 5.7481 N/mm2

Maximum σ̂s(tensile) = 𝜎𝑏𝑠 + 𝜎𝑤𝑠(𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔) = 3.3012 N/mm2 + 1.0997 N/mm

2

Maximum σ̂s(tensile) =2.2015 N/mm2

Design Criteria

The skirt thickness should be such that under the worst combination of wind and dead weight

loading, 2 design criteria must be satisfied:

259

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑓𝑠𝐽 sin 𝜃𝑠

∴ 𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸 (𝑡𝑠𝐷𝑠

) 𝑠𝑖𝑛𝜃𝑠

From previous, Joint efficiency, J = 0.85

𝑓𝑠𝐽 sin 𝜃𝑠 = 141 N/mm2 x 0.85 sin (87.62

o) = 119.7466 N/mm

2

∴ 𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑓𝑠𝐽 sin 𝜃𝑠

0.125𝐸 (𝑡𝑠

𝐷𝑠) 𝑠𝑖𝑛𝜃𝑠 =0.125(20000N/mm

2)(9,53mm/(1.1 x 1000mm))sin(88.57

o) = 67.0737 N/mm

2

∴ 𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸 (𝑡𝑠𝐷𝑠

) 𝑠𝑖𝑛𝜃𝑠

Both criteria are satisfied.

Base Ring and Anchor Bolts design

Take the pitch circle diameter (Ds) approximately 1.2 m

Circumference of bolt circle = π x (1000 x 1.2) = 3769.91 mm

Minimum bolt spacing is recommended at 600 mm

No. of bolts required at minimum recommended spacing = 3769.91mm / 600mm = 6.28

Since the no. of bolts must be multiple of 4, so, 4 bolts are chosen.

Bolt stress, fb = 141 N/mm2

Area of bolt, Ab =1

Nbfb[4Ms

Db− W] =

1

4(141N/m𝑚2)[4(35859.71×1000)Nmm

(1.2×1000)mm− 39820.43N]

Ab = 141.33 m𝑚2

Diameter of bolt = √𝐴𝑏×4

𝜋= √

93.25×4

𝜋= 13.41 𝑚𝑚

Scheiman (Coulson & Richardson`s Chemical Engineering) suggest that the minimum bolt`s

diameter of 18.45 mm should be used for supporting the vessel, by referring to Table 13.30

(Coulson & Richardson`s Chemical Engineering, 4th edition, pg 852), the bolt size of M24 (root

area 353 mm2) is used.

Total compressive load on base ring, 𝐹𝑏 =4𝑀𝑠

𝜋𝐷𝑠𝑘𝑖𝑟𝑡2 +

𝑊

𝜋𝐷𝑠𝑘𝑖𝑟𝑡= 42273.34 N/m

Take maximum allowable bearing pressure on concrete foundation pad, fc = 5 N/mm2

260

𝑀𝑖𝑛𝑖𝑚𝑢𝑛 𝑤𝑖𝑑𝑡ℎ 𝑜𝑑 𝑏𝑎𝑠𝑒 𝑟𝑖𝑛𝑔, 𝐿𝑏 =𝐹𝑏

𝑓𝑐=

32758.25 N/m

5 𝑁/𝑚𝑚2= 8.4547 mm

This is the minimum width required; actual width will depend on the chair design.

Let distance from the edge of the skirt to the outer edge of the ring, Lr = 200 mm

Actual width required = Lr + ts +50mm = 200mm + 6mm + 50mm = 259.53 mm

Actual bearing pressure on base, fc' = 𝐹𝑏

𝐴𝑐𝑡𝑢𝑎𝑙 𝑤𝑖𝑑𝑡ℎ=

42273.34 N/m

259.53 𝑚𝑚 = 0.1629 N/mm

2

Let allowable design tressinring material, fr = 140 N/mm2

Maximum thickness, tb =𝐿𝑟√3𝑓′

𝑐

𝑓𝑟= 11.8159𝑚𝑚 ≈ 12𝑚𝑚

Nozzles Design

The Harker equation (1978), modified for SI unit, for the optimum pipe (and nozzle) diameter:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

where W is mass flow rate (kg.hr) and ρ is density of fluid (kg/m3)

From mass balance spreadsheet,

Stream W (kg/hr) ρ (kg/m3)

Feed Inlet (14) 5656.131 739.6562

Exit Gas (15) 2681.945 731.6309

Exit liquid (16) 22598.22 987.7776

Solvent (28) 27639.06 999.939

For feed inlet:

Dopt = 52.97 mm = 2.09 in.

The nearest standard pipe which is bigger than the optimum is selected.

∴ 3 in. diameter nozzle is used.

For exit gas

Dopt = 37.99 mm = 1.50 in.

The nearest standard pipe which is bigger than the optimum is selected.

∴ 2 in. diameter nozzle is used.

For exit liquid

Dopt = 90.32 mm = 3.56 in.

The nearest standard pipe which is bigger than the optimum is selected.

∴ 4 in. diameter nozzle is used.

For solvent

Dopt = 98.51 mm = 3.88 in.

The nearest standard pipe which is bigger than the optimum is selected.

∴ 4 in. diameter nozzle is used.

261

Distillation Column, T-103

Design Criteria:

This distillation column is used to separate methanol from mixture of MTBE and water. The recover

methanol and water can recycle back to the feed.

Design Parameters:

Component

Distribution

Column Sizing Plate Hydraulic

Design

Mechanical Design

Number of Stages Tray Spacing Active Area Design Pressure

Reflux Ratio Flooding Velocity Hole Area Design Temperature

Number of Actual

Stages

Net Area Tray Thickness Material of

Construction

Tray Efficiency Downcomer Area Hole Diameter Column Wall

Thickness

Location of Feed

Stage

Column Diameter Liquid Flow

Arrangement

Column Head Design

Column Height Column Pressure Drop Insulation

Weeping Checking Stress Analysis

Downcomer Liquid

Backup

Column Support

Residence Time Nozzle Size

Entrainment Checking

Number of Holes

Design Basic:

Feed stream into the distillation column T-103 consist of a mixture of methanol, water and MTBE. The

total mass flow rate of feed is 30533.095 kg/hr at 85 oC and 100kPa. Distillate is carried out from the top of

the column operating at 38 oC and 100kPa. On the other hand, the bottom of column operate at 90

oC and

100kPa.

Design Method:

Fenske-Underwood-Gilliland method is used for component distribution calculation. The column sizing,

plate hydraulic design and mechanical design of the distillation column is based on Coulson and

Richardson’s Chemical Engineering Design and Ray Sinnott and Gavin Towler’s Chemical Engineering

Design.

2. Component Distribution:

Step 1: Identification of Light Key (LK) and Heavy Key (HK) Component

Methanol is light key component, water is heavy key component and MTBE is light non-key component.

Step 2: Relative Volatility Calculation

Relative volatility is calculated from the volatility of respective component, which is determined from the

partial pressure of component and the system pressure. Partial pressure of component is determined from

Antoine’s equation. The Antoine Equation is stated as

log10 𝑝 = 𝐴 −𝐵

𝑇 + 𝐶

262

Where p= vapour pressure(mmHg)

A,B,C= regression coefficients for chemical compound

T= temperature(oC)

The constant for each component as stated below which get from Richard M.Felder and Ronald’s

Elementary Principles of Chemical Processes:

Components A B C

Methanol 7.87863 1473.110 230.0

Water (0-60 oC) 8.10765 1750.286 235.0

Water (60-150 oC) 7.96681 1668.210 228.0

MTBE 5.89600 708.690 179.9

Component

TF = 85 oC TD =33

oC TB =100

oC

vapor pressure α vapor pressure α vapor pressure α

Methanol 2.12 3.67 0.25 5.02 3.46 3.42

Water 0.58 1.00 0.05 1.00 1.01 1.00

MTBE 2.22 3.83 0.49 9.78 3.08 3.04

𝑊ℎ𝑒𝑟𝑒 𝛼𝐿𝐾/𝐻𝐾 =𝑃𝐿𝐾

𝑠𝑎𝑡

𝑃𝐻𝐾𝑠𝑎𝑡

𝛼𝑎𝑣𝑔 = (3.67 × 5.02 × 3.42)13

= 3.98

Step 3: Minimum number of stages, Nmin

Component XB XD 𝛼𝐿𝐾/𝐻𝐾

Methanol (LK) 0.0006 0.8234 3.98

Water (HK) 0.9994 0.0350

𝑁𝑚𝑖𝑛 =ln[(

𝑥𝐿𝐾𝑥𝐻𝐾

)𝐷 × (𝑥𝐻𝐾𝑥𝐿𝐾

)𝐵

ln[𝛼𝐿𝐾𝛼𝐻𝐾

]

=ln [(

0.82340.0350

) × (0.99940.0006)]

ln 3.98 = 7.63 𝑠𝑡𝑎𝑔𝑒𝑠

Step 4: Minimum reflux ratio, Rmin

Before calculating R, minimum reflux ratio, Rmin is determined by using the Underwood equation:

∑𝛼𝑖𝑥𝐹,𝑖

𝛼𝑖 − 𝜃= 1 − 𝑞

𝑛

𝑖=1

263

At feed condition (85 oC, 100kPa), the feed exist as saturated liquid. Thus q=1 since vapor

fraction=0.

Component XB XD α(TF) XF

methanol 0.0006 0.8234 3.673032122 0.0553

water 0.9994 0.035 1 0.9423

MTBE 0 0.1417 3.833742776 0.0023

3.67 × 0.0553

3.67 − 𝜃+

0.9423 × 1.00

1.00 − 𝜃+

3.83 × 0.0023

3.83 − 𝜃= 0

By using SOLVER in Excel, we get the value of θ=3.186

Minimum reflux ratio, Rmin can be determined by using θ value through the equations:

𝑅𝑚𝑖𝑛 + 1 = ∑𝛼𝑖𝑥𝐷,𝑖

𝛼𝑖 − 𝜃𝑖

For θ=3.186,

𝑅𝑚𝑖𝑛 + 1 =𝛼𝐿𝐾𝑥𝐷,𝐿𝐾

𝛼𝐿𝐾 − 𝜃+

𝛼𝐻𝐾𝑥𝐷,𝐻𝐾

𝛼𝐻𝐾 − 𝜃+

𝛼𝑁𝐾𝑥𝐷,𝑁𝐾

𝛼𝑁𝐾 − 𝜃

𝑅𝑚𝑖𝑛 + 1 =3.67 × 0.8234

3.67 − 3.186+

1.00 × 0.1417

1.00 − 3.186+

3.83 × 0.035

3.83 − 3.186

Rmin = 6.04

Step 5: Determination of reflux ratio, R

According to rule of thumb, actual reflux ratio is R=1.2Rmin

R=1.2(6.04) =7.25

Step 6: Determination of number of theoretical stages, N

𝑋 =𝑅−𝑅𝑚𝑖𝑛

𝑅+1=

7.25−6.04

7.25+1= 0.1465

𝑌 = 1 − exp [(1+54.4𝑋

11+117.2𝑋) (

𝑋−1

𝑋0.5)]

= 1 − exp [(1+54.4(0.1465)

11+117.2(0.1465)) (

0.1465−1

(0.1465)0.5)] = 0.5084

𝑌 =𝑁−𝑁𝑚𝑖𝑛

𝑁+1

0.5084 =𝑁−7.63

𝑁+1

𝑁 = 16.56 𝑠𝑡𝑎𝑔𝑒𝑠

Step 7: Overall Tray Efficiency

The tray efficiency is determined through the equation shown below:

264

𝐸0 =0.492

[(𝛼𝐿𝐾 𝐻𝐾⁄ )𝑎𝑣𝑒𝜇𝐹]0.245

Where μF = viscosity of feed mixture, by which μF can be estimated by using the equation:

1

𝜇𝐹= ∑

𝑥𝑖

𝜇𝑖

Below is the table of viscosity of each component in the feed at T=85 oC

Component μi (Pa.s) XF Xi/ μi

Methanol 0.000287687 0.0553 192.2229619

Water 0.000191772 0.9423 4913.653017

MTBE 0.000333303 0.0023 6.900631622

Total 5112.776611

𝜇𝐹 = 0.19559𝑚𝑃𝑎. 𝑠

𝐸0 =0.492

(3.98×0.19559)0.245 = 0.5226

Step 8: Actual number of stages

𝑁𝑎𝑐𝑡𝑢𝑎𝑙 =𝑁

𝐸0=

16.56

0.5226= 30.69 𝑠𝑡𝑎𝑔𝑒𝑠

Number of theoretical stages, N= Nactual -1= 30.69-1 = 29.69

≈ 30 stages

Step 9: Determination of location of feed tray

By using Kirkbride equation, the location of the feed point calculated from bottom is determined.

log𝑁𝑟

𝑁𝑠= 0.206 log{

𝐵

𝐷(𝑥𝐻𝐾

𝑥𝐿𝐾)𝐹[

(𝑥𝐿𝐾)𝐵

(𝑥𝐻𝐾)𝐷]2} ………….. (1)

𝑁𝑟 + 𝑁𝑠 = 𝑁𝑎𝑐𝑡 ………(2)

Bottom, B 28743.74 XF,HK 0.9423 XB,LK 0.0006

Distillate, D 24006.47 XF,LK 0.0553 XD,HK 0.0350

Subsitute the values in the table into equation (1). We will get:

𝑁𝑟 = 0.349𝑁𝑠 ……..(3)

𝑁𝑟 + 𝑁𝑠 = 30 ……..(4)

Solve equation (3) & (4) simultaneously, thus we will get:

Ns=23

Nr=7

265

Thus, the feed enter the column at 23rd

stages from the bottom of column

Number of stages/trays in rectifying section = 7

Number of stages in stripping section =23

Number of trays in stripping section =22 (excluding partial reboiler)

3. Column Sizing

The distillation column is sized based on the top condition and the bottom condition. Besides,

the size of distillation column is decided based on the larger diameter calculated from the top

or bottom condition. For column sizing, the important information is the flow rate of each

stream related to distillation column and their respective density.

Step 1: Determination of column height

Tray spacing of 0.3-0.6m are normally employed in industry. Hence, tray spacing, Hs=0.6m is

chosen.

Column height is calculated with tray spacing and the additional space for vapor-liquid

disengagement at column top and for liquid sump at column bottom. An approximation of 15%

allowance for the additional space for phase disengagement and required internal hardware.

Column height, HC = 1.15NHS

HC= 1.15(30)(0.6)

= 20.7 m

Step 2: Determination of physical properties of distillate and bottom product

To determine the diameter of a column, the surface tension (σ) of liquid-vapor interaction is

prerequiste. According to Sugden (1924), a method was developed to estimate the surface tension

of pure component as well as mixture of components, known as contribution to Sudgens’ parachor

for organic compounds as shown in Table 8.7 (pg. 335) in Coulson & Richardson Chemical

Engineering, vol. 6, 4th

edition.

266

For pure component: 𝜎 = [𝑃𝑐ℎ(𝜌𝐿−𝜌𝑉)

𝑀]4 × 10−12

Where σ= Surface tension (mJ/m2)

Pch= Sudgen’s parachor (Refer Table 8.7)

ρL= Liquid density (kg/m3)

ρV= Density of saturated vapour (kg/m3)

M= Molecular weight

For mixture of liquid: 𝜎𝑚 = 𝜎1𝑥1 + 𝜎2𝑥2 + ⋯

Where x1,x2 is the component mole fractions

Pch estimation:

For methanol:

Atom, Group or

Bond

Contribution Value Total Contribution

C 1 4.8 4.8

H-O 1 11.3 11.3

H-C 3 51.3 51.3

O 1 20 20

87.4

For MTBE:

Atom, Group or

Bond

Contribution Value Total Contribution

C 5 4.8 24

H-O 0 11.3 0

H-C 12 17.1 205.2

O 1 20 20

249.2

For water:

Atom, Group or

Bond

Contribution Value Total Contribution

H-O 2 11.3 22.6

O 1 20 20

42.6

267

To determine the density of vapour at particular pressure, the ideal gas behaviour can be assumed

for pure component and non-ideal for mixture to account for the molecular interaction of

individual component.

For pure component: 𝜌𝑉 =𝑃𝑀

𝑅𝑇

For mixture: 𝜌𝑣,𝑚 =𝑃𝑟

′𝑀𝑟,𝑚𝑖𝑥

𝑧𝑅𝑇𝑟′

Where Pr’= Pseudoreduced pressure = P/Pc’

Mr,mix= Molecular weight of mixture

Tr’= Pseudoreduced temperature = T/Tc’

Z= Compressibility factor

P= Pressure of system

Pc’= Preudocritical pressure= yAPcA + yBPcB+….

Tc’= Pseudocritical temperature= yATcA + yBTcB+….

yA, yB= component mole fraction

PcA, PcB= component critical pressure

TcA, TcB= component critical temperature

The physical properties of pure component in distillate and bottom product:

Pure Components Methanol MTBE Water

ρv (kg/m3) Top 1.26 3.46 0.71

Bottom 1.03 2.84 0.58

ρL (kg/m3) Top 780.84 726.40 994.66

Bottom 709.02 650.89 958.35

Pch 87.4 249.2 42.6

σ (J/m2) Top 0.021 0.018 0.031

Bottom 0.014 0.011 0.026

Molecular mass (kg/kmol) 32 88 18

PC (bar) 79.54 35.87 221.19

TC (K) 786.35 497.25 920.40

XD 0.8587 0.0364 0.1049

XB 0.0008 0.000 0.9992

268

For mixture:

Properties Mixture

Top Bottom

Pc’ (bar) 92.809497 221.07668

Pr’ (bar) 0.010774759 0.004523317

Tc’ (K) 789.888605 920.29276

Tr’ (K) 0.387586298 0.405468799

Z 1 1

Mr

(kg/kmol)

30.2335946 18.00630221

ρL (kg/m3) 796.634315 958.0804718

ρv (kg/m3) 1.187805964 0.580404898

L (kmol/hr) 5439.73 7052.05

V (kmol/hr) 7052.05 5455.91

FLV 0.03 0.03

Compressibility factor,z is obtained by interpolation from Figure 3.8 based on the value of Pr’ and

Tr’ in Coulson, Chemical Engineering Design.

For mixture in both liquid and vapour in overhead and bottom product, the methods used to

estimate the physical properties (ρL, ρV and Mr) are stated as below:

Molecular weight, Mr: 1

𝑀𝑟=

𝑥𝐴

𝑀𝐴+

𝑥𝐵

𝑀𝐵+ ⋯

Where xA, xB= component mass fraction

MA,MB= component molecular weight

Liquid density, ρL: 1

𝜌𝐿=

𝑥𝐴

𝜌𝐴+

𝑥𝐵

𝜌𝐵+ ⋯

Where xA, xB= component mass fraction

ρA,ρB= component density

269

Step 3: Determination of K value

From the value of FLV get previously, we can get the value of K1 from Coulson & Richardson

Chemical Engineering, Vol. 6, 4th

edition Figure 11.27 (pg. 568).

Top Bottom

K1 0.13 0.13

Step 4: Determination of vapour flooding velocity, uf

Assuming column diameter is larger than 1m, tray spacing of 0.5m is typically chosen.

𝑢𝑓 = 𝐾1(𝜌𝐿 − 𝜌𝑉

𝜌𝑉)0.5

Top Bottom

Uf

0.13 (798.46 − 1.14

1.14)0.5

=3.44 m/s

0.085 (965.10 − 0.60

0.60)0.5

=5.23 m/s

270

Step 5: Determination of actual vapour velocity, uV

Assume 50% flooding for column operation

𝑢𝑉 = 0.5𝑢𝑓

Top Bottom

UV 0.5(3.44 m/s)= 1.72 m/s 0.5(5.23 m/s)= 2.61 m/s

Step 6: Determination of volumetric flow rate, �̇�

�̇� =𝑣 (

𝑘𝑚𝑜𝑙ℎ𝑟

) × 𝑀𝑟 (𝑘𝑔

𝑘𝑚𝑜𝑙)

𝜌𝑉 (𝑘𝑔𝑚3) ×

3600𝑠ℎ𝑟

Top Bottom

�̇� 7052.05×29.41

1.14×3600

=50.67 m3/s

5455.91×18.00

0.60×3600

=45.76 m3/s

Step 7: Determination of net column area, An

𝐴𝑛 =�̇�

𝑢𝑣

Top Bottom

An 50.67/1.72

=29.44 m2

45.76/2.61

=17.50 m2

Step 8: Determination of cross sectional area, Ac

Assume downcomer occupies 20% of column cross sectional area, 𝐴𝑐 =𝐴𝑛

0.8

Top Bottom

Ac 29.44/0.8

=36.80 m2

17.50/0.8

=21.88 m2

271

Step 9: Determination of cross sectional area of downcomer, Ad

𝐴𝑑 = 𝐴𝑐 − 𝐴𝑛

Top Bottom

Ad 36.80-29.44

=7.36 m2

21.88-17.50

=4.38 m2

Step 10: Determination of column diameter, Dc

𝐷𝑐 = √4𝐴𝑐

𝜋

Top Bottom

Dc √

4𝐴𝑐

𝜋

=√4(36.80)

𝜋

=6.84 m

√4𝐴𝑐

𝜋

=√4(21.88)

𝜋

=5.28 m

Since limiting vapour condition occurs at the top of column, so the column inner diameter is taken

as 6.84m. Since the column diameter is larger than 1m, the tray spacing of 0.6 m is justified.

There are two limitations on the design conditions of distillation column, which are the column

height and height-to-diameter ratio. The general guidelines are column height, Hc < 54m and the

height-to-diameter ratio, Hc/Dc < 30 [James M.Douglas, 1988. “Conceptual Design of Chemical

Processes”, McGraw Hill, pg 457]

Previously, we calculated Hc = 20.7 m which is less than 54m. Thus, it is acceptable. On the other

hands, ratio Hc/Dc = 20.7/ 6.84= 3.03 (<30). Hence, it is acceptable.

4. Plate hydraulic design

Consider the preliminary specification of column T-103 on the basis of top section.

Column diameter, Dc= 6.84 m

Column area, Ac=36.80 m2

Net area, An= 29.44 m2

Downcomer area, Ad= 7.36 m

2

Step 1: Provisional plate design

Active area, 𝐴𝑎 = 𝐴𝑐 − 2𝐴𝑑 = 36.80 − 2(7.36) = 22.08𝑚2

Assume all active holes take 6% of active area.

Hole area, 𝐴ℎ = 0.06𝐴𝑎 = 0.06(22.08) = 1.32 𝑚2

Hole size/diameter:

272

The optimum size of hole that can be punched is twice the plate thickness. Due to handling

of heavy hydrocarbons in the column, large-sized hole will not susceptible to fouling. Thus,

hole size or diameter = 5 mm

Plate thickness = 2mm

Weir height, hw = 0.05m (suggestion from Coulson & Richardson)

Weir length, lw:

From figure 11.31 in Coulson & Richardson Chemical Engineering, Vol.6, 4th

edition,

when Ad/Ac X 100% = 20%; lw/Dc = 0.86

Thus, lw = 5.89m

Hole pitch, lp:

The normal range of hole pitch to diameter ratio is 2.5 to 4. Taking average value of the

range, assume hole pitch is 3.25 times of hole diameter.

𝑙𝑝 = 3.25(5) = 16.25𝑚𝑚 = 0.016𝑚

Area of active hole:

𝐴ℎ = 𝜋(𝐷ℎ

2)2

= 𝜋(0.005

2)2

= 1.964 × 10−5𝑚2

Number of holes per tray: 𝐴ℎ,𝑡𝑜𝑡𝑎𝑙

𝐴ℎ=

1.32

1.964×10−5 = 67460.75 ≈ 67461 ℎ𝑜𝑙𝑒𝑠

Step 3: Check weeping

The height of the liquid crest over the weir, how can be determined by using Francis weir formula:

ℎ𝑜𝑤 = 750[𝐿𝑤

𝑙𝑤 × 𝜌]2 3⁄

273

Maximum liquid rate = 44.44 kg/s

Minimum liquid rate at 70% Turndown Ratio = (0.70)(44.44) = 31.11 kg/s

Maximum how = 750 (44.44

796.63×5.89)

2

3= 33.54 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Minimum how= 750 (31.11

796.63×5.89)

2

3= 26.44 mm liquid

To ensure an even flow of liquid along the wier, the crest should be at least 10mm at the

lowest liquid rate. Thus, we chosen crest at 40mm at the lowest liquid rate.

At minimum liquid flow rate, how+hw= 26.44 + 40 =66.44mm

From Coulson and Richardson’s Chemical Engineering Design, Figure 11.30,

we get K2= 30.5

Minimum design vapour velocity,

𝑢ℎ =[𝐾2−0.90(25.4−𝑑ℎ)]

(𝜌𝑣)0.5

𝑢ℎ =[30.5−0.90(25.4−5)]

(1.187)0.5

= 11.39 𝑚/𝑠

Maximum vapour flowrate = 50.67 m3/s

Minimum vapour rate at 70% turndown ratio: 0.70(𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒)

𝐴ℎ=

0.7(50.67)

1.32= 26.78 𝑚/𝑠

Actual minimum vapour velocity > weeping velocity, so minimum operating rate will be

well below weep point

Step 4: Determination of plate pressure drop

Maximum vapour flowrate, �̇�= 50.67 m3/s

Maximum vapour velocity through holes, 𝑢ℎ =�̇�

𝐴ℎ,𝑡𝑜𝑡𝑎𝑙=

50.67

1.32= 38.25 𝑚/𝑠

Percentage of perforated area, 𝐴ℎ

𝐴𝑝× 100% ≈

𝐴ℎ

𝐴𝑎× 100% = 10%

Plate thickness/ hole diameter =2

5=0.4

From figure 11.34 (pg 576), Coulson & Richardson’s Chemical Engineering, vol.6, 4th

edition, the orifice coefficient Co can be estimated.

274

Thus, C0=0.69

Dry plate drop, hd:

ℎ𝑑 = 51[𝑢ℎ

𝐶𝑜]2

𝜌𝑉

𝜌𝐿

= 51(38.25

0.69)2 0.6

965.10

= 96.85 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Residual head, ℎ𝑟 =12500

𝜌𝐿,𝑇𝑜𝑝=

12500

796.63= 15.66 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Total pressure drop, ℎ𝑇 = ℎ𝑑 + (ℎ𝑤 + ℎ𝑜𝑤) + ℎ𝑟 = 178.94 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Step 5: Downcomer liquid backup

Height of the bottom edge of the apron above the plate, hap:

ℎ𝑎𝑝 = ℎ𝑤 − 10 = 40 − 10 = 30 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Clearance area under downcomer apron, Aap:

𝐴𝑎𝑝 = 𝑙𝑤ℎ𝑎𝑝 = 5.89 × 0.03 = 0.1766 𝑚2

As this is less than Ad, Aap is used

275

ℎ𝑑𝑐 = 166(𝐿𝑤𝑑

𝜌𝐿𝐴𝑚)2

= 166(44.44

965.1×0.1766)2

=11.29 mm

Back-up in downcomer

ℎ𝑏 = ℎ𝑑𝑐 + (ℎ𝑤 + ℎ𝑜𝑤) + ℎ𝑡

= 11.29 + (40 + 26.44) + 178.94

= 256.67 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

To avoid flooding, hb < (0.5)(tray spacing + weir height)

0.5(0.6+0.05)= 0.325 m

hb < 0.325 m. Thus, it can avoid flooding.

Contact/residence time, tr:

𝑡𝑟 =𝐴𝑑ℎ𝑏𝜌𝐿

𝐿𝑤𝑑

=7.36×(256.67×10−3)×798.46

44.44

= 33.94 𝑠

A residence time of at least 3s is recommended. Since tr > 3s, thus it is acceptable.

Step 6: Check Entrainment

𝑢𝑣 =max𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒

𝐴𝑛

=50.67

29.44= 1.72 𝑚/𝑠

Percentage of flooding =𝑢𝑣

𝑉𝑛𝑓,𝑡𝑜𝑝=

1.72

3.44= 0.5 = 50%

Fractional entrainment

From figure 11.29 (pg 570) in Coulson & Richardson’s Chemical Engineering, vol.6, 4th

edition, the fractional entrainment is determined by using flooding percentage and FLV

value.

With FLV = 0.03 and 50% flooding, the fractional entrainment Ψ=0.02

276

The entrainment is below 0.1, thus it is acceptable.

5. Mechanical Design

Step 1: Design Pressure

The operating pressure of the column is 100kPa. However, there is quite a lot of number of plates

and lead to a significant of pressure drop. It is predicted that pressure at bottom of the column will

be higher. Therefore, an extra 10% of pressure will be considered in mechanical design.

Design pressure, Pi = 110kPa

Step 2: Design temperature

Feed temperature, TF =85 oC

Distillate temperature, TD =38 oC

Bottom temperature, TB =90 oC

277

For design temperature, 10 oC is added to the operating temperature.

Design temperature, Ti = 90+10= 100 oC

Step 3: Material of construction and corrosion allowance

Carbon steel is selected as material of construction since we do not have corrosive material to

handle. Besides, it is the most commonly used engineering material. It is cheap and is available in

a wide range of standard forms and sizes. It can be easily worked and welded. It has good tensile

strength and ductility.

From table 13.2 Coulson & Richardson 6th

volume 4th

edition (pg 812), at T =100 oC, the design

stress is 125 N/mm2, which is much higher than the column design pressure. Hence, it is a suitable

material of construction for this distillation column.

Step 4: Welded joint efficiency

The strength of a welded joint will depend on the type of joint and the quality of the welding. A

double welded butt type of welding is used for this distillation column to balance the tradeoff

between higher cost and higher strength of weld joint. The welded joint efficiency, J of this weld

joint is 0.85.

Step 5: Minimum Column Thickness

Internal diameter of column, Di = 6.84m = 6844.54mm

Wall thickness is calculated based on Coulson & Richardson’s Chemical Engineering Design.

278

Minimum wall thickness, 𝑡 =𝑃𝑖𝐷𝑖

2𝐽𝑓−𝑃𝑖=

0.11×6844.54

2(0.85)(125)−0.11= 3.54𝑚𝑚

Take corrosion allowance of 2mm.

Thus, fabrication thickness of tube wall = 3.54 + 2 =5.54mm ≈ 6mm

The maximum allowable working pressure (MAWP) for this wall thickness is given by:

𝑀𝐴𝑊𝑃 =2 × 𝑡𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ × 𝑤𝑒𝑙𝑑 𝑗𝑜𝑖𝑛𝑡 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 × 𝑡

𝐷𝑖 + 𝑡

=2 × 360 × 0.85 × 6

6844.54 + 6= 0.536 𝑁/𝑚𝑚2

Since MAWP is greater than the operating pressure, thus the thickness of column is

acceptable.

Step 6: Column head design

The type of head chosen is torispherical head. It is often used as the end closure of cylindrical

vessels. The shape is close to that of an ellipse but is easier and cheaper to fabricate. For

torispherical head, the head thickness is designed as below:

Crown radius, Rc=Di=6.84m

Knuckle radius, Rk=0.06 Rc=0.411m

𝐶𝑠 =1

4(3 + √

𝑅𝑐

𝑅𝑘)

=1

4(3 + √

6.84

0.411)

= 1.77

𝑡 =𝑃𝑖𝑅𝑐𝐶𝑠

2𝑓𝐽+𝑃𝑖(𝐶𝑠−0.2)

=0.11×6844.54×1.77

2(0.85)(125)+0.11(1.77−0.2)

= 6.268 mm

Take corrosion allowance of 2mm.

Fabrication thickness of vessel head = 6.268+2 = 8.268mm ≈9mm

The maximum allowable working pressure (MAWP) for this wall thickness is given by

𝑀𝐴𝑊𝑃 =2 × 𝑡𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ × 𝑤𝑒𝑙𝑑 𝑗𝑜𝑖𝑛𝑡 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 × 𝑡

𝐷𝑖 + 𝑡

=2 × 360 × 0.85 × 9

6844.54 + 9= 0.8037 𝑁/𝑚𝑚2

Since MAWP is greater than the operating pressure, thus the thickness of head is

acceptable.

Step 7: L/D ratio of reactor

Column outer diameter = column inner diameter + 2 x column thickness

279

Do = Di + 2 x t = 6844.54 + 2 x 6 = 6856.54 mm = 6.86m

𝐿

𝐷𝑟𝑎𝑡𝑖𝑜 =

𝐻

𝐷𝑜=

20.72

6.86= 3.02

Since the L/D ratio < 30 , the column size is acceptable.

Step 8: Insulation Design

Rock wool is chosen as the insulation material as it can be used up to the temperature of 659 oC.

Rock wool has the density of 130 kg/m3 and the insulation thickness of 75 mm.

Step 9: Weight of vessel

The total weight of vessel consists of the column weight, tray weight and weight of insulation.

Each weight is calculated separately and summed up to get the total weight of vessel which is

required for stress analysis of the column. The weight of column is calculated based on formula in

Coulson & Richardson’s Chemical Engineering Design.

d. Weight of column

Take Cv = 1.15 as a factor to account for the weight of nozzle, manway, internal support

Mean diameter, Dm = Di + t = 6844.54+6=6850.54 mm =6.85m

Weight of column, Wt = 240CvDm(Hv+0.8Dm)t

= 240(1.15)(6.85)(20.72+0.8x6.85)(6)

= 297003.83N=297.00kN

e. Weight of trays

Weight of single tray = (An-Ah) x Plate thickness x Carbon steel density x g

= (29.44-1.32) x (0.002) x (7787.40) x (9.81)

= 4295.56N = 4.29kN

Weight of trays = Weight of single tray x Number of trays

= 4.29 x 30= 128.87 kN

f. Weight of insulation

Vessel diameter, Dt = Column outer diameter + 2 x Insulation thickness

= 6.844 + 2 x 0.075

= 6.995m

Volume of insulation =𝜋(𝐷𝑡

2−𝐷𝑜2)

4𝐻 =

𝜋(6.9952−6.8442)

4(20.72) = 33.75𝑚3

Weight of insulation = 2 x volume of insulation x insulation material density x g

= 2 x 33.75 x 130 x 9.81

= 86090.94N = 86.09 kN

Total weight of distillation column, W = 297.00+128.87+86.09 =511.96 kN

Step 10: Stress analysis

Stress analysis must be made to ensure that the reactor structure is strong and safe. Stress

analysis is solely based on Coulson and Richardson’s Chemical Engineering Design.

b. Wind loading

Typically, wind pressure = 1280 N/m2 for preliminary design

Effective column diameter = Vessel diameter = 6.995m

Wind loading per unit length of column, Fw = 1280(6.995) = 8953.01 N/m

Bending moment at bottom tangent line, Mx =𝐹𝑤𝐻2

2

=8953.01(20.7)2

2= 1918137.63𝑁𝑚

280

Longitudinal stress, 𝜎ℎ =𝑃𝐷𝑖

2𝑡=

0.11(6844.54)

2(6)= 62.74𝑁/𝑚𝑚2

Circumferential stress, 𝜎𝐿 =𝑃𝐷𝑖

4𝑡=

0.11(6844.54)

4(6)= 31.37𝑁/𝑚𝑚2

Dead weight stress, 𝜎𝑊 =𝑊

𝜋(𝐷𝑖+𝑡)𝑡=

511.96 × 1000

𝜋(6844.54+6)6= 3.96

𝑁

𝑚𝑚2

Second moment area of the vessel about the plane of bending, 𝐼𝑣 =𝜋

64(𝐷𝑜

4 − 𝐷𝑖4)

𝐼𝑣 =𝜋

64(6856.544 − 6844.544) = 7.576 × 1011𝑚𝑚4

Bending stress, 𝜎𝑏 = ±𝑀𝑥

𝐼𝑣(𝐷𝑖

2+ 𝑡) = ±

1918137.63(1000)

7.576×1011 (6844.54

2+ 6) = ±8.68𝑁/𝑚𝑚2

Total longitudinal stress, 𝜎𝑧 = 𝜎𝐿 + 𝜎𝑤 ± 𝜎𝑏

Since the vessel is above the support, so stress is applied from top of support, thus,

comprehensive (negative value)

𝜎𝑧(𝑢𝑝𝑤𝑖𝑛𝑑) = 62.74 − 31.37 + 8.68 = 36.09𝑁/𝑚𝑚2

𝜎𝑧(𝑑𝑜𝑤𝑛𝑤𝑖𝑛𝑑) = 62.74 − 31.37 − 8.68 = 18.73𝑁/𝑚𝑚2

Torsional shear stress needs not be considered in preliminary design.

Under this condition, the 3 principal stresses and their difference are calculated as shown:

Principle stress (N/mm2) Upwind Downwind

𝜎1 = 𝜎ℎ 62.74 62.74

𝜎2 = 𝜎𝑧 36.09 18.73

𝜎3 = 0.5𝑃 0.055 0.055

𝜎1 − 𝜎2 26.66 44.01

𝜎1 − 𝜎3 62.69 62.69

𝜎2 − 𝜎3 36.03 18.67

The greatest difference between the principal stresses will be on the down-wind side which

is 62.29 N/mm2. It is well below the maximum allowable design stress. Hence, the design

is acceptable.

Critical buckling stress, 𝜎𝑐 = 2 × 104 (𝑡

𝐷𝑜) = 2 × 104 (

6

6844.54) = 17.53 𝑁/𝑚𝑚2

Maximum compressive where the vessel is not under pressure

= 𝜎𝑤 + 𝜎𝑏 = 3.96 + 8.68 = 12.64 𝑁/𝑚𝑚2

The maximum compressive when vessel is not under pressure is below the critical

buckling stress. Thus, the design is satisfactory.

Step 11: Vessel support

Type of support chosen: Conical skirt (used for tall, vertical column)

Take skirt bottom diameter, Ds = 7m

Take skirt height, Hs = 4m

Skirt base angle, 𝜃𝑠 = tan−1 𝐻𝑠1

2(𝐷𝑠−𝐷𝑖)

= tan−1 41

2(7−6.884)

= 88.89𝑜

This angle is between 80o and 90

0, hence the skirt base angle is satisfactory.

The maximum dead weight load on the skirt will occur when the vessel is full of water.

Approximate water weight, 𝑊𝑤 = (𝜋

4× 𝐷𝑖

2 × 𝐻) × 1000 × 9.81

281

= (𝜋

4× 6.8442 × 20.72) × 1000 × 9.81

= 7472643.053𝑁 = 7472.64𝑘𝑁

Take skirt thickness, ts be 14mm,

Bending moment at bottom of skirt, 𝑀𝑠 =𝐹𝑤(𝐻+𝐻𝑠)

2

2

=8953.01(20.72 + 4)2

2

= 2731071.81 𝑁𝑚

Bending stress in skirt, 𝜎𝑏𝑠 =4𝑀𝑠

𝜋(𝐷𝑠+𝑡𝑠)𝐷𝑠𝑡𝑠=

4(2731071.81)(103)

𝜋(7000+14)7000×14= 5.06 𝑁/𝑚𝑚2

Dead weight stress in the skirt, 𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) =𝑊𝑤

𝜋(𝐷𝑠+𝑡𝑠)𝑡𝑠=

7472643.053

𝜋(7000+14)14= 24.22 𝑁/𝑚𝑚2

𝜎𝑤𝑠(𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔) =𝑊

𝜋(𝐷𝑠 + 𝑡𝑠)𝑡𝑠=

511.96 × 103

𝜋(7000 + 14)14= 1.66 𝑁/𝑚𝑚2

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) = 5.06 + 24.22 = 29.28 𝑁/𝑚𝑚2

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) = 5.06 − 1.66 = 3.40 𝑁/𝑚𝑚2

The skirt thickness should be such that under the worst combination of wind and dead-

weight loading, 2 design criteria must be satisfied. Choosing the skirt material to be carbon

steel, maximum allowable design stress at 20 oC is 135 N/mm

2. The young modulus of

stainless steel type 304 is 210000 MPa.

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑓𝑠𝐽 sin 𝜃

3.40 < (0.85)(135) sin 88.89𝑜

3.40 < 91.45

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸(𝑡𝑠

𝐷𝑠) sin 𝜃

29.28 < 0.125(210000)(14

7000) sin 88.89𝑜

29.28 < 31.38

Since both design criteria are satisfied, the skirt thickness is acceptable.

Take corrosion allowance of 2mm, skirt thickness =14+2=16mm

Step 12: Base ring and anchor bolt design

Take pitch circle diameter, Db =5.2m

Circumference of bolt circle = 5.2 X 103(π)= 16336.28 mm

Minimum bolt spacing is recommended at 600mm

No of bolts required =16336.28

600= 27.23 ≈ 28 𝑏𝑜𝑙𝑡𝑠 (𝑚𝑢𝑠𝑡 𝑏𝑒 𝑚𝑢𝑙𝑡𝑖𝑝𝑙𝑒 𝑜𝑓 4)

Bolt stress, fb = 125 N/mm2 (from Coulson & Richardson’s Chemical Engineering Design)

Area of bolt, 𝐴𝑏 =1

𝑁𝑏𝑓𝑏[4𝑀𝑠

𝐷𝑏− 𝑊] =

1

28(125)[4(2731071.805)

5.2− 511.96 × 103]

= 453.96 mm2

Diameter of bolt= √𝐴𝑏×4

𝜋= √

453.96×4

𝜋= 24.04𝑚𝑚

Referring to Figure 13.2 Coulson & Richardson 6th

volume 4th

edition, the bolt size of

M24 (root area 353) is used.

Total compressive load on base ring, Fb

282

=4𝑀𝑠

𝜋𝐷𝑠2+

𝑊

𝜋𝐷𝑠=

4(2731071.805)

𝜋(7)2+

511.96 × 103

𝜋(7)= 94233.61 𝑁/𝑚2

From Coulson and Richardson’s Chemical Engineering Design, maximum allowable

bearing pressure on concrete foundation pad, fc = 7 N/mm2

Minimum base ring width, 𝐿𝑏 =𝐹𝑏

𝑓𝑐×

1

1000=

94233.61

1

1000= 13.46𝑚𝑚

From figure 13.30 Coulson & Richardson Chemical Engineering, vol.6, 4th

edition, for

M24 bolts, Lr =150mm.

Actual base ring width = Lr + ts +50=150+14+50= 214mm

Actual bearing pressure on concrete foundation pad, f’c =94233.61

214×1000= 0.44 𝑁/𝑚𝑚2

Allowable design stress in ring material, fr=140 N/mm2 (From Coulson and Richardson’s

Chemical Engineering Design)

Minimum base ring thickness, tb = 𝐿𝑟√3𝑓𝑐

𝑓𝑟= 150√

3(0.44)

140= 14.57 𝑚𝑚

Step 13: Nozzles Design

The Harker equation (1978), modified for SI unit, for the optimum pipe and nozzle

diameter:

For feed opening, 𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where W is mass flow rate in kg/hr and ρ is density of fluid in kg/m3

f. For feed inlet

𝐷𝑜𝑝𝑡 = 8.4130533.0950.45

950.190.31= 104.67 𝑚𝑚 = 4.12 𝑖𝑛 ≈ 6.0 𝑖𝑛

g. For top outlet

𝐷𝑜𝑝𝑡 = 8.4124006.470.45

1.1370.31= 756.256 𝑚𝑚 = 29.77 𝑖𝑛 ≈ 30.0 𝑖𝑛

h. For bottom outlet

𝐷𝑜𝑝𝑡 = 8.4128743.7370.45

965.0960.31= 101.37 𝑚𝑚 = 3.99 𝑖𝑛 ≈ 4.0 𝑖𝑛

i. For reflux inlet

𝐷𝑜𝑝𝑡 = 8.4120576.9740.45

803.1150.31= 92.33 𝑚𝑚 = 3.63 𝑖𝑛 ≈ 4.0 𝑖𝑛

j. For reboiler inlet

𝐷𝑜𝑝𝑡 = 8.411640.1380.45

0.6960.31= 263.149 𝑚𝑚 = 10.36 𝑖𝑛 ≈ 12.0 𝑖𝑛

Summary of nozzle design:

Stream W (kg/hr) Ρ (kg/m3) Dopt (in)

Feed Inlet 30533.095 950.19 6.0

Top Outlet 24006.47 1.137 30.0

Bottom Outlet 28743.737 965.096 4.0

Reflux Inlet 20576.974 803.115 4.0

Reboiler Inlet 1640.138 0.696 12.0

283

Heat Transfer Equipment Design E-101-Feed Heater

The feed heater E-101 is used to heat up the mixture of methanol, water, dimethyl ether, hydrogen,

nitrogen, carbon dioxide and carbon monoxide from storage tank and also recycle stream at 11.00

bar from T=90OC to T= 100

OC, before this stream enters the synthesis reactor (R-101). The steam

used to heat up the mixture enters at T=250OC and leaves at T=150

OC at 11.10 bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

284

Design Procedure

Step 1: Specification

Specification Tube (Process Fluid) Shell (Mixture)

Heat Duty, Q (kW) 445.53

Inlet Temperature (OC) Tc1 28 Th1 = 150

Outlet Temperature

(OC) Tc2 75 Th2 = 120

Pressure (bar) 3.98 1.78

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 43011.388 𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 11.95

𝑘𝑔

𝑠

Mass flow rate for shell side = 19.19𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠×

1000𝑘𝑔

1 𝑡𝑜𝑛 = 5.33

𝑘𝑔

𝑠

Step 2: Physical Properties

Mean Temperature of steam at tube side:

= 28+75

2 = 103°𝐶

Mean temperature of process fluid at shell side:

= 150+120

2 = 135°𝐶

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Physical Properties Tube Shell

Mean Temperature of mixture gas

(OC)

51.50 135.00

Total molecular 46.92 30.94

Density (kg/m3) 635.49 850.43

Viscosity (Pa.s) 0.00002 0.00001

K (W/m. K) 0.1375 0.6565

Cp (kJ/kg.K) 2.6470 4.3071

285

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with process mixture as the cold fluid and steam as

hot fluid, the overall coefficient will be in the range of 500-1000 W/m2o

C. To start with, the

overall coefficient (U) is taken to be 950 W/m2o

C.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(150 − 75) − (120 − 28)

ln ((400 − 75)120 − 28 )

= 83.21℃

𝑅 =𝑇𝐻1−𝑇𝐻2

𝑇𝐶1−𝑇𝐶2=

150−120

75−28= 0.3261

𝑆 =𝑇𝐶1−𝑇𝐶2

𝑇𝐻1−𝑇𝐶2=

75−28

150−120= 0.3849

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft= 0.9849

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 81.95 ℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

445.53

950 × 81.95= 5.72𝑚2

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

Step 6: Layout and Tube Size

286

In order to obtain higher efficiency and ease the cleaning process, a split-ring floating-

head exchanger is used.

The material of construction for heat exchangers is stainless steel 316. Allocating the fluid

with the highest flow rate to the tube side will normally give the most economical design.

Besides, in reference 1, it is said that the fluid with the lowest allowable pressure drop

should be allocated to the tube side.

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 19.05 mm = 0.019m

Internal diameter, DI = 15.8 mm = 0.0158m

Length of tube, LT = 1.83 long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0238𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.019 𝑚 × 1.83 𝑚 = 0.11 𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 5.72 𝑚2

0.11 𝑚2= 𝟓𝟐 = 𝟐𝟔

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes is selected. So, for 2 passes,

tubes per pass = 1505 tubes

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.0158)2

4= 1.96 × 10−4𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 26 × 1.96 × 10−4𝑚2 = 0.0051 𝑚2

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 11.95 𝑘𝑔/𝑠

635.50 𝑘𝑔/𝑚3= 0.019 𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.019 𝑚3/𝑠

0.0051 𝑚2= 3.67 𝑚/𝑠

287

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 2 tube passes,

K1 = 0.249 n1 =2.207

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.01905 (52

0.249)

12.207⁄

= 0.21 𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 2.27 m,

the shell clearance is 80mm = 0.08m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 0.21 𝑚 + 0.05 𝑚 = 𝟎. 𝟐𝟔 𝒎

TEMA standard Ds is max 1.520 m. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

11.95𝑘𝑔𝑠

0.0051𝑚2= 𝟐𝟑𝟑𝟐. 𝟒𝟑 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

𝟐𝟑𝟑𝟐. 𝟒𝟐𝑘𝑔𝑚2𝑠

× 0.0158𝑚

0.002 𝑘𝑔𝑚. 𝑠

= 163847.77

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

2.65𝑘𝐽

𝑘𝑔.𝐾×1000×0.002

𝑘𝑔

𝑚.𝑠

0.1375𝑊

𝑚.𝐾

= 4.33

𝐿

𝑑𝑜=

1.83 𝑚

0.01905 𝑚𝑚= 𝟗𝟔. 𝟎𝟔

288

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0021

𝑁𝑢 =ℎ𝑖𝑑𝑖

𝑘𝑓= 𝑗ℎ𝑅𝑒𝑃𝑟0.33 (

𝜇

𝜇𝑤)0.14

Neglect (𝜇

𝜇𝑤)

ℎ𝑖 = 4855.83𝑊

𝑚2𝐾

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n= 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

0.2647

5= 0.05295 𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.0028 𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.019(0.02382 − 0.917 × 0.0192) = 0.0135𝒎

𝑠ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

5.33𝑘𝑔𝑠

0.0028𝑚2= 1901.09 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

1901.09𝑘𝑔𝑚2𝑠

× 0.0135 𝑚

0.0001𝑘𝑔𝑚. 𝑠

= 200977.18

289

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

4.3071𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0001

𝑘𝑔𝑚. 𝑠

0.6565𝑊

𝑚.𝐾

= 0.8395

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0027

𝑁𝑢 =ℎ𝑂𝑑𝑒

𝑘𝑓= 𝑗ℎ𝑅𝑒𝑃𝑟0.33

ℎ𝑂 = 24844.01𝑊

𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod = outside dirt coefficient (fouling factor)

hid = inside dirt coefficient (fouling factor)

kw = thermal conductivity of the tube wall material

di = tube inside diameter

do = tube outside diameter

290

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/moC.

1

𝑈𝑜=

1

286.11+

1

5000+

0.019𝑙𝑛 (0.0190.0158

)

2(18.8)+

0.019

0.0158×

1

5000+

0.019

0.0158×

1

593.55

𝑈𝑜 = 𝟏𝟐𝟏𝟐. 𝟗𝟏 𝑾/𝒎𝟐. °𝑪

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

1212.91 − 950

1212.91× 100% = 27.68 %

Hence, Uo assume is between 0% – 30%. So, Uo= 1212.91 W/m2K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.0046

For isothermal flow,

∆𝑃 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= 57889.00 𝑁/𝑚2 = 0.58 bar

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.004

∆𝑃 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2= 45996.74 𝑃𝑎 = 0.45 𝑏𝑎𝑟

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

291

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟒. 𝟕𝟓 𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

445.53 𝑘𝐽𝑠

4.75 𝑚2= 𝟗𝟑𝟖𝟔𝟖. 𝟕𝟐 𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 51.5℃ −

𝟗𝟑𝟖𝟔𝟖. 𝟕𝟐 𝑊𝑚2

4855.83 𝑊𝑚2 °𝐶

= 70.83℃

𝑊ℎ𝑒𝑛 𝑡 = 70.83℃, 𝜇 = 0.0001998 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.0002

0.0001998)0.14

= 𝟏. 𝟎𝟎

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 13: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

Tube Pitch = 0.0238m, tube diameter = 0.0158mm

0.0238 − 0.0158

0.0158× 100% = 50.71%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where

Dopt = optimum diameter (mm), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

292

Tube

𝐷𝑜𝑝𝑡 = 8.41(11.95)0.45

(635.50)0.31 = 0.08(𝑖𝑛𝑙𝑒𝑡)

Therefore, a 3.47 m diameter nozzle was specified for the tube-side inlet

Shell

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(5.33)0.45

(850.43)0.31 = 0.05 𝑚 (𝑖𝑛𝑙𝑒𝑡)

A nozzle size of 3.47 m diameter is selected for the inlet and outlet at the shell side of the

exchanger.

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

K fiber glass= 0.04 W/m. K

r = 𝐾

ℎ𝑜=

0.04

248446.1 =0.000016𝑚 = 1.69x10

-9 mm

Summary

Split ring, floating head, 1 shell pass, and 2 tube passes.

Stainless Steel tubes, 1.83 m long, 0.019 mm o.d., 0.0158 mm i.d., triangular pitch 0.0238m.

Heat transfer area 5.72 m2 (based on outside diameter).

Shell i.d. 0.26 m, baffle spacing 0.05295 m, 25% cut.

Tube-side coefficient 4855.83 W/m2. K., clean.

Shell-side coefficient 24844.01 W/ m2.K., clean.

Overall coefficient, estimated 950 W/m2. K.

Overall coefficient, calculated 1212.91 W/m2.K.

Dirt/fouling factors:

293

Tube side (mixture gas) 5000 (W/m2.K)

-1.

Shell side (mixture gas) 5000 (W/m2.K)

-1.

Pressure drops:

Tube side, estimated 0.58 bar; allowable 0.8 bar.

Shell side, estimated 0.46 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.08m and 0.05m, respectively.

E-102- Condenser

The Condenser E-102 is used to condense the mixture of methanol, water, dimethyl ether,

hydrogen, nitrogen, carbon dioxide and carbon monoxide from synthesis reactor (R-101) at 7.50

bar from T=67OC to T= 62

OC, before this stream enters the distillation column (T-101). The brine

solution used to cool down the mixture enters at T=5OC and leaves at T=15

OC at 7.50 bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

294

Design Procedure

Step 1: Specification

Specification Tube (chilled Water) Shell (Process Fluid)

Heat Duty, Q (kW) 10562.63

Inlet Temperature (OC) TC2 = 5 TH1 = 67

Outlet Temperature

(OC) TC1 = 15 TH2 = 62

Pressure (bar) 7.50 7.50

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 28280.66 𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 7.86

𝑘𝑔

𝑠

Mass flow rate for shell side = 454.85 𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠×

1000𝑘𝑔

1 𝑡𝑜𝑛 = 126.35

𝑘𝑔

𝑠

Step 2: Physical Properties

Mean Temperature of brine solution at tube side:

= 5+15

2 = 10°𝐶

Mean temperature of process fluid at shell side:

= 67+62

2 = 64.5°𝐶

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Physical Properties Tube Shell

Mean Temperature (OC) 10 64.5

Total molecular 18.72 44.67

Density (kg/m3) 1198.8 664.78

Viscosity (Pa.s) 0.0013 0.0002

K (W/m.K) 0.6235 0.1497

Cp kJ/kg.K 4.1787 2.7123

295

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with organic solvent as the hot fluid and water as cold

fluid, the overall coefficient will be in the range of 250-750 W/m2o

C. To start with, the overall

coefficient (U) is taken to be 390 W/m2o

C.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(67 − 15) − (62 − 5)

ln (67 − 1562 − 5

)= 54.46℃

𝑅 =𝑇𝐻1 − 𝑇𝐻2

𝑇𝐶1 − 𝑇𝐶2=

67 − 15

15 − 5= 5.20

𝑆 =𝑇𝐶1 − 𝑇𝐶2

𝑇𝐻1 − 𝑇𝐶2=

15 − 5

67 − 5= 0.1613

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft = 0.8177

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 44.53℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

10562.6278

500×44.5323= 474.38𝑚24

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

Step 6: Layout and Tube Size

In order to obtain higher efficiency and ease the cleaning process, a split-ring floating-

head exchanger is used.

The material of construction for heat exchangers is stainless steel 316. A higher flow rate

stream should be allocated to the tube side as it will normally give the most economical

design. Besides, in reference 1, it is said that the fluid with the lowest allowable pressure

drop should be allocated to the tube side.

296

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 19.05 mm = 0.019m

Internal diameter, DI = 15.8 mm = 0.0158m

Length of tube, LT = 5 m long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0238𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.019 𝑚 × 7.32 𝑚 = 0.30𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 474.38𝑚2

0.30𝑚2= 𝟏𝟖𝟖𝟏. 𝟕 = 𝟏𝟓𝟖𝟓

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes or multiple of four is

selected. So, for 4 passes, tubes per pass = 396

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.015)2

4= 1.961 × 10−4𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 396 × 1.961 × 10−4𝑚2 = 0.077 𝑚2

At mean temperature, the density of tube side is 1198.80 kg/m3

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 126.35 𝑘𝑔/𝑠

1198.80 𝑘𝑔/𝑚3= 0.1054𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.1054𝑚3/𝑠

0.0777 𝑚2= 0.437 𝑚/𝑠

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 2 tube passes,

K1 = 0.249 n1 =2.207

297

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.019 (1585

0.175)

12.207⁄

= 1.03 𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 1.03 m,

the shell clearance is 73 mm = 0.073 m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 1.03 + 0.073𝑚 = 𝟏. 𝟏𝟎𝟑 𝒎

TEMA standard Ds is max 1.52 m. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

126.35𝑘𝑔𝑠

0.07771𝑚2= 𝟏𝟔𝟐𝟓. 𝟗𝟔 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

1625.96𝑘𝑔

𝑚2𝑠×0.0158𝑚

0.0013𝑘𝑔

𝑚.𝑠

= 19506.57

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

4.179𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0013

𝑘𝑔𝑚. 𝑠

0.6235𝑊

𝑚.𝐾

= 8.826

𝐿

𝑑𝑖=

5 𝑚

0.0158 𝑚𝑚= 𝟑𝟏𝟔. 𝟒𝟔

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0038

298

ℎ𝑖 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33(

𝜇

𝜇𝑤)0.14

𝑑𝑖= 6001.69 𝑊/𝑚2𝐾 Neglect (

𝜇

𝜇𝑤)

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n = 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

1.1002

5= 0.22 𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.048 𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.019(0.02382 − 0.917 × 0.0192) = 0.0135𝒎

ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

7.8557𝑘𝑔𝑠

0.04842𝑚2= 162.25𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

162.25𝑘𝑔𝑚2𝑠

× 0.0135𝑚

2 × 10−5 𝑘𝑔𝑚. 𝑠

= 9219.63

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

2.7123𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 2 × 10−5 𝑘𝑔

𝑚. 𝑠

0.1497𝑊

𝑚.𝐾

= 4.3116

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.006

299

ℎ𝑂 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33

𝑑𝑒= 361.56𝑊/𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod= outside dirt coefficient (fouling factor) =5000 W/mK

hid = inside dirt coefficient (fouling factor) = 5000 W/mK

kw = thermal conductivity of the tube wall material

di = tube inside diameter

do = tube outside diameter

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/mK.

1

𝑈𝑜=

1

361.56+

1

5000+

0.019𝑙𝑛 (0.0190.0158

)

2(18.8)+

0.019

0.0158×

1

5000+

0.019

0.0158×

1

3997

𝑈𝑜 = 𝟓𝟕𝟒. 𝟔𝟖 𝑾/𝒎𝟐. 𝑲

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

𝟓𝟕𝟒. 𝟔𝟖 − 500

500× 100% = 14.94%

Hence, Uo assume is between 0% – 30%. So, Uo= 574.68W/m2 K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.004

For isothermal flow,

∆𝑃 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= ∆𝑃 = 55691.40

𝑁

𝑚2= 0.55𝑏𝑎𝑟

300

* 2.5 is the recommended value for the velocity heads per pass. Neglecting the viscosity

correction term

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.005

∆𝑃 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2=

1463.77

𝑚2= 0.01464 𝑏𝑎𝑟

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟑𝟗𝟑. 𝟒𝟓𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

10562.63 𝐾𝑊 × 1000

393.45 𝑚2= 𝟐𝟔𝟖𝟒𝟔. 𝟐𝟎 𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 15℃ +

10526.63𝑊𝑚2

6001.69𝑊𝑚2 °𝐶

= 14.47℃

𝑊ℎ𝑒𝑛 𝑡 = 14.47℃, 𝜇 = 0.0013 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.0013

0.00131)0.14

= 𝟎. 𝟗𝟗𝟖𝟗

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 14: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

301

Tube Pitch = 0.0238m, tube diameter = 0.0158m

0.0238 − 0.0158

0.0158× 100% = 50.71%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where

Dopt = optimum diameter (m), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

Tube

𝐷𝑜𝑝𝑡 = 8.41(126.3472)0.45

(1198.80)0.31 = 0.328𝑚

`

Therefore, an 0.328 m diameter nozzle was specified for the tube-side inlet

Shell

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(5.44)0.45

(2.4)0.31 = 0.113𝑚

A nozzle size of 0.113 m diameter is selected for the inlet and outlet at the shell side of the

exchanger.

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

302

K fiber glass= 0.04 W/m.K

r = 𝐾

ℎ𝑜=

0.04

3997 =1 × 10−5𝑚=0.01 mm

Summary

Split ring, floating head, one shell pass, and two tube passes.

Stainless Steel tubes, 5 m long, 19.05 mm o.d., 15.8 mm i.d., triangular pitch = 23.8 mm.

Heat transfer area 474.38 m2 (based on outside diameter).

Shell i.d. 1.1m, baffle spacing 0.22 m, baffle diameter 0.072 m 25% cut.

Tube-side coefficient 6001.68 W/m2. K, clean.

Shell-side coefficient 996.73 W/ m2. K, clean.

Overall coefficient, estimated 500 W/m2. K.

Overall coefficient, calculated 574.68 W/m2. K.

Dirt/fouling factors:

Tube side (chilled water) 5000 (W/m2. K)

-1.

Shell side (process fluid) 5000 (W/m2. K)

-1.

Pressure drops:

Tube side, estimated 0.56 bar; allowable 0.8 bar.

Shell side, estimated 0.015 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.328 m and 0.113 m, respectively.

303

E-103 – Reboiler

The reboiler E-103 is used to vaporise the mixture of methanol and water at 7.50 bar from T =

120OC to T = 130

OC. The steam used to vaporise the mixture enters at T=350

OC and leaves at

T=150OC at 7.50 bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

304

Design Procedure

Step 1: Specification

Specification Tube Shell

Heat Duty (kW) 11427.8083

Inlet Temperature (OC) Tc2 = 120 Th1 = 350

Outlet Temperature

(OC) Tc1 = 130 Th2 = 150

Pressure (bar) 7.50 7.50

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 74747.239 𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 𝟐𝟎. 𝟕𝟔

𝒌𝒈

𝒔

Mass flow rate for shell side = 18.22 𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 𝟓. 𝟎𝟔

𝒌𝒈

𝒔

Step 2: Physical Properties

Mean Temperature of process fluid at tube side:

= 99.93+40

2= 70℃

Mean temperature of chilled water at shell side:

= 5+25

2= 15℃

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Physical Properties Tube Shell

Mean Temperature (OC) 125 250

Total molecular 87.76 18.02

Density (kg/m3) 617.25 856.86

Viscosity (Pa.s) 0.00013991 0.00013251

305

K (W/m.K) 0.08698 0.66185

Cp kJ/kg.K 2.6404 4.8632

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with aqueous vapour as the hot fluid and chilled water

as cold fluid, the overall coefficient will be in the range of 600-900 W/m2. K. To start with, the

overall coefficient (U) is taken to be 750 W/m2. K.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(350 − 130) − (150 − 120)

ln (350 − 130150 − 120

)= 95.36℃

𝑅 =𝑇𝐻1 − 𝑇𝐻2

𝑇𝐶1 − 𝑇𝐶2=

350 − 130

130 − 120= 22

𝑆 =𝑇𝐶1 − 𝑇𝐶2

𝑇𝐻1 − 𝑇𝐶2=

130 − 120

350 − 120= 0.21

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft= 0.7463

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 80.70℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

114727.80

750 × 80.70= 188.79𝑚2

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

306

Step 6: Layout and Tube Size

The material of construction for heat exchangers is stainless steel 316. A higher

temperature rate stream should be allocated to the tube side as it will normally reduce the

overall cost. Besides, in reference 1, it is said that the fluid with the lowest allowable

pressure drop should be allocated to the tube side.

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 19.05 mm = 0.019m

Internal diameter, DI = 15.8 mm = 0.0148m

Length of tube, LT = 2.44m (8 ft) long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0238𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.019 𝑚 × 2.44 𝑚 = 0.146𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 188.7947 𝑚2

0.146𝑚2= 𝟏𝟐𝟗𝟑

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes or multiple of four is

selected. So, for 8 passes, tubes per pass = 162 tubes

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.015)2

4= 0.0001727𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 162 × 0.0001727 𝑚2 = 0.02791𝑚2

307

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 =

20.76𝑘𝑔𝑠

617.25𝑘𝑔𝑚3

= 0.03364 𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.03364𝑚3/𝑠

0.02791𝑚2= 1.21 𝑚/𝑠

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 8 tube passes,

K1 = 0.0365 n1 =2.675

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.019 (162

0.0365)

12.607⁄

= 0.96𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 0.95 m,

the shell clearance is 71mm = 0.071 m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 0.95𝑚 + 0.071 = 𝟏. 𝟎𝟐𝟏𝒎

TEMA standard Ds is max 1.52 m. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

20.76𝑘𝑔𝑠

0.0001728𝑚2= 𝟕𝟒𝟑. 𝟖𝟎 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

𝟕𝟒𝟑.𝟖𝟎𝑘𝑔

𝑚2𝑠×0.0148𝑚

0.00013991𝑘𝑔

𝑚.𝑠

=78841.48

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

2.6404𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0001399

𝑘𝑔𝑚. 𝑠

0.08698𝑊

𝑚.𝐾

= 4.2470

308

𝐿

𝑑𝑜=

5 𝑚

0.019 𝑚𝑚= 𝟏𝟐𝟖. 𝟎𝟖

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0029

ℎ𝑖 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33(

𝜇

𝜇𝑤)0.14

𝑑𝑖= 2161.27 𝑊/𝑚2𝐾 Neglect (

𝜇

𝜇𝑤)

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n= 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

1.02

5= 0.029𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.006029𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.019(0.02382 − 0.917 × 0.0192) = 0.0135𝒎

𝑠ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

5.06𝑘𝑔𝑠

0.006 𝑚2= 839.39𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

839.39𝑘𝑔𝑚2𝑠

× 0.0135𝑚

0.0013𝑘𝑔𝑚. 𝑠

= 85684.01

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

4.863𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0013

𝑘𝑔𝑚. 𝑠

0.66185𝑊

𝑚.𝐾

= 0.9737

309

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0017

ℎ𝑂 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33

𝑑𝑒= 7064.18 𝑊/𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod= outside dirt coefficient (fouling factor) =5000 W/mK

hid = inside dirt coefficient (fouling factor) = 5000 W/mK

kw = thermal conductivity of the tube wall material

di = tube inside diameter

do = tube outside diameter

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/mK.

1

𝑈𝑜=

1

8295.4+

1

5000+

0.019𝑙𝑛 (0.0190.0148)

2(18.8)+

0.019

0.0148×

1

5000+

0.019

0.0148×

1

3507.9

310

𝑈𝑜 = 𝟕𝟓𝟕. 𝟕𝟓𝑾/𝒎𝟐. 𝑲

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

𝟕𝟓𝟕. 𝟓𝟕 − 750

750× 100% = 1.033%

Hence, Uo assume is between 0% – 30%. So, Uo= 750 W/m2 K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.0029

For isothermal flow,

∆𝑃 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= ∆𝑃 =

19616.37𝑁

𝑚2= 0.20𝑏𝑎𝑟

* 2.5 is the recommended value for the velocity heads per pass. Neglecting the viscosity

correction term

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.0036

∆𝑃 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2= 74496.82 𝑁/𝑚2 = 0.74𝑏𝑎𝑟

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

311

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟏𝟒𝟔. 𝟗𝟕𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

2104.97𝐾𝑊 × 1000

𝟐𝟔. 𝟏𝟐𝑚2= 𝟕𝟕𝟕𝟓𝟒. 𝟕𝟓 𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 70℃ +

𝟕𝟕𝟕𝟓𝟒. 𝟕𝟓𝑊𝑚2

2161.27𝑊𝑚2 °𝐶

= 160.98℃

𝑊ℎ𝑒𝑛 𝑡 = 160.98℃, 𝜇 = 0.00014 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.00014

0.00013991)0.14

= 𝟏. 𝟎

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 13: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

Tube Pitch = 0.0238m, tube diameter = 0.0148m

0.0238 − 0.0148

0.0148× 100% = 60.57%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where

Dopt = optimum diameter (m), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

Tube

𝐷𝑜𝑝𝑡 = 8.41(8.39)0.45

(982.29)0.31 = 0.179𝑚

Therefore, a 4.49 m diameter nozzle was specified for the tube-side inlet

Shell

312

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(25.11)0.45

(999.2)0.31 = 0.086𝑚

A nozzle size of 2.15 m diameter is selected for the inlet and outlet at the shell side of the

exchanger.

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

K fiber glass= 0.04 W/m.K

r = 𝐾

ℎ𝑜=

0.04

7959.64 =0.000057 𝑚 = 5.7x10

-3 mm

Summary

Fixed and U-tube exchanger, one shell pass, and two tube passes.

Stainless Steel tubes, 2.44 m long, 19.05 mm o.d., 14.8 mm i.d., triangular pitch=23.8 mm.

Heat transfer area 188.79 m2 (based on outside diameter).

Shell i.d. 1.03 m, baffle spacing 0.029 m, baffle diameter 25% cut.

Tube-side coefficient 2161.27 W/m2. K, clean.

Shell-side coefficient 7064.18 W/ m2. K, clean.

Overall coefficient, estimated 750 W/m2. K.

Overall coefficient, calculated 757.50W/m2. K.

Dirt/fouling factors:

Tube side (chilled water) 5000 (W/m2. K)

-1.

Shell side (process fluid) 5000 (W/m2. K)

-1.

Pressure drops:

Tube side, estimated 0.20 bar; allowable 0.8 bar.

Shell side, estimated 0.74 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.179 m and 0.086m , respectively.

313

E-104 - Heater

The heater E-104 is used to heat up the process fluid from T= 62OC to T= 110

OC. The steam used

to heat the mixture enters at T=250OC and leaves at T=150

OC at 7 bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

314

Design Procedure

Step 1: Specification

Specification Tube Shell

Heat Duty (kW) 2208.98

Inlet Temperature (OC) Tc2 = 250 Th1 = 62

Outlet Temperature

(OC) Tc1 = 150 Th2 = 110

Pressure (bar) 7.50 7.50

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 95.12 𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠×

1000𝑘𝑔

1 𝑡𝑜𝑛= 𝟐𝟔. 𝟒𝟐

𝒌𝒈

𝒔

Mass flow rate for shell side = 5656.13𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 𝟏. 𝟓𝟕

𝒌𝒈

𝒔

Step 2: Physical Properties

Mean Temperature of compressed water at tube side:

= 250+150

2= 200℃

Mean temperature of process fluid at shell side:

= 62+110

2= 86℃

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Step 2: Physical

Properties Tube Shell

315

Mean Temperature (OC) 200 81

Total molecular 26.42 1.57

Density (kg/m3) 859.87 635.63

Viscosity (Pa.s) 0.0001325 0.00002

K (W/m.K) 0.66185 0.14425

Cp kJ/kg.K 4.8836 2.8294

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with organic solvent as the hot fluid and compressed

water as cold fluid, the overall coefficient will be in the range of 500-1000 W/m2. K. To start with,

the overall coefficient (U) is taken to be 950 W/m2. K.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(250 − 110) − (150 − 62)

ln (250 − 110150 − 62

)= 111.99℃

𝑅 =𝑇𝐻1 − 𝑇𝐻2

𝑇𝐶1 − 𝑇𝐶2=

250 − 150

110 − 60= 2.9167

𝑆 =𝑇𝐶1 − 𝑇𝐶2

𝑇𝐻1 − 𝑇𝐶2=

110 − 62

250 − 150= 0.2553

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft = 0.8091

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 180.6℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

2208.98

950 × 90.6186= 25.6596

316

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

Step 6: Layout and Tube Size

In order to obtain higher efficiency and ease the cleaning process, a split-ring floating-

head exchanger is used.

The material of construction for heat exchangers is stainless steel 316. Fluid with the

lowest allowable pressure drop should be allocated to the tube side. Besides allocating

lowest flowrate fluid to the shell-side will give the most economical design.

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 19.05 mm = 0.01905m

Internal diameter, DI = 14.83 mm = 0.01483 m

Length of tube, LT = 3.66 m long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0238𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.019 𝑚 × 3.66 𝑚 = 0.219𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 25.659 𝑚2

0.219𝑚2= 𝟏𝟏𝟕

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes or multiple of four is

selected. So, for 1 passes, tubes per pass = 117 tubes

317

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.015)2

4= 1.727 × 10−4𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 117 × 1.727 × 10−4𝑚2 = 0.0202𝑚2

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 24.42𝑘𝑔/𝑠

859.865𝑘𝑔/𝑚3= 0.0307𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.03073𝑚3/𝑠

0.0202𝑚2= 1.5186 𝑚/𝑠

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 2 tube passes,

K1 = 0.319 n1 =2.142

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.019 (238

0.249)

12.207⁄

= 0.30𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 0.43m, the

shell clearance is 54 mm = 0.054m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 0.30𝑚 + 0.35𝑚 = 𝟎. 𝟔𝟓 𝒎

TEMA standard Ds is max 1520mm. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

56.15𝑘𝑔𝑠

0.0204𝑚2= 𝟏𝟑𝟎𝟓. 𝟕𝟗 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

𝟏𝟑𝟎𝟓.𝟕𝟗𝑘𝑔

𝑚2𝑠×0.0148𝑚

0.00013251𝑘𝑔

𝑚.𝑠

= 146138.67

318

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

3.6750𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.00013251

𝑘𝑔𝑚. 𝑠

0.6198𝑊

𝑚.𝐾

= 0.9778

𝐿

𝑑𝑜=

2.44 𝑚

0.019 𝑚𝑚= 𝟏𝟗𝟐. 𝟏𝟑

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0027

ℎ𝑖 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33(

𝜇

𝜇𝑤)0.14

𝑑𝑖= 14850.47 𝑊/𝑚2𝐾 Neglect (

𝜇

𝜇𝑤)

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n= 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

0.49

5= 0.0177𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.0125 𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.019(0.02382 − 0.917 × 0.0192) = 0.0135𝒎

319

𝑠ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

1.5711𝑘𝑔𝑠

0.02028𝑚2= 1252.66 𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

1252.66𝑘𝑔𝑚2𝑠

× 0.0135𝑚

0.0002𝑘𝑔𝑚. 𝑠

= 90434.10

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

12.8294𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0002

𝑘𝑔𝑚. 𝑠

0.14425𝑊

𝑚.𝐾

= 3.6750

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0022

ℎ𝑂 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33

𝑑𝑒= 3274.28 𝑊/𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod= outside dirt coefficient (fouling factor) =5000 W/mK

hid = inside dirt coefficient (fouling factor) = 5000 W/mK

320

kw = thermal conductivity of the tube wall material

di = tube inside diameter

do = tube outside diameter

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/mK.

1

𝑈𝑜=

1

588.2+

1

5000+

0.019𝑙𝑛 (0.0190.0148)

2(18.8)+

0.019

0.0148×

1

5000+

0.019

0.0148×

1

14850.47

𝑈𝑜 = 𝟏𝟎𝟑𝟖𝑾/𝒎𝟐. 𝑲

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

𝟏𝟎𝟑𝟖. 𝟕𝟔 − 950

950× 100% = 9.34%

Hence, Uo assume is between 0% – 30%. So, Uo= 1038 W/m2 K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.0027

For isothermal flow,

∆𝑃 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= ∆𝑃 = 6593.28

𝑁

𝑚2= 0.065 𝑏𝑎𝑟

* 2.5 is the recommended value for the velocity heads per pass. Neglecting the viscosity

correction term

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.0015

∆𝑃 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2= 80157

𝑁

𝑚2= 0.80158𝑏𝑎𝑟

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

321

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟏𝟗. 𝟓𝟖 𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

2208.9778𝐾𝑊 × 1000

𝟏𝟗. 𝟓𝟖𝑚2= 𝟏𝟏𝟎𝟓𝟖𝟒. 𝟔𝟐𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 200℃ +

𝟏𝟏𝟎𝟓𝟖𝟒. 𝟔𝟐𝑊𝑚2

17479.26𝑊𝑚2 °𝐶

= 206.33℃

𝑊ℎ𝑒𝑛 𝑡 = 206.33℃, 𝜇 = 0.0008 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.00013251

0.00013)0.14

= 𝟏. 𝟎

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 14: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

Tube Pitch = 0.0238m, tube diameter = 0.0148m

0.0238 − 0.0148

0.0148× 100% = 60.57%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

322

Where

Dopt = optimum diameter (m), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

Tube

𝐷𝑜𝑝𝑡 = 8.41(26.42)0.45

(859.865)0.31 = 0.180𝑚

Therefore, a 0.180 m diameter nozzle was specified for the tube-side inlet

Shell

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(1.5711)0.45

(635.63)0.31 = 0.056 𝑚

A nozzle size of 0.056 m diameter is selected for the inlet and outlet at the shell side of the

exchanger.

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

K fiber glass= 0.04 W/m.K

r = 𝐾

ℎ𝑜=

1.5711

635.63 =0.0000122𝑚𝑚 = 0.01222 m

323

Summary

Split ring, floating head, one shell pass, and 1 tube passes.

Stainless Steel tubes, 3.66 m long, 19.05 mm o.d., 14.8 mm i.d., triangular pitch=23.8 mm.

Heat transfer area 25.66 m2 (based on outside diameter).

Shell i.d. 0.354 m, baffle spacing 0.0177 mm, baffle 25% cut.

Tube-side coefficient 17479.26 W/m2. K, clean.

Shell-side coefficient 3274.28 W/ m2. K, clean.

Overall coefficient, estimated 500 W/m2. K.

Overall coefficient, calculated 421.87 W/m2. K.

Dirt/fouling factors:

Tube side (compressed water) 5000 (W/m2.

K)-1

.

Shell side (process fluid) 5000 (W/m2. K)

-1.

Pressure drops:

Tube side, estimated 0.066 bar; allowable 0.8 bar.

Shell side, estimated 0.80 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.18 m and 0.056 m, respectively.

324

E-105 – Condenser

The condenser E-105 is used to condense the process mixture at 1 bar from T=38OC to T=

33OC.The brine solution used to condense the mixture enters at T=5

OC and leaves at T=15

OC at 1

bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

325

Design Procedure

Step 1: Specification

Specification Tube Shell

Heat Duty (kW) 7989.0278

Inlet Temperature (OC) Tc2 5 Th1 38

Outlet Temperature

(OC) Tc1 15 Th2 33

Pressure (bar) 1.00 1.00

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 343.9𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠×

1000𝑘𝑔

1 𝑡𝑜𝑛 = 𝟗𝟓. 𝟓𝟑

𝒌𝒈

𝒔

Mass flow rate for shell side = 23541.029𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 𝟔. 𝟓𝟏

𝒌𝒈

𝒔

Step 2: Physical Properties

Mean Temperature of process fluid at tube side:

= 151.63+260

2= 214.8℃

Mean temperature of steam at shell side:

= 350+260

2= 310℃

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Physical Properties Tube Shell

Mean Temperature (OC) 10 35.5

Total molecular 18.7158 132.5786

Density (kg/m3) 1100.80 792.97

Viscosity (Pa.s) 0.001317 0.000464

K (W/m.K) 0.62354 0.23951

Cp kJ/kg.K 4.1787 2.7849

326

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with steam as the hot fluid and process fluid as cold

fluid, the overall coefficient will be in the range of 500-700 W/m2. K. To start with, the overall

coefficient (U) is taken to be 75W/m2. K.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(38 − 15) − (33 − 5)

ln (38 − 1533 − 5

)= 25.4181℃

𝑅 =𝑇𝐻1 − 𝑇𝐻2

𝑇𝐶1 − 𝑇𝐶2=

5 − 33

33 − 38= 5.60

𝑆 =𝑇𝐶1 − 𝑇𝐶2

𝑇𝐻1 − 𝑇𝐶2=

33 − 38

38 − 5= 0.1515

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft = 0.8190

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 20.8163℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

1881.22

75 × 79.37= 697.79 𝑚2

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

Step 6: Layout and Tube Size

327

In order to obtain higher efficiency and ease the cleaning process, a split-ring floating-

head exchanger is used.

The material of construction for heat exchangers is stainless steel 316. A higher pressure

stream should be allocated to the tube side as high-pressure tube is cheaper than high-

pressure shell. Besides the more corrosive material should allocated to the tube side to

reduce cost.

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 25 mm = 0.025m

Internal diameter, DI = 22.8 mm = 0.0228m

Length of tube, LT = 4.88m (16 ft) long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0313𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.01905𝑚 × 5 𝑚 = 0.2992𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 697.7940 𝑚2

0.2992𝑚2= 𝟐𝟑𝟑𝟐

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes or multiple of four is

selected. So, for 6 passes, tubes per pass = 389 tubes

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.01905)2

4= 0.0002668 𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 389 × 0.0002668𝑚2 = 0.10368𝑚2

328

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 95.53𝑘𝑔/𝑠

1100.8𝑘𝑔/𝑚3= 0.08678 𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.08678𝑚3/𝑠

0.10368𝑚2= 0.8370 𝑚/𝑠

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 2 tube passes,

K1 = 0.0742 n1 =2.499

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.025 (2332

0.0742)

12.207⁄

= 1.20 𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 1.20 m,

the shell clearance is 75 mm = 0.075 m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 1.20𝑚 + 0.075 𝑚 = 𝟏. 𝟐𝟎𝟕𝟓𝒎

TEMA standard Ds is max 1520mm. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

95.53𝑘𝑔𝑠

0.10368𝑚2= 𝟗𝟐𝟏. 𝟑𝟔𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

𝟗𝟐𝟏. 𝟑𝟔𝑘𝑔𝑚2𝑠

× 0.01843𝑚

0.001317𝑘𝑔𝑚. 𝑠

= 12893.40

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

4.1787𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.001317

𝑘𝑔𝑚. 𝑠

0.62354𝑊

𝑚.𝐾

= 8.8260

𝐿

𝑑𝑜=

5 𝑚

0.01905 𝑚= 𝟐𝟔𝟐. 𝟒𝟕

329

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0045

ℎ𝑖 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33(

𝜇

𝜇𝑤)0.14

𝑑𝑖= 1735.15 𝑊/𝑚2𝐾 Neglect (

𝜇

𝜇𝑤)

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n= 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

1.28

5= 0.2552 𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.06513 𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.025(0.03132 − 0.917 × 0.0252) = 0.01353𝒎

𝑠ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

6.5142𝑘𝑔𝑠

0.06512𝑚2= 100.02𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

100.02𝑘𝑔𝑚2𝑠

× 0.01353𝑚

0.00046375𝑘𝑔𝑚. 𝑠

= 2917.49

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

2.7849𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.00046375

𝑘𝑔𝑚. 𝑠

0.23941𝑊

𝑚.𝐾

= 5.3946

330

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0098

ℎ𝑂 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33

𝑑𝑒= 887.51 𝑊/𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod= outside dirt coefficient (fouling factor) =5000 W/mK

hid = inside dirt coefficient (fouling factor) = 5000 W/mK

kw = thermal conductivity of the tube wall material

di = tube inside diameter

do = tube outside diameter

331

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/mK.

1

𝑈𝑜=

1

103.1+

1

5000+

0.025𝑙𝑛 (0.0250.0228)

2(18.8)+

0.025

0.0228×

1

5000+

0.025

0.022148×

1

1735.15

𝑈𝑜 = 𝟓𝟓𝟑. 𝟒𝟒 𝒘/𝒎𝟐. 𝑲

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

𝟓𝟓𝟑. 𝟒𝟒 − 500

500× 100% = 0.62%

Hence, Uo assume is between 0% – 30%. So, Uo= 75W/m2 K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.0045

For isothermal flow,

∆𝑃𝑇 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= ∆𝑃 = 27643.55 𝑁/𝑚2 = 0.27

* 2.5 is the recommended value for the velocity heads per pass. Neglecting the viscosity

correction term

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.0059

∆𝑃𝑆 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2= 550.33

𝑁

𝑚2= 0.0055𝑏𝑎𝑟

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

332

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟔𝟕𝟓. 𝟎𝟖 𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

7989.03𝐾𝑊 × 1000

𝟔𝟕𝟓. 𝟎𝟖𝑚2= 𝟏𝟏𝟖𝟑𝟒. 𝟏𝟑 𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 10℃ +

𝟔𝟓𝟐𝟔. 𝟗𝟏𝑊𝑚2

1735.15𝑊𝑚2 °𝐶

= 12.94℃

𝑊ℎ𝑒𝑛 𝑡 = 211.04℃, 𝜇 = 0.0008 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.0013171

0.001317)0.14

= 𝟏. 𝟎

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 14: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

Tube Pitch = 0.02382m, tube diameter = 0.01483m

0.02382 − 0.01843

0.01843× 100% = 29.21%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where

Dopt = optimum diameter (m), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

333

Tube

𝐷𝑜𝑝𝑡 = 8.41(95.53)0.45

(1100.8)0.31 = 0.30 𝑚

Therefore, a 0.30 m diameter nozzle was specified for the tube-side inlet

Shell

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(6.5142)0.45

(792.97)0.31 = 0.10𝑚

A nozzle size of 0.10 m diameter is selected for the inlet and outlet at the shell side of the

exchanger.

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

K fiber glass= 0.04 W/m.K

r = 𝐾

ℎ𝑜=

0.04

103.1 =3.9 × 10−4𝑚=0.39 mm

334

Summary

Split ring, floating head, one shell pass, and 6 tube passes.

Stainless Steel tubes, 5 m long,0.01905m o.d., 0.01843m i.d., triangular pitch=0.02381 mm.

Heat transfer area 697.79 m2 (based on outside diameter).

Shell i.d. 1.276m, baffle spacing 0.2552m, 25% cut.

Tube-side coefficient 4027.36 W/m2.K, clean.

Shell-side coefficient 887.51 W/ m2. K, clean.

Overall coefficient, estimated 550 W/m2. K.

Overall coefficient, calculated 553.4 W/m2. K.

Dirt/fouling factors:

Tube side (process fluid) 5000 (W/m2. K)

-1.

Shell side (steam) 5000 (W/m2.

K)-1

.

Pressure drops:

Tube side, estimated 0.276 bar; allowable 0.8 bar.

Shell side, estimated 0.0055 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.30 m and 0.10 m, respectively.

335

E-106 Reboiler

The Reboiler E-106 is used to vaporise the process mixture at 25 bar from T=90OC to T= 100

OC.

The steam used to heat up the mixture enters at T=250OC and leaves at T=150

OC at 26 bar.

Reference:

1. The calculation here follow the example paged 623-630 from Coulson and Richardson’s,

“Chemical Engineering, Volume 6”, 4th

edition.

2. FELDER, R. M. R., R. W. 2005. Elementary Principles of Chemical Processes, John

Wiley & Sons, Inc.

3. PERRY, R. H. A. G., DON W. 1984. Perry's Chemical Engineers' Handbook McGraw-

Hill.

4. SINNOTT, R. K. 2003. Chemical Engineering, Butterworth-Heineman

Design parameters:

Outside diameter (OD) and inside diameter (ID) for tubes Number of tubes

Number of tube passes and shell passes

Diameter of tube bundle, DB

Diameter of shell, DS

Baffle spacing, lb

Overall heat transfer coefficient

Tube side pressure drop, ΔPt

Shell side pressure drop, ΔPs

336

Design Procedure

Step 1: Specification

Specification Tube Shell

Heat Duty (kW) 5919.03

Inlet Temperature (OC) Tc2 = 90 Th1 = 250

Outlet Temperature

(OC) Tc1 = 100 Th2 = 150

Pressure (bar) 25.00 26.00

Number of parallel heat exchanger = 1

From energy balance calculation,

Mass flow rate for tube side = 20888.215 𝑘𝑔

ℎ𝑟×

1ℎ𝑟

3600𝑠 = 𝟓. 𝟖𝟎𝟐𝟑

𝒌𝒈

𝒔

Mass flow rate for shell side = 1.92𝑡𝑜𝑛

ℎ𝑟×

1ℎ𝑟

3600𝑠×

1000𝑘𝑔

1 𝑡𝑜𝑛 = 𝟎. 𝟓𝟑

𝒌𝒈

𝒔

Step 2: Physical Properties

Mean Temperature of chilled water at tube side:

= 90+100

2= 95℃

Mean temperature of process fluid at shell side:

= 250+150

2= 200℃

The function of temperature for viscosity, density, heat capacity and also conductivity have been

created in the excel file. Therefore, the physical properties of the mixture have calculated based on

the mean temperature of each shell and tube side.

Physical Properties Tube Shell

Mean Temperature (OC) 95 200

Total molecular 31.9790 18.0200

Density (kg/m3) 715.37 958.15

337

Viscosity (Pa.s) 0.0001371 0.0001375

K (W/m.K) 0.1904 0.6619

Cp kJ/kg.K 3.1432 4.8658

Step 3: Overall Coefficient

From table 12.1 in reference 1, for a system with aqueous vapours as the hot fluid and water as

cold fluid, the overall coefficient will be in the range of 600-900 W/m2. K. To start with, the

overall coefficient (U) is taken to be 800W/m2. K.

Step 4: True mean temperature difference

For 1 shell and 2 tubes pass exchanger,

Logarithmic mean temperature:

∆𝑇𝑙𝑚 =(𝑇𝐻1 − 𝑇𝐶1) − (𝑇𝐻2 − 𝑇𝐶2)

ln ((𝑇𝐻1 − 𝑇𝐶1)𝑇𝐻2 − 𝑇𝐶2

)=

(250 − 100) − (150 − 90)

ln (250 − 100150 − 90

)= 98.22℃

𝑅 =𝑇𝐻1 − 𝑇𝐻2

𝑇𝐶1 − 𝑇𝐶2=

250 − 100

100 − 90= 10.00

𝑆 =𝑇𝐶1 − 𝑇𝐶2

𝑇𝐻1 − 𝑇𝐶2=

100 − 90

250 − 90= 0.0625

Temperature correction factor,

]11[2

]11[2ln1

)1(

1ln1

2

2

2

RRS

RRSR

RS

SR

Ft= 0.9817

∆𝑇𝑚 = 𝐹𝑇∆𝑇𝑙𝑚 = 96.4254℃

Step 5: Heat Transfer Area

𝐴 =𝑄

𝑈∆𝑇𝑚=

5919.03

800 × 96.43= 76.7307𝑚2

* As first estimation, the heat transfer area needed lied in the normal area of a shell and tube

exchanger, which are 3-1000m2, thus, a shell and tube exchanger is selected.

338

Step 6: Layout and Tube Size

In order to obtain higher efficiency and ease the cleaning process, a split-ring floating-

head exchanger is used.

The material of construction for heat exchangers is stainless steel 316. Allocating the fluid

with the highest flow rate to the tube side will normally give the most economical design.

Besides, in reference 1, it is said that the fluid with the lowest allowable pressure drop

should be allocated to the tube side.

The preferred tube diameter for most duties is from 5/8 to 2 in., as they will give more compact

and therefore cheaper exchangers.

Outer diameter, DO = 19.05 mm = 0.0126m

Internal diameter, DI = 14.8 mm = 0.016m

Length of tube, LT = 5m long, which is the most popular size.

As there is no presence of heavily fouling fluids in this system, triangular pattern of tube

arrangements can be applied. The triangular patterns can give a higher heat transfer rates.

The recommended tube pitch (distance between tube canters) is 1.25 × 𝐷𝑂 = 0.0238𝑚 is

employed.

Step 7: Number of Tubes

Area of one tube (neglecting thickness of tube sheets)

= 𝜋 × 𝐷𝑂 × 𝐿𝑇 = 𝜋 × 0.016 𝑚 × 5 𝑚 = 0.2513𝑚2

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓𝑡𝑢𝑏𝑒𝑠 = 76.73 𝑚2

0.2513𝑚2= 𝟑𝟎𝟓

339

Earlier before, a heat exchanger with 1 shell passes and 2 tubes passes or multiple of four is

selected. So, for 2 passes, tubes per pass = 153 tubes

𝑇𝑢𝑏𝑒 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 = 𝜋 × (𝐷𝐼)

2

4=

𝜋 × (0.016)2

4= 0.00012469 𝑚2

𝐴𝑟𝑒𝑎 𝑝𝑒𝑟 𝑝𝑎𝑠𝑠 = 153 × 0.00012649 𝑚2 = 0.01903𝑚2

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 5.8023𝑘𝑔/𝑠

715.37𝑘𝑔/𝑚3= 0.008111𝑚3/𝑠

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝑢𝑡 = 0.008111𝑚3/𝑠

0.00012649𝑚2= 0.42613 𝑚/𝑠

Step 8: Bundle and Shell Diameter

From Table 12.4 (Coulson & Richardson’s Chemical Engineering), for 2 tube passes,

K1 = 0.249 n1 =2.207

𝐵𝑢𝑛𝑑𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝐷𝑏(𝑚𝑚) = 𝑑𝑜 (𝑁𝑡

𝐾1)

1𝑛1

= 0.019 (305

0.249)

12.207⁄

= 0.4014𝑚

where Nt= number of tubes

do= tube outside diameter, mm

Referring to Figure 12.10 (Coulson & Richardson’s Chemical Engineering), when Db= 0.4014 m,

the shell clearance is 55mm = 0.055m.

Hence, the shell inside diameter will be:

𝐷𝑠 = 0.40𝑚 + 0.055𝑚 = 𝟎. 𝟒𝟓𝟔𝟒𝒎

TEMA standard Ds is max 1520mm. So, Ds is within the allow range.

Step 9: Tube-side Heat Transfer Coefficient

𝑇𝑢𝑏𝑒 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑡 =𝑊𝑡

𝐴𝑡=

5.80223𝑘𝑔𝑠

0.019034𝑚2= 𝟐𝟖𝟎𝟎𝟖. 𝟓𝟎 𝒌𝒈/𝒎𝟐𝒔

340

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑡𝑑𝑖

𝜇𝑐=

𝟐𝟖𝟎𝟎𝟖.𝟓𝟎𝑘𝑔

𝑚2𝑠×0.0148𝑚

0.0001371𝑘𝑔

𝑚.𝑠

=28008.50

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,𝑐𝜇𝑐

𝑘𝑐=

3.1432𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 0.0001371

𝑘𝑔𝑚. 𝑠

0.1904𝑊

𝑚.𝐾

= 2.2637

𝐿

𝑑𝑜=

5 𝑚

0.01903 𝑚= 𝟑𝟏𝟐. 𝟓

From Figure 12.23 (Coulson & Richardson’s Chemical Engineering),

ℎ𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0038

ℎ𝑖 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33(

𝜇

𝜇𝑤)0.14

𝑑𝑖= 8269.34 𝑊/𝑚2𝐾 Neglect (

𝜇

𝜇𝑤)

Step 10: Shell-side Heat Transfer Coefficient

For first trial, take n= 5, 𝑏𝑎𝑓𝑓𝑙𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔, 𝑙𝑏 =𝐷𝑠

𝑛=

0.4567

5= 0.02282𝑚

𝐶𝑟𝑜𝑠𝑠 𝑓𝑙𝑜𝑤 𝑎𝑟𝑒𝑎, 𝐴𝑠 =(𝑝𝑡 − 𝑑𝑜)𝐷𝑠𝑙𝐵

𝑝𝑡= 0.002083𝑚2

For an equilateral triangular pitch arrangement, equivalent diameter can be calculated using the

formula as below:

𝑑𝑒 =1.1

𝑑𝑜

(𝑝𝑡2 − 0.917𝑑𝑜

2) =1.1

0.019(0.02382 − 0.917 × 0.0192) = 0.01136𝒎

341

𝑠ℎ𝑒𝑙𝑙 𝑠𝑖𝑑𝑒 𝑚𝑎𝑠𝑠 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦, 𝐺𝑠 =𝑊𝑠

𝐴𝑠=

0.5333𝑘𝑔𝑠

0.00208𝑚2= 256.07𝒌𝒈/𝒎𝟐𝒔

𝑅𝑒𝑦𝑛𝑜𝑙𝑑𝑠 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑅𝑒 =𝐺𝑠𝑑𝑒

𝜇ℎ=

256.07𝑘𝑔𝑚2𝑠

× 0.01136𝑚

1.96 × 10−5 𝑘𝑔𝑚. 𝑠

= 21165.54

𝑃𝑟𝑎𝑛𝑑𝑡𝑙 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑃𝑟 =𝐶𝑝,ℎ𝜇ℎ

𝑘ℎ=

4.8658𝑘𝐽

𝑘𝑔. 𝐾× 1000 × 1.96 × 10−5 𝑘𝑔

𝑚. 𝑠

0.66185𝑊

𝑚.𝐾

= 1.0105

A 25% baffle cut is chosen and from Figure 12.29 (Coulson & Richardson’s Chemical

Engineering), 𝐻𝑒𝑎𝑡 𝑡𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑗ℎ = 0.0099

ℎ𝑂 =𝑘𝑓𝑗ℎ𝑅𝑒𝑃𝑟0.33

𝑑𝑒= 12249.78 𝑊/𝑚2𝐾

Step 11: Overall Coefficient

1

𝑈𝑜=

1

ℎ0+

1

ℎ𝑜𝑑+

𝑑𝑜𝑙𝑛 (𝑑𝑜

𝑑𝑖)

2𝐾𝑤+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖×

1

ℎ𝑖

Where

Uo = overall coefficient based on the outside area of the tube

ho = outside fluid film coefficient

hi = inside fluid film coefficient

hod= outside dirt coefficient (fouling factor) =5000 W/mK

hid = inside dirt coefficient (fouling factor) = 5000 W/mK

kw = thermal conductivity of the tube wall material

342

di = tube inside diameter

do = tube outside diameter

The stainless steel as the material of construction has a conductivity Kw of 18.8 W/mK.

1

𝑈𝑜=

1

1113.92+

1

5000+

0.019𝑙𝑛 (0.0190.0148)

2(18.8)+

0.019

0.0148×

1

5000+

0.019

0.0148×

1

8269.34

𝑈𝑜 = 𝟖𝟎𝟔. 𝟑𝟓𝑾/𝒎𝟐. 𝑲

𝑈𝑜,𝑐𝑎𝑙𝑐 − 𝑈𝑜,𝑎𝑠𝑠𝑢

𝑈𝑜,𝑎𝑠𝑠𝑢× 100% =

𝟖𝟎𝟔. 𝟑𝟓 − 800

800× 100% = 0.793%

Hence, Uo assume is between 0% – 30%. So, Uo= 800W/m2 K is acceptable.

Step 12: Pressure Drop

Tube side

From figure 12.24 reference 1, jf = 0.003

For isothermal flow,

∆𝑃 = 𝑁𝑝 [8𝑗𝑓 (𝐿

𝑑𝑖) (

𝜇

𝜇𝑤)−𝑚

+ 2.5]𝜌𝑢𝑡

2

2= ∆𝑃 = 1299/𝑚2 = 0.01299

* 2.5 is the recommended value for the velocity heads per pass. Neglecting the viscosity

correction term

This is within the specification with 0.8 bar.

Shell side

The pressure drop in the shell side is predicted using Kern‟s method.

Again, neglecting the viscosity correction term;

From figure 12.24, jf = 0.03

∆𝑃 = [8𝑗𝑓 (𝐷𝑠

𝑑𝑒) (

𝐿

𝑙𝐵)]

𝜌𝑢𝑠2

2=

60240.41𝑁

𝑚2= 0.6024 𝑏𝑎𝑟

343

This result is well within specification as the allowable pressure drop for this stream is 0.8 bar.

Step 13: Viscosity Correction Factor

The correction factor (μ/μw) was neglected when calculating the heat transfer coefficients and

pressure drops.

Estimate of the temperature at the tube wall, tw is needed in order to check on the viscosity

correction temperature.

𝐼𝑛𝑠𝑖𝑑𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝜋 × 𝐷𝐼 × 𝐿 × 𝑁𝑜. 𝑜𝑓 𝑡𝑢𝑏𝑒𝑠 = 𝟔𝟎. 𝟎𝟒𝒎𝟐

𝐻𝑒𝑎𝑡𝑓𝑙𝑢𝑥, 𝑞 =𝑄

𝐴=

5919.03𝐾𝑊 × 1000

𝟔𝟎. 𝟎𝟒𝑚2= 𝟗𝟖𝟓𝟗𝟐. 𝟗𝟕𝑾/𝒎𝟐

(𝑡 − 𝑡𝑤)ℎ𝑖 = 𝑞

𝑡𝑤 = 𝑡 +𝑞

ℎ𝑖= 95℃ +

𝟗𝟖𝟓𝟗𝟐. 𝟗𝟕𝑊𝑚2

8269.34𝑊𝑚2 °𝐶

= 141.51℃

𝑊ℎ𝑒𝑛 𝑡 = 141.51℃, 𝜇𝑤 = 0.000137 𝑃𝑎. 𝑠

(𝜇

𝜇𝑤)0.14

= (0.0013701

0.000137)0.14

= 𝟏. 𝟎

∴ 𝑇ℎ𝑒 𝑑𝑒𝑐𝑖𝑠𝑖𝑜𝑛 𝑡𝑜 𝑛𝑒𝑔𝑙𝑒𝑐𝑡 𝑖𝑡 𝑤𝑎𝑠 𝑗𝑢𝑠𝑡𝑖𝑓𝑖𝑒𝑑.

Step 14: Mechanical design

Tube plate design

General requirements (AS1210)

Tube pitch must be more than 25% larger than the tube diameter fulfilled.

Tube Pitch = 0.02m, tube diameter = 0.0126m

0.02 − 0.0126

0.0126× 100% = 58.73%

Nozzles Diameter

The Harker equation (1978), modified for SI units, for the optimum pipe (and nozzle) diameter is:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Where

344

Dopt = optimum diameter (m), W = mass flow rate, kg/hr, ρ = fluid density, kg/m3

For this system, the nozzle diameter at the outlet and inlet of the tube and shell side can be taken

as the same as there is no phase change occur and the density change is negligible.

Tube

𝐷𝑜𝑝𝑡 = 8.41(5.8023)0.45

(715.37)0.31 = 0.0963 𝑚

Therefore, a 0.0963 m diameter nozzle was specified for the tube-side inlet

Shell

Nozzle

𝐷𝑜𝑝𝑡 = 8.41(0.5333)0.45

(958.15)0.31 = 0.0301𝑚

Therefore, a 0.0301 m diameter nozzle was specified for the shell-side inlet

Support design

For a horizontal vessel, it is usually mounted on two saddles supports.

Foundation: Concrete slab

Insulation

We were using fiber glass for insulated the heat exchanger.

K fiber glass= 0.04 W/m.K

r = 𝐾

ℎ𝑜=

0.04

12249 =0.00000327m =0.00336 mm

345

Summary

Split ring, floating head, one shell pass, and two tube passes.

Stainless Steel tubes, 5 m long, 0.016 m o.d., 0.0126m i.d., triangular pitch = 0.02 m.

Heat transfer area 77.12 m2 (based on outside diameter).

Shell i.d. 0.456m, baffle spacing 0.0228 m, 25% cut.

Tube-side coefficient 2106.20 W/m2. K, clean.

Shell-side coefficient 12249.78 W/ m2. K, clean.

Overall coefficient, estimated 800 W/m2. K.

Overall coefficient, calculated 806.35W/m2. K.

Dirt/fouling factors:

Tube side (compressed water) 5000 (W/m2.

K)-1

.

Shell side (process fluid) 5000 (W/m2. K)

-1.

Pressure drops:

Tube side, estimated 0.013 bar; allowable 0.8 bar.

Shell side, estimated 0.60 bar; allowable 0.8 bar.

Nozzle diameter for tube and shell side is 0.0963 m and 0.0301 m, respectively.

346

Reactor Design MTBE REACTOR (R-101) DESIGN

Design Basic:

This plant design is aimed to produce 300,000 metric tonnes of Methyl Tert-Butyl Ether (MTBE)

per annum to fulfil the demand from market either local or international. Reactor is important as it

is where the desired product (MTBE) is formed from feed reactants. In this design, since a

continuous reaction is desired, so the reactor used is catalytic packed bed reactor where its

packings are made up catalyst named Amberlyst-15. Isobutylene will feed together with methanol

into the reactor. The operating temperature of the reactor is fixed at 75oC and pressure 1100kPa.

Water coolant is used to cool down the heat generated by the exothermic reaction in the reactor by

circulating cold water around the reactor. Since this reaction is reversible, to ensure the reaction

equilibrium always shift to right (towards the formation of MTBE), the temperature of reaction

must be low. Also, at low temperature the catalyst activity and life span can be prolonged. At the

operating condition, the conversion and selectivity of isobutylene to MTBE is 92% and 96.5%,

respectively.

Design Parameter:

Reactor design Mechanical design

xiii) Weight of catalysts

xiv) Number of tubes

xv) Tubes configuration

xvi) Shell dimension

xvii) Baffle configuration

xviii) Cooling requirement analysis

xix) Heat transfer area

xx) Heat transfer coefficient

xvii) Design temperature

xviii) Design pressure

xix) Material of construction

xx) Reactor head design

xxi) Wall thickness (Shell, tubes, vessel head)

xxii) L/D ratio

xxiii) Stress analysis

xxiv) Vessel support and base

xxv) Nozzle size

Design Criteria:

Operating Temperature : 75oC

Operating Pressure : 1100kPa

Vessel Orientation : Vertical

Type of Catalyst : Heterogeneous

Type of Reactor : Multi-tubular Packed Bed Reactor

Design Method:

This MTBE reactor in this plant is designed based on the kinetic data collected for MTBE

production. With the aids of POLYMATH®

software, the weight of catalyst required to achieve

the production rate can be determined. The cooling requirement design is based on shell and tube

heat exchanger design based on the requirement of TEMA. The mechanical design is based on

Coulson and Richardson’s Chemical Engineering Design. Physical property data of the process

fluid are obtained either from Perry’s Chemical Engineer’s Handbook or calculated using Aspen

Plus®

software.

Reactor Design

347

Step 1: Catalyst Bed Sizing

Based on the mass balance that has been submitted as Task 2, the desired product (MTBE) molar

flow rate in the outlet stream of the reactor (R-101) is 4.166 x 105 mol/hr. Polymath software is

used to perform the calculation based on the kitnetic data obtained from literature review, to

calculate the weight of catalyst (Amberlyst-15) bed required in order to obtain that particular

product outlet molar flow rate is 1.805 x 104 kg.

.

With the density of 770kg/m3, the volume of catalyst required for each reactor is 23.44 m

3.

Volume of catalyst bed, Vbed(m3) =

Catalyst mass,mcatalyst(kg)

Density of catalyst,ρcatalyst (kg

m3) = 23.4416 m

3

Since multitubular reactor is selected for reactor R-101, this amount of catalysts will be packed

into tubes with circulation of water coolant outside the tubes within the reactor shell to constantly

remove the heat generated from the exothermic reaction.

From literature review, the reaction rate is given by:

𝑟𝑀𝑇𝐵𝐸 = 𝑘𝑠𝐾𝐴𝑎

[ 𝐶𝐴

𝑎𝐶𝐵𝑏 −

𝐶𝐶𝑐

𝐾𝑒𝑞

(1 + 𝐾𝐴𝐶𝐴 + 𝐾𝐶𝐶𝐶)𝑎

]

𝑘𝑠 = 1.2 × 1013exp (−87900

𝑅𝑇)

𝐾𝐴 = 5.1 × 10−13exp (97500

𝑅𝑇)

𝐾𝐶 = 1.6 × 10−16exp (119000

𝑅𝑇)

ln(𝐾𝑒𝑞) = −10.0982 +4254.05

𝑇+ 0.2667 ln 𝑇 −

1

𝑅𝑇∑0.0242ʋ𝑖𝑉𝑖

𝑛

𝑖=1

(𝑃 − 𝑃𝑖′)

Where,

𝑘𝑠 = 𝑆𝑢𝑟𝑓𝑎𝑐𝑒 𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

𝐾𝐴 = 𝐸𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑎𝑑𝑠𝑜𝑟𝑝𝑡𝑖𝑜𝑛 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

𝐾𝐶 = 𝐸𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑎𝑑𝑠𝑜𝑟𝑝𝑡𝑖𝑜𝑛 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

𝐾𝑒𝑞 = 𝐸𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

348

𝐶𝐴 = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙

𝐶𝐵 = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐼𝑠𝑜𝑏𝑢𝑡𝑦𝑒𝑙𝑒𝑛𝑒

𝐶𝐶 = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑀𝑒𝑡ℎ𝑦𝑙 𝑇𝑒𝑟𝑡 − 𝐵𝑢𝑡𝑦𝑙 𝐸𝑡ℎ𝑒𝑟 (𝑀𝑇𝐵𝐸)

𝑎, 𝑏 𝑎𝑛𝑑 𝑐 = 𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑟𝑑𝑒𝑟 𝑓𝑜𝑟 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙, 𝐼𝑠𝑜𝑏𝑢𝑡𝑦𝑙𝑒𝑛𝑒 𝑎𝑛𝑑 𝑀𝑇𝐵𝐸

𝑅 = 𝐺𝑎𝑠 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡, 8.314𝐽

𝑚𝑜𝑙 ∙ 𝐾

𝑇 = 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒, 𝐾

𝑃 = 𝑃𝑟𝑒𝑠𝑠𝑢𝑟𝑒, 𝑎𝑡𝑚

𝑃𝑖′ = 𝑆𝑎𝑡𝑢𝑟𝑎𝑡𝑖𝑜𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝑓𝑜𝑟 𝑠𝑝𝑒𝑐𝑖𝑒𝑠 𝑖, 𝑎𝑡𝑚

ʋ𝑖 = 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑐𝑜𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑡

𝑉𝑖 = 𝑀𝑜𝑙𝑎𝑟 𝑙𝑖𝑞𝑢𝑖𝑑 𝑣𝑜𝑙𝑢𝑚𝑒,𝑚𝐿

𝑚𝑜𝑙

****The fourth term of the right hand side of equilibrium constant equation represents the

influence of pressure on fugacity and it was found to be negligible for pressures below 20 atm.

ODE Result Graph (extracted from Polymath)

Step 2: Reactor Tubes Sizing

a. Number of Tubes

The number of tubes to be installed for the catalyst packing in the multitubular reactor will be

determined using the equations below:

Volume of catalyst bed per tube, Vtube(m3) =

πdi2

4x Lt

Number of tube, N = Volume of catalyst bed, Vbed(m

3)

Volume of catalyst bed per tube, Vtube(m3)

where di = tube outer diameter , Lt = length of tube

349

The selection of tube will follow the fabricated tubing available in the market The tube selected is

the tube with NPS 2 inch (with outer diameter of 60.3mm) from ASME Schedule 10S. The

number of tubes are fixed at 300 tubes. As reported in the Perry’s Chemical Engineer’s Handbook,

maximum number of tubes for multitubular reactor used in the industries is 4000 tubes. Thus, the

designed number of tubes is logically acceptable within the range. Refer table below for the brief

specifications of the tube chosen.

From © Tioga Pipe, Inc. (PIPE DIMENSIONS AND WEIGHTS,

http://www.tiogapipe.com/assets/files/pipe-chart.pdf)

Tube Characteristics

Tube outer diameter, do (m) 0.0603

Thickness of tube (mm) 2.77

Tube inner diameter, di (m) 0.05476

Cross sectional area of tube (Inner), Ai (m2) 0.00235514

Cross sectional area of tube (Outer), Ao (m2) 0.002855778

Length of tube, Ltube (m) 7.32

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡𝑢𝑏𝑒, 𝐿𝑡𝑢𝑏𝑒(𝑚)

=𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 (𝑚3)

𝐿𝑒𝑛𝑔𝑡ℎ 𝑜𝑓 𝑡𝑢𝑏𝑒, 𝐿𝑡𝑢𝑏𝑒(𝑚) × Cross sectional area of tube (Inner), A𝑖(𝑚2)

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡𝑢𝑏𝑒, 𝐿𝑡𝑢𝑏𝑒(𝑚) = 1359.6 ≈ 1360

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 𝑏𝑒𝑑 𝑝𝑒𝑟 𝑡𝑢𝑏𝑒, 𝑉𝑡𝑢𝑏𝑒(𝑚3) =

𝜋𝑑02

4𝑥 𝐿𝑡𝑢𝑏𝑒= 0.0172m

3

b. Tubes Arrangement

Since the water is selected as the coolant for the heat removal, the tube will be arranged in

triangular pattern as it give higher heat-transfer rates. Generally, the tube pitch used is 1.25 times

the tube outside diameter.

350

c. Tube Bundle Diameter

𝐷𝑏 = 𝑑𝑜(𝑁𝑡

𝐾1)1/𝑛1

Where 𝐷𝑏= bundle diameter

𝑁𝑡= number of tubes

𝑑𝑜= tube outer diameter

Since only one tube pass in established in the reactor, constants used are:

K1= 0.319

n1 = 2.142

Substituting into the tube bundle diameter formula, we can obtain:

𝐷𝑏 = 𝑑𝑜(𝑁𝑡

𝐾1)1/𝑛1 = 2.9845 m

The tube in the centre row = 𝐷𝑏

𝑃𝑡=

2.9845

0.0905= 32.9966 ≈ 33 tubes

Step 3: Reactor Shell Sizing

a. Shell Diameter

The reactor shell sizing can be determined by considering a clearance between the outermost tube

in the bundle and the shell inside diameter. The shell diameter must be selected to give as close a

fit to the bundle as is practical. This can reduce the bypassing possibility of the heat transfer

media round the outside of the bundle.

𝑑𝑜 = 0.0603 𝑚

𝑃𝑡 = 1.25𝑑𝑜 = 0.075375𝑚

351

Based on the plot as shown above, an equation has been established to correlate the bundle

diameter and the clearance for fixed tube type.

Clearance, C (mm) = 10 Db + 8

With the bundle diameter, Db of 2.9845 m, clearance calculated is 37.85 mm.

Shell Diameter, Ds = Db + C = 3.0224 m ≈ 3.1 m

b. Baffle Configuration

Baffles are used in the shell to direct the fluid stream across the tubes, to increase the fluid

velocity, and so to improve the rate of heat transfer. Single segmental baffle with 25% baffle cut

will be used for optimum heat transfer rate. Figure below shows the single segmental baffle.

The baffle spacing used is normally at the range of 0.2 to 1.0 shell diameter. Since close baffle

spacing give higher heat transfer coefficient, factor of 0.25 will be used.

Baffle spacing, lB = 0.25 Ds = 0.775 m

As the tube length used for the catalyst packing is 5.65 m, the number of baffle to be installed can

be calculated as:

NB = Lt / lB = 9.5 ≈ 10 baffles (round of to nearest number)

Step 4: Cooling Requirement

Heat generated from the exothermic reaction will be removed constantly to prevent the buildup of

hot spot which further alter the reaction and cause catalyst deactivation. Water which has the

boiling point temperature of 100oC will be used to constantly remove heat to maintain the catalyst

packed tube temperature at 75 o

C. Generally, at least 10oC of temperature difference will be

implemented. But for ourcase, the coolant return temperature will be set at 50oC .

Shell Side

Water coolant supply temperature, 𝑇𝑠𝑢𝑝𝑝𝑙𝑦(℃) 30

Water coolant return temperature, 𝑇𝑟𝑒𝑡𝑢𝑟𝑛(℃) 50

Mean temperature, 𝑇𝑚𝑒𝑎𝑛(℃) *

40

Fluid properties at mean temperature, 𝑇𝑚𝑒𝑎𝑛(℃)

Density, 𝜌 (𝑘𝑔/𝑚3) 992.2

Viscosity (Pa.s) 0.000653

Thermal Conductivity (𝑊/𝑚℃) 0.6305

Specific Heat Capacity (J/kg℃) 4134.99

352

Prandtl Number, Pr *

4.2826

Tube Side

Catalyst bed temperature, 𝑇𝑊(℃) 75

Fluid properties at wall temperature, 𝑇𝑤(℃)

Density, 𝜌 (𝑘𝑔/𝑚3) 697.77

Viscosity (Pa.s) 0.00095

Thermal Conductivity (𝑊/𝑚℃) 0.0486

Specific Heat Capacity (J/kg℃) 1770.89

Prandtl Number, Pr * 2.8355

* 𝑀𝑒𝑎𝑛 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒, 𝑇𝑓 =𝑇𝑠𝑢𝑝𝑝𝑙𝑦+𝑇𝑟𝑒𝑡𝑢𝑟𝑛

2 ; 𝑃𝑟 =

𝐶𝑝𝜇

𝑘𝑓

a. Log Mean Temperature Difference, ∆𝑻𝑳𝑴𝑻𝑫

For counter current flow,

∆𝑇𝐿𝑀𝑇𝐷 =(𝑇1 − 𝑡2) − (𝑇2 − 𝑡1)

ln[(𝑇1 − 𝑡2) (𝑇2 − 𝑡1)⁄ ]

Where

𝑇1 = ℎ𝑜𝑡 𝑖𝑛𝑙𝑒𝑡 𝑓𝑙𝑢𝑖𝑑 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒

𝑇2 = ℎ𝑜𝑡 𝑜𝑢𝑡𝑙𝑒𝑡 𝑓𝑙𝑢𝑖𝑑 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒

𝑡1 = 𝑐𝑜𝑙𝑑 𝑖𝑛𝑙𝑒𝑡 𝑓𝑙𝑢𝑖𝑑 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒

𝑡2 = 𝑐𝑜𝑙𝑑 𝑜𝑢𝑡𝑙𝑒𝑡 𝑓𝑙𝑢𝑖𝑑 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒

∆𝑇𝐿𝑀𝑇𝐷 = 34.03℃

b. Overall Heat Transfer Coefficient

Amount of heat to be constantly removed from the reactor, Q = 180778.85 MJ/hr

𝑁𝑡= 1360 tubes

𝑑𝑜 = 0.0603 m

𝐿𝑡 = 7.32 m

Heat transfer area, A = Total outside tube area = 𝜋𝑑𝑜𝐿𝑡𝑁𝑡 = 1885.895 m2

Overall heat transfer coefficient, 𝑈𝑜 =𝑄

𝐴(∆𝑇𝐿𝑀𝑇𝐷) = 83.0736 W/m

2K

c. Mass Flow of Coolant

Amount of heat to be constantly removed from the reactor, Q = 180778.85 MJ/hr

Cp = 4134.99 J/kg℃

Water coolant supply temperature, 𝑇𝑠𝑢𝑝𝑝𝑙𝑦 = 30 ℃

Water coolant return temperature, 𝑇𝑟𝑒𝑡𝑢𝑟𝑛 = 50 ℃

353

Mass flow rate of water coolant,𝑚𝑠 =𝑄

𝐶𝑝(𝑇𝑟𝑒𝑡𝑢𝑟𝑛−𝑇𝑠𝑢𝑝𝑝𝑙𝑦) = 2.1860 kg/s

d. Tube Side Heat Transfer Coefficient, hi

In order to calculate the tube side heat transfer coefficient, the Nu has to be determined.

𝑁𝑢𝑠𝑠𝑒𝑙𝑡 𝑛𝑢𝑚𝑏𝑒𝑟, 𝑁𝑢 =ℎ𝑖𝑑𝑒

𝑘𝑓

Volumetric flow rate of the gases, �̇� = 65.7506 m3/h = 6.917 m

3/s

Cross sectional area of one tube, Ai = 0.00235514 m2

Total cross sectional area, AI = Ai x Nt = 3.2030 m2

Fluid velocity, ut = �̇�

𝐴𝐼 = 0.005702 m/s

Equivalent diameter, de = inner tube diameter, di = 0.0548 m

𝑅𝑒 =𝜌𝑢𝑡𝑑𝑒

𝜇 = 1228.67

Below a Reynolds number of about 2000 the flow in pipes will be laminar. Providing the natural

convection effects are small, which will normally be so in forced convection, the following

equation can be used to estimate the film heat-transfer coefficient:

𝜇𝑤 is the viscosity at wall temperature of 75oC; since the tube side fluid is evaluated at 75

oC , 𝜇

will equal to 𝜇𝑤.

The equation will then reduce to:

At operating temperature of 75oC, Pr = 2.8355

de = 0.05476 m

L = 7.32 m

Nu = 5.68

de = di = 0.0548 m

kf = 0.05951 𝑊/𝑚℃

ℎ𝑖 =𝑁𝑢 𝑘𝑓

𝑑𝑒 = 34.214 𝑊/𝑚2𝐾

e. Shell Side Heat Transfer Coefficient, ho

The area for cross flow, As for the row of tubes at the shell equator can be calculated as:

354

𝐴𝑠 =(𝑃𝑡 − 𝑑0)𝐷𝑠𝑙𝐵

𝑃𝑡

𝑑𝑜 = 0.0603 𝑚

𝑃𝑡 = 1.25𝑑𝑜 = 0.07375𝑚

Ds = 3.1 m

lB = 0.25 Ds = 0.7750 m

𝐴𝑠 =(𝑃𝑡−𝑑0)𝐷𝑠𝑙𝐵

𝑃𝑡 = 0.4805 m

2

Fluid mass flow rate at the shell side, �̇�𝑠=2.1860 kg/s

Density of fluid, 𝜌 = 992.2 𝑘𝑔/𝑚3

Fluid velocity, us = �̇�𝑠

𝜌𝐴𝑠 = 0.004585 m/s

Viscosity of fluid, 𝜇 =0.000653 Pa.s

The shell side hydraulic diameter, de of square pitch arrangement can be calculated as:

𝑑𝑒 =1.27

𝑑𝑜(𝑃𝑡

2 − 0.785𝑑𝑜2) = 0.0595 𝑚

𝑅𝑒 =𝜌𝑢𝑠𝑑𝑒

𝜇 = 1414.82

From the chart above, with baffle cut of 25% and Reynold number of 1752.64, heat transfer factor,

jh is 0.008.

𝑁𝑢 = 𝑗ℎ𝑅𝑒𝑃𝑟0.33(𝜇

𝜇𝑤)0.14 =

ℎ𝑜𝑑𝑒

𝑘𝑓

355

At wall temperature of 75℃, the viscosity of the water coolant is equal to 0.000653Pa.s.

𝑁𝑢 = 𝑗ℎ𝑅𝑒𝑃𝑟0.33(𝜇

𝜇𝑤)0.14 = 5.05

Thermal conductivity of shell side fluid, kf = 0.6305 𝑊/𝑚℃

ℎ𝑜 =𝑁𝑢 𝑘𝑓

𝑑𝑒 = 53.46 𝑊/𝑚2𝐾

f. Overall Heat Transfer Coefficient, Uo Verification

1

𝑈𝑜=

1

ℎ𝑜+

1

ℎ𝑜𝑑+

𝑑𝑜ln (𝑑𝑜

𝑑𝑖)

2𝑘𝑤+

𝑑𝑜

𝑑𝑖𝑥

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖𝑥

1

ℎ𝑖

hi = 32.2144 W/m2.K

ho = 53.46 W/m2.K

do = 0.0603 m

di = 0.05476 m

Since the tube material used is the stainless steel 316, the thermal conductivity is between 13-17

W/m K. An average value of 15 W/m K is used for calculation.

The average fouling factor of town water used in the shell side with a range of 1000- 2000 W/m2K

is taken 1500W/m2K while the reactant fluids (hydrocarbon) in the tube side is considered as

light hydrocarbons with fouling factor of 5000 W/m2K.

356

1

𝑈𝑜=

1

ℎ𝑜+

1

ℎ𝑜𝑑+

𝑑𝑜ln (𝑑𝑜𝑑𝑖

)

2𝑘𝑤+

𝑑𝑜

𝑑𝑖𝑥

1

ℎ𝑖𝑑+

𝑑𝑜

𝑑𝑖𝑥

1

ℎ𝑖 = 0.01449

Overall heat transfer coefficient, Uo = 68.6862 W/m2K

Let:

Uo calculated based on the equation: 𝑈𝑜 =𝑄

𝐴(∆𝑇𝐿𝑀𝑇𝐷) = Uo1

Uo calculated based on the equation:𝑈𝑜 =1

1

ℎ𝑜+

1

ℎ𝑜𝑑+

𝑑𝑜ln (𝑑𝑜𝑑𝑖

)

2𝑘𝑤+

𝑑𝑜𝑑𝑖

𝑥1

ℎ𝑖𝑑+

𝑑𝑜𝑑𝑖

𝑥1

ℎ𝑖

= Uo2

Deviation = |Uo1−Uo2|

Uo1 x 100% =

|83.0736 − 68.6862|

83.0736𝑥100% = 17.32%

Since the deviation less than 30%, all the computations above are correct. Normally, the overall

heat transfer coefficient in the packed catalyst bed reactor will in the range of 20-80 W/m2K.

Since the calculated Uo fall within this range, the effective heat removal can be done well.

Mechanical Design

Step 1: Design Pressure

Normally, safety margin of 10% above the operating pressure, Po will be applied for reactor

design.

Design pressure, 𝑃𝑑 = 110% of the operating pressure, 𝑃𝑜.

Operating pressure, 𝑃𝑜 = 1100 kPa = 1.1N/mm2

Design pressure, 𝑃𝑑 = 1.21 N/mm2

Step 2: Design Temperature

Design temperature, 𝑇𝑑 is taken to be 50℉ (10℃) above the operating temperature, 𝑇𝑜

Design temperature, 𝑇𝑑 = Operating temperature, 𝑇𝑜 + 10℃

Operating temperature, 𝑇𝑜 = 75℃

Design temperature, 𝑇𝑑 = 85℃

Step 3: Material of Construction

The material used for the reactor will be stainless steel 316 as water is present in the methanol

feedstock during MTBE production.

The tensile strength of the stainless steel 316 is 520 MPa, which is considerably high. In other

words, explosion due to high pressure in the reactor is impossible.

357

By interpolation, at design temperate of 75oC, the design stress, f of stainless steel 316 is 162.5

N/mm2.

Step 4: Welded joint efficiency

A double welded butt type of welding is used for this reactor to balance the trade off between

higher cost and higher strength of weld joint. The welded join efficiency, J of this weld joint is

0.85.

Step 5: Tube Wall Design

Minimum tube wall thickness can be computed as follow:

Minimum thickness, 𝑒𝑡 = 𝑃𝑑𝑑𝑖

2𝐽𝑓−𝑃𝑑

The pressure inside the tube will be the reaction pressure of 1100kPa.

Design pressure, 𝑃𝑑 = 1.21 N/mm2

Internal diameter of tube, di = 0.05476 m = 54.76 mm

Design stress, f = 162.5 N/mm2

Joint factor, J = 0.85

Minimum thickness, 𝑒𝑡 = 𝑃𝑑𝑑𝑖

2𝐽𝑓−𝑃𝑑= 0.2409 mm

For stainless steels, where severe corrosion is not expected, a minimum allowance of 2.0 mm

should be used, so:

Corrosion allowance = 2mm

Wall thickness, 𝑡 = 𝑒𝑡 + corrosion allowance = 2.2409 mm

Check for the minimum practical wall thickness:

358

Since the diameter of the tube is < 1 m, by extrapolation, we can conclude that the thickness

computed is greater than the minimum thickness needed.

Minimum wall thickness, t = 2.2409mm

The tube wall thickness will be taken as the nearest greater thickness of fabricated tube which is

equal to 2.1082 mm with the selection of NPS 2inch tube from Schedule ASME 10/10S.

Tube wall thickness, tt = 2.77 mm

With the tube wall thickness, tt selected, the maximum allowable working pressure (MAWP) for

the respective thickness will be computed. The MAWP is expected to be greater than the

operating pressure to allow it to be used under safety concern. The maximum allowable working

pressure (MAWP) for this wall thickness is given by:

MAWP =2×𝑇𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ×𝐽×𝑡𝑡

𝑑𝑖+ 𝑡𝑡

Tensile strength of the stainless steel = 520MPa

Tube wall thickness, 𝑡𝑡= 2.77 mm

Internal diameter of tube, di = 0.05476 m = 54.76 mm

Joint factor, J = 0.85

MAWP = =2×𝑇𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ×𝐽×𝑡𝑡

𝑑𝑖+ 𝑡𝑡 = 42.56 N/mm

2

Since the MAWP is greater than the operating pressure at 1.21 N/mm2, the thickness of tube is

acceptable

Step 6: Shell Wall Design

Minimum wall thickness of shell will be computed as follow:

Minimum thickness, 𝑒𝑠 = 𝑃𝑑Ds

2𝐽𝑓−𝑃𝑑

The pressure inside the shell will be at the pressure of 101.325 kPa (0.101325N/mm2).

Design pressure, 𝑃𝑑 = 0.1114575 N/mm2

Internal diameter of shell, Ds = 1.5 m = 1508.15 mm

Design stress, f = 162.5 N/mm2

Joint factor, J =0.85

Minimum thickness, 𝑒𝑡 = 𝑃𝑑Ds

2𝐽𝑓−𝑃𝑑 = 1.2512 mm

Corrosion allowance = 2mm

Wall thickness, 𝑡 = 𝑒𝑡 + corrosion allowance = 3.2512 mm

359

Check for the minimum practical wall thickness:

Check for the minimum thickness; since the diameter of the tube is 3.1 m, the thickness computed

is smaller than the minimum thickness. Thus, new wall thickness will be selected.

Minimum wall thickness, 𝑡 = 12 mm

The shell wall thickness will be taken based on the pipe diameter (must be greater than 3.1m) and

the pipe thickness (consider the stress that need to be withstand by the load inside the shell) of

fabricated metal sheet thickness which is equal to 1.0 in (=25.40 mm).

Shell wall thickness, 𝑡𝑠= 25.40 mm

With the shell wall thickness, ts, selected, the maximum allowable working pressure (MAWP) for

the respective thickness will be computed. The MAWP is expected to be greater than the

operating pressure to allow it to be used under safety concern.The maximum allowable working

pressure (MAWP) for this wall thickness is given by:

MAWP =2×𝑇𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ×𝐽×𝑡𝑠

𝐷𝑠+ 𝑡𝑠

Tensile strength of the stainless steel 316 = 520MPa

Shell wall thickness, 𝑡𝑠= 25.4 mm

Internal diameter of shell, Ds = 3.6068 m = 3606.8 mm

Joint factor, J = 0.85

MAWP = 6.1818 N/mm2

Since the MAWP is greater than the operating pressure at 0.101 N/mm2, the thickness of tube is

acceptable.

Step 7: Reactor Vessel Head Design

Ellipsoidal head (major and minor axis ratio of 2:1) will be used as it is able to withstand the

pressure above 15 bar (=1500kPa). As the domed head selected is the formed head with no joints

in the head, the joint factor is taken as 1.0. made with a short straight cylindrical section called a

360

flange or skirt. The formed head ensures the weld line is away from the point of the discontinuity

between the head and the cylindrical section of the vessel.

Minimum head wall thickness, 𝑒ℎ = 𝑃𝑑𝐷ℎ

2𝐽𝑓−0.2𝑃𝑑

The pressure inside the shell will be at the pressure of 101.325kPa = 0.101325 N/mm2.

Design pressure, 𝑃𝑑 = 0.111458 N/mm2

Internal diameter of head, Dh = Internal diameter of shell, Ds = 3.6068 m = 3606.8 mm

Design stress, f = 162.5 N/mm2

Joint factor, J = 0.85

Minimum head wall thickness, 𝑒ℎ = 𝑃𝑑𝐷ℎ

2𝐽𝑓−0.2𝑃𝑑 = 1.4553 mm

Corrosion allowance = 2mm

Wall thickness, 𝑡 = 𝑒𝑡 + corrosion allowance = 3.4553 mm

Same as the shell wall thickness, the fabricated metal sheet thickness for vessel head is equal to

1.0 in. = 25.40mm.

Head wall thickness, th = 25.40mm

With the head wall thickness, th, selected, the maximum allowable working pressure (MAWP) for

the respective thickness will be computed. The MAWP is expected to be greater than the

operating pressure to allow it to be used under safety concern. The maximum allowable working

pressure (MAWP) for this wall thickness is given by:

Tensile strength of the stainless steel 316 pipe chosen = 520 MPa

Head wall thickness, th = 25.40 mm

Internal diameter of shell, Dsi = Ds = 3.6068 m = 3606.8 mm

Joint factor, J = 0.85

MAWP = 6.1818 N/mm2

Since the MAWP is greater than the operating pressure at 0.101 N/mm2, the thickness of tube is

acceptable.

Step 8: L/D Ratio of Reactor

a. Length of Reactor

Normally in the catalytic reactor, a catalyst support grid will be needed to retain costly catalyst.

The perforation hole or mesh size are selected taking into account the catalyst particle size.

Typical grid height is 100 to 150mm.

361

The shape of the ellipsoidal head is defined by the ratio of the major and minor axis. A standard

arrangement on vessels is the 2:1 elliptical head (see figure below). This will have a depth of

head which is a quarter of the vessel’s internal diameter, D.

Ltube = 7.32m

Lsupport = 0.15m

Lhead = 0.9017m

Total height of the reactor, L = Ltube +Lsupport + Lhead = 8.3177 m

b. Diameter of Reactor

Reactor shell outer diameter, D = Reactor shell inner diameter, Ds + 2 x shell thickness, ts

Internal diameter of shell, Ds = 3.6068 m = 3606.8 mm

Shell wall thickness, 𝑡𝑠= 25.4 mm

Reactor shell outer diameter, D = Ds + 2ts = 3.6576 m

𝐿

𝐷 = 2.29 (>0.5, satisfactory)

The L/D ratio of the reactor is within the range of general vessel L/D ratio of 2.5 to 5. Hence, the

reactor sizing is appropriately done with acceptable L/D ratio.

Step 9: Weight of Vessel

The total weight of the vessel consists of the reactor shell weight, reactor tubes weight and weight

of catalyst. Each weight is calculated separately and totalled up to get the total weight of vessel

which is required for stress analysis of the reactor. Since both the tubes and shell are in cylindrical

shape and made of stainless steel 316, the weight is calculated based on formula in Coulson and

Richardson’s Chemical Engineering Design:

a. Weight of Tubes

From tube specification table,

Weight per unit length of stainless steel 316 pipe = 3.93 kg/m

Ltube = 7.32m

Ntube = 1360 tubes

Weight of tube, Wt = 3.93 kg/m × Ltube x Ntube = 39123.94 kg = 383805.81 N

b. Weight of Shell

Weight of shell, Ws = Cv 𝜋 𝜌m Dm g (Hv+ 0.8Dm) ts

362

Cv = 1.15; as a factor to account for the weight of nozzle, manway and internal support.

Density of the vessel material (Stainless Steel 316), 𝜌m = 7850 kg/m3

Internal diameter of shell, Ds = 3.6068 m

Shell wall thickness, 𝑡𝑠= 25.40 mm = 0.0254 m

Mean diameter of vessel, Dm = Ds + 2ts = 3.6576 m

Gravitational acceleration, g = 9.81m/s2

Height of vessel, Hv = Length of vessel, L = 8.3717 m

Weight of shell, Ws = Cv 𝜋 𝜌m Dm g (Hv+0.8Dm) ts = 292017.86 N

c. Weight of Catalyst

The weight of catalyst is chosen based on the result provided by polymath. The weight is chosen

when the desired product (MTBE) molar flow rate in the outlet stream is same on both polymath

generated table and excel spreadsheet.

Weight of catalyst,Wc = 18050 kg = 177070.5 N

Total weight of reactor vessel, Wv = Wt + Ws + Wc = 852894.2 N

Step 10: Stress Analysis

Stress analysis must be done to ensure that the reactor structure is strong and safe.

a. Wind loads

The consideration of wind loads is important on tall columns installed in the open area. It is

normally considered in design of columns and chimney-stacks which are usually free standing,

mounted on skirt supports and not attached to structural steel work.

Wind speed, uw = 160 km/h

Wind pressure, Pw = 0.05uw2 = 1280 N/m2

0.4m of allowance should be added for a caged ladder to obtain the effective column diameter.

Vessel diameter, D = 3.6576 m

Effective column diameter, Deff = Vessel diameter, D + 0.4m = 4.0576 m

Loading per unit length of column, Fw = PwDeff = 5193.73 N/m

Height of vessel, Hv = Length of vessel, L = 8.3717m

Bending moment, Mx(Nm) =FwHv

2

2 = 182002.15 Nm

b. Stresses Analysis

Design pressure, 𝑃𝑑 = 1.21 N/mm2

Internal diameter of shell, Ds = 3.6068 m = 3606.80 mm

Shell wall thickness, 𝑡𝑠 = 0.0254 m= 25.40 mm

Reactor shell outer diameter, D = 3.6576 m = 3676.6 mm

Longitudinal, 𝜎𝐿 =𝑃𝑑𝐷𝑠

4𝑡𝑠 = 42.955 N/mm

2

363

Circumferential, 𝜎ℎ =𝑃𝑑𝐷𝑠

2𝑡𝑠 = 85.91 N/mm

2

Direct (due to weight), 𝜎𝑊 =𝑊𝑣

𝜋(𝐷𝑠+𝑡𝑠)𝑡𝑠 = 2.7719 N/mm

2

𝐼𝑣 =𝜋

64(𝐷4 − 𝐷𝑠

4) = 477995823522.17 mm4

Bending, 𝜎𝑏 = ±𝑀𝑥

𝐼𝑣(𝐷𝑠

2+ 𝑡𝑠) = ± 0.6963 N/mm

2

𝜎𝑧 = 𝜎𝐿+𝜎𝑤 ± 𝜎𝑏

Since dead weight stress is compressible, it is negative.

𝜎𝑧 = 𝜎𝐿−𝜎𝑤 ± 𝜎𝑏

Upwind: 𝜎𝑧 = 𝜎𝐿−𝜎𝑤 + 𝜎𝑏 = 40.8794 N/mm2

Downwind: 𝜎𝑧 = 𝜎𝐿−𝜎𝑤 − 𝜎𝑏= 39.4867 N/mm2

𝜎1 =1

2[𝜎ℎ + 𝜎𝑧 + √(𝜎ℎ − 𝜎𝑧)2 + 4𝜏2

𝜎2 =1

2[𝜎ℎ + 𝜎𝑧 − √(𝜎ℎ − 𝜎𝑧)2 + 4𝜏2

Since torsional shear stress, 𝜏 is not significant to be considered in preliminary design,

𝜎1 = 𝜎ℎ

𝜎2 = 𝜎𝑧

𝜎3 = 0.5𝑃𝑑

From the table, the greatest principle

stress difference is 85.3050 N/mm2.

This does not exceed the design stress for the material construction of this reactor at 130 N/mm2.

Hence, the design is acceptable.

Critical buckling stress, 𝜎𝑐 = 2 × 104 (𝑡𝑠

𝐷) = 138.89 𝑁/𝑚𝑚2

Maximum compressive where the vessel is not under pressure = 𝜎𝑤 + 𝜎𝑏 = 3.6390𝑁/𝑚𝑚2

The maximum compressive stress well below the critical buckling stress and maximum allowable

design stress. Hence, the design is satisfactory.

Step 11: Vessel Support

Principle Stress

(N mm-2

) Upwind Downwind

𝜎1 − 𝜎2 45.0306 46.4233

𝜎1 − 𝜎3 85.3050 85.3050

𝜎2 − 𝜎3 40.2744 38.8817

364

Type of support chosen: Conical Skirt

Approximate skirt bottom diameter, Dskirt = Ds+ 0.1 = 3.7068 m

Approximate skirt height, Hskirt = 3.0 m

𝑡𝑎𝑛 𝜃𝑠𝑘𝑖𝑟𝑡 =𝐻𝑠𝑘𝑖𝑟𝑡

12

(𝐷𝑠𝑘𝑖𝑟𝑡 − 𝐼𝐷𝑠)= 9.8879

The skirt base angle,𝜃𝑠 = 89.05° is acceptable which is within common range of 80° 𝑡𝑜 90°

Total height of the reactor, L = 8.2717m

Loading per unit length of column, Fw = 5193.73 N/m

Bending moment at bottom of skirt, 𝑀𝑠 =𝐹𝑤(𝐿+𝐻𝑠𝑘𝑖𝑟𝑡)

2

2= 335814.92 𝑁 𝑚

Take skirt thickness, tskirt = ts = 0.00254m

Bending stress in skirt, 𝜎𝑏𝑠 =4𝑀𝑠

𝜋(𝐷𝑠𝑘𝑖𝑟𝑡+𝑡𝑠𝑘𝑖𝑟𝑡)𝐷𝑠𝑘𝑖𝑟𝑡𝑡𝑠𝑘𝑖𝑟𝑡= 12.168 𝑁 𝑚𝑚−2

The maximum dead weight load on the skirt will occur when the vessel space is full of water.

Volume of shell, Vs = 𝜋𝐷𝑠

2

4𝑥 𝐿 = 55.25 m

3

Volume of tube, Vt = 𝜋𝑑𝑜

2

4𝑥 𝐿 𝑥 𝑁𝑡 = 28.42 m

3

Volume of water, Vwater = Volume of shell, Vs – Volume of tube, Vtube = 25.824 m3

Approximate water weight, 𝑊𝑤𝑎𝑡𝑒𝑟 = 𝑉𝑤𝑎𝑡𝑒𝑟 × 𝜌𝑤𝑎𝑡𝑒𝑟 × 𝑔 = 261094.81N

Total weight of reactor vessel, Wv = Wt + Ws + Wc = 852894.2 N

Total Weight of reactor including coolant and reactant, WTOTAL = Wt + Ws + Wc + Wwater +

Wreactants = 1130348.8 N

Dead weight stress in the skirt,

𝜎𝑤𝑠(𝑡𝑒𝑠𝑡) =𝑊𝑤𝑎𝑡𝑒𝑟+ 𝑊𝑣

𝜋(𝐷𝑠𝑘𝑖𝑟𝑡+𝑡𝑠𝑘𝑖𝑟𝑡)𝑡𝑠𝑘𝑖𝑟𝑡=3.74 𝑁/ 𝑚𝑚2

𝜎𝑤𝑠(𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔) =𝑊𝑣

𝜋(𝐷𝑠𝑘𝑖𝑟𝑡+𝑡𝑠𝑘𝑖𝑟𝑡)𝑡𝑠𝑘𝑖𝑟𝑡= 2.86 𝑁/ 𝑚𝑚2

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) = 𝜎𝑏𝑠−𝜎𝑤𝑠

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) = 𝜎𝑏𝑠+𝜎𝑤𝑠

Maximum σ̂s(compressive) = 12.1678 − 2.8638 =15.9083 N/ mm2

365

Maximum σ̂s(tensile) = 12.1678 − 3.7405 = 8.4273 N/ mm2

The skirt thickness should be such that under the worst combination of wind and dead weight

loading, 2 design criteria must be satisfied:

𝜎𝑠(𝑡𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑓𝑠𝐽 sin 𝜃𝑠

𝜎𝑠(𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸 (𝑡𝑠𝐷𝑠

) 𝑠𝑖𝑛𝜃𝑠

The skirt material is choosen to be stainless steel with maximum allowable design stress ( at

30 °C ) of 135 N/mm2. The Young modulus of stainless steel is 203395.3 MPa.

fs = 135 N/mm2

J = 0.85

𝜃𝑠 = 89.05° E=203395.3 MPa

tskirt = 0.00792m

Dskirt = 1.60815 m

𝑓𝑠𝐽 sin 𝜃𝑠 = 114.7342 N/mm2

Maximum σ̂s(tensile)(8,4273 N/ mm2) < 𝑓𝑠𝐽 sin 𝜃𝑠 [Satisfy]

0.125𝐸 (𝑡𝑠𝑘𝑖𝑟𝑡

𝐷𝑠𝑘𝑖𝑟𝑡) 𝑠𝑖𝑛𝜃𝑠 = 174.1911 N/mm

2

Maximum σ̂s(compressive)(15.9083 N/ mm2) < 0.125𝐸 (𝑡𝑠

𝐷𝑠) 𝑠𝑖𝑛𝜃𝑠 [Satisfy]

Since both design criteria are satisfied, the skirt thickness is acceptable.

Take corrosion allowance of 2 mm, skirt thickness = 25.4 + 2 =27.40 mm

Step 12: Base ring and anchor bolt design

Area of bolt, Ab =1

Nbfb[4Ms

Db− W]

𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑎𝑙𝑙𝑜𝑤𝑎𝑏𝑙𝑒 𝑏𝑜𝑙𝑡 𝑠𝑡𝑟𝑒𝑠𝑠, 𝑓𝑏 = 125𝑁

𝑚𝑚2

𝐵𝑒𝑛𝑑𝑖𝑛𝑔 𝑚𝑜𝑚𝑒𝑛𝑡 𝑎𝑡 𝑡ℎ𝑒 𝑏𝑎𝑠𝑒,𝑀𝑠 = 335814.92 𝑁𝑚

Weight of the vessel, W= 852894.2 N

Approximate bolt pitch circle diameter, Db = 3.4 m

Circumference of bolt circle = 3350.8 × π = 10526.85 mm

Minimum bolt spacing is recommended at 600 mm.

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑏𝑜𝑙𝑡𝑠, 𝑁𝑏 =10536.85

600= 17.54 ≈ 16 𝑏𝑜𝑙𝑡𝑠 (Must be multiple of 4)

Area of bolt, Ab = 1

𝑁𝑏𝑓𝑏[4𝑀𝑠

𝐷𝑏− 𝑊] = 226.01 𝑚𝑚2

Diameter of bolt = √𝐴𝑏×4

𝜋= 16.96 𝑚𝑚

The bolt type selected is M20 as it is the closest standard size bolt larger than 16.96 mm. Its root

area is 234.77 mm2.

366

Total compressive load on base ring, 𝐹𝑏 =4𝑀𝑠

𝜋𝐷𝑠𝑘𝑖𝑟𝑡2 +

𝑊

𝜋𝐷𝑠𝑘𝑖𝑟𝑡= 104357.6356𝑁/𝑚

Maximum allowable bearing pressure on concrete foundation pad, fc =7 N mm-2

.

Minimum base ring width, 𝐿𝑏 =𝐹𝑏

𝑓𝑐×

1

1000= 14.91 𝑚𝑚

Using bolt M30 Distance from skirt edge to ring edge, Lr = 53mm.

Actual base ring width = Lr + ts + 50 = 53 + 25.40 + 50 = 128.4 mm

Actual bearing pressure on base, fc′ =

𝐹𝑏

Actual base ring width x 1000= 0.8128

Allowable design stress in the ring material, fr = 140N/mm2

Minimum base ring thickness, tb = Lr√3fc

fr = 6.99 ≈ 7 mm

Step 13: Nozzle Design

a. Water Coolant Inlet

Since the viscosity of the inlet water coolant is low, the nozzle sizing will based on the following

equation

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒, �̇�𝑉 = 0.0022 𝑚3/𝑠

𝑑𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌 = 992.2 𝑘𝑔/𝑚3

𝐷𝑖,𝑜𝑝𝑡 = 0.363�̇�𝑉0.45𝜌0.13 = 0.05673 m = 56.73 mm

367

The stainless steel 316 pipe 2.5 in Sch 80S has the characteristics of:

Pipe outer diameter, OD = 73mm

Pipe thickness = 7.01mm

Pipe inner diameter, ID = 58.98mm

This pipe type can be used as the nozzle of the water coolant inlet.

b. Water Coolant Inlet

Since the viscosity of the outlet coolant is still low, the nozzle sizing will based on same equation

as above:

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒, �̇�𝑉 = 0.0022 𝑚3/𝑠

𝑑𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌 = 992.2 𝑘𝑔/𝑚3

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13 = 0.057 m = 56.73 mm

368

The stainless steel 2.5 in Sch 80S has the characteristics of:

Pipe outer diameter, OD = 73mm

Pipe thickness = 7.01 mm

Pipe inner diameter, ID = 58.98mm

This pipe type can be used as the nozzle of the water coolant outlet.

c. Process Fluid Inlet

For process fluid inlet, the same formula that used in coolant nozzle calculation can be used as the

density of the process inlet fluid is 0.952mPa (almost same as water).

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒, �̇�𝑉 = 0.0183 𝑚3/𝑠

𝑑𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌 = 697.77 𝑘𝑔/𝑚3

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13 = 0.1404 m = 140.38 mm

369

Diamater of nozzle inlet, D (m) = 146.34 mm

The 6 in Sch 80S pipe with inlet diameter of 146.34mm can well accommodate the inlet nozzle

size.

d. Process Fluid Outlet

For process fluid outlet, the same formula that used in coolant nozzle calculation can be used as

the density of the process outlet fluid is 1.035mPa (almost same as water).

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13

𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒, �̇�𝑉 = 0.0183 𝑚3/𝑠

𝑑𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌 = 736.89 𝑘𝑔/𝑚3

𝐷𝑖,𝑜𝑝𝑡 = 0.363 �̇�𝑉0.45𝜌0.13 = 0.1404 m = 173.64 mm

370

Diamater of nozzle outlet, D (m) = 193.70 mm

The 8 in Sch 80S pipe with inlet diameter of 193.70 mm can well accommodate the inlet nozzle

size.

371

Auxiliary Equipment Design FEED PUMP, P-101

P-101

4

3

Step 1: Design Calculation

Parameters (Inlet & Outlet)

Molar flow rate (kmol/hr) 993.47

Mass flow rate (ton/hr) 430.1139

Volumetric flow rate (𝑚3/hr) 45.2077

Design criteria

Inlet temperature (K) 301.15

Inlet Pressure (bar) 8.15

Outlet Pressure (bar) 11.5

Length of suction side, 𝐿1(m) 3.00

Length of discharge side, 𝐿2 (m) 10.00

Total length of pipe, L (m) 13.00

Inlet elevation, 𝑍1 (m) 5.00

Outlet elevation, 𝑍2 (m) 10.00

Density (kg/𝑚3) 951.4164

Viscosity (Ns/𝑚2) 0.0000735

Volumetric flow rate, ѵ(𝑚3/s)

𝑣 =�̇�

𝜌

𝑣 =43011.39𝑘𝑔/ℎ𝑟

951.4164 𝑘𝑔/𝑚3 𝑥

1 ℎ𝑟

60 𝑚𝑖𝑛 𝑥

1 𝑚𝑖𝑛

60 𝑠

𝑣 = 0.0126𝑚3

𝑠

Step 2: Nozzles design

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

= 8.4143011.390.45

951.41640.31

𝐷𝑜𝑝𝑡 = 122.0713 𝑚𝑚 = 4.80596 𝑖𝑛

Based on Table 38.the pipe size to be chosen is 5 in nominal size.

From Table 38. Internal diameter, ID is = 5.047 in = 0.1282 m

𝐴𝑟𝑒𝑎 = π𝐷2

4

372

𝐴𝑟𝑒𝑎 = π x 0.12822

4

𝐴𝑟𝑒𝑎 = 0.0129 𝑚2

Table 38 – Schedule 40 Pipe Dimensions

Step 3: Velocity of liquid

𝑄 = 𝐴𝑣 → 𝑣 =𝑄

𝐴

𝑣 =0.0126𝑚3/𝑠

0.0129𝑚2

𝑣 = 0.9767𝑚

𝑠

Step 4: Friction in pipe

Relative roughness:

373

From the table above, ɛ for stainless steel = 0.015 mm

ɛ

𝐷=

0.015 𝑚𝑚

128.2 𝑚𝑚= 0.000117

Reynolds Number:

𝑅𝑒 =𝜌𝑣𝐷

µ

𝑅𝑒 =(951.4164 kg/𝑚3) 𝑥 (0.972844

𝑚𝑠 ) 𝑥 (0.1282 𝑚)

(0.0000735 Ns/𝑚2)

𝑅𝑒 = 1614412.547

374

The Moody Diagram

From The Moody Diagram:

𝐹𝑟𝑖𝑐𝑡𝑖𝑜𝑛 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑓 =0.015

Assume Length of pipe = 13 m,

ℎ𝑓 =8𝑓

𝐷 𝐿 𝑣2

2𝑔

ℎ𝑓 =8 𝑥 0.015

0.1282 𝑚 13 𝑥 (0.972844 𝑚/𝑠)2

2 𝑥 9.81 𝑚/𝑠

𝐹𝑟𝑖𝑐𝑡𝑖𝑜𝑛 𝑙𝑜𝑠𝑠 𝑖𝑛 𝑝𝑖𝑝𝑒, ℎ𝑓 = 0.58698 𝑚

Step 5: Total head, 𝒉𝒑

ℎ𝑝 =(𝑃2 − 𝑃1)

𝜌𝑔+ (𝑍2 − 𝑍1) + ℎ𝑓

ℎ𝑝 =(1150000 − 815000)𝑃𝑎

951.4164kg𝑚3 𝑥 9.81 𝑚/𝑠

+ (10 − 5)𝑚 + 0.58698 𝑚

ℎ𝑝 = 41.4796 𝑚 = 136.0879 𝑓𝑡

375

Step 6: Power required

𝑃𝑜𝑤𝑒𝑟 = 𝑚𝑔ℎ𝑝

𝑃𝑜𝑤𝑒𝑟 = (43011.39 𝑘𝑔/ℎ𝑟)𝑥 9.81𝑚

𝑠𝑥 41.4796𝑚

𝑃𝑜𝑤𝑒𝑟 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 = 17501975 𝑊 = 175019.8 𝑘𝑊

Step 7: NPSH

𝑁𝑃𝑆𝐻𝐴 =(𝑃1 − 𝑃𝑣)

𝜌𝑔+ (𝑍1 − ℎ𝑓1)

𝑁𝑃𝑆𝐻𝐴 =(815000 − 100000)𝑃𝑎

951.4164kg𝑚3 𝑥 9.81 𝑚/𝑠

+ (5 − 0.58698 )𝑚

𝑁𝑃𝑆𝐻𝐴 = 81.0197 𝑚

Volumetric flow rate = 45.2077𝑚3

ℎ= 199.0436

𝑔𝑎𝑙

𝑚𝑖𝑛

Graph Pump efficiency

From graph pump efficiency:

𝑁𝑃𝑆𝐻𝑅 = 150 𝑚 = 492.126 𝑓𝑡

Therefore, NPSHA> NPSHR. The pump is applicable.

Step 8: Actual motor power

376

From graph pump efficiency:

Efficiency, ƞ = 0.63

Thus the actual power motor of the pump is:

𝐴𝑐𝑡𝑢𝑎𝑙 𝑃𝑜𝑤𝑒𝑟 =𝑃𝑜𝑤𝑒𝑟 𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑

𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦

=17501975𝑊

0.63= 27780912.7𝑊 = 27780.91𝑘𝑊 = 37254.76 ℎ𝑝

Step 9: Type of pump

Normal operating range of pumps Total Head versus Flow Rate

Type of pump chosen = Centrifugal

Speed of pump = Single-stage

(Coulson & Richardson’s Chemical Engineering)

377

REFLUX PUMP (P-102)

DESIGN BASIS:

INLET and OUTLET

Molar Flow Rate (kmol/hr) 704.56

Mass Flow Rate (kg/hr) 22624.52

Volumetric Flow Rate (m3/hr) 33.42

DESIGN PARAMETERS:

Pump

Nozzle size

Total Head

NPSH

Motor Power

DESIGN CRITERIA:

Inlet Temperature 62 OC=335.15K

Pressure 750 kPa to 770 kPa

Length of suction side, L1(m) 5.00

Length of discharge side, L2(m) 5.00

Total length of pipe,L(m) 10.00

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

Density (kg/m3) 677.01

Pv(Pa) 100000

Viscosity (Pa.s) 0.00024

378

Step 1: Nozzles design:

Liquid Inlet and Outlet

The Harker equation (1978), modified for SI unit, for the optimum pipe (and nozzle) diameter:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Dopt = 8.41 ×22624.520.45

677.010.31= 101.59 mm = 3.999 in ≈ 4 in

Where: W in kg/hr and in kg/m3

W = Mass Flow Rate = 22624.52 kg/hr

ρ = 677.01 kg/m3

Based on Schedule 40 pipe dimension, the pipe size to be chosen is 4 in nominal size.

For nominal size of 4 in, internal diameter is 4.026 in or 0.1023 m

Therefore, area of pipeline (based on internal diameter):

A =πD2

4=

π × 0.10232

4= 0.008214m2

Step 2: Velocity of Liquid

Based on area of the pipeline, the velocity of the liquid flow:

Fluid volumetric flow rate =mass flow

density=

22624.52kghr

677.01kgm3

=33.42m3

hr×

1hr

3600s

379

Q = 0.00928m3/s

Q = Av

Rearrange, v =Q

A=

0.00928m3/s

0.008214m2=1.1301 m/s

Step 3: Friction in pipe

In calculating the friction in pipe, the whole length of the pipe is taken into account which is the

summation of length in suction side and discharge side. Friction in pipe is determined based on

the following equation:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔

In determining the value of friction factor, f, the value is taken based on Moody diagram as in

below with known Reynolds number, Re and relative roughness, 𝜀/D;

Reynolds Number is determined based on the following equation:

𝑅𝑒 =𝜌𝑣𝐷

𝜇= 237808.5874

Taking the type of the pipe used as commercial steel pipe, the roughness, ε is 0.046 mm. Thus the

relative roughness is:

𝜀

𝐷= 0.0004498

Therefore based on the Moody diagram, the friction factor is 0.0037.Thus the friction loss in pipe

is:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔 = 0.18842m

380

Step 4: Total Head

The velocity flow in both suction and discharge side is the same. Thus through the

rearrangement of Bernoulli’s Equation, the total head is:

ℎ𝑝 = (𝑃2−𝑃1

𝜌𝑔) + (𝑧2 − 𝑧1) + ℎ𝑓 = 6.79980𝑚 = 14.04865𝑓𝑡

Step 5: Power Required

Power required by the pump is based on the following equation:

𝑃𝑜𝑤𝑒𝑟 = �̇�𝑔ℎ𝑝 = 1509192.68𝑊

Step 6: NPSHA

NPSHA only involves the suction side. Thus the length of pipe involved is only the suction side.

NPSHA is calculated with the following equation:

𝑁𝑃𝑆𝐻𝐴 =𝑃1−𝑃𝑣

𝜌𝑔+ 𝑧1 − ℎ𝑓1

Friction loss is calculated only on the suction side

ℎ𝑓 =8𝑓𝐿1

𝐷

𝑣2

2𝑔= 0.09421𝑚

Thus, NPSHA = 100.9757m

For a pump to operate without cavitation, NPSHA > NPSHR. This requirement is checked for the

suitability of the pump. NPSHR is determined by using the following graph.

From the graph, volumetric flow rate of 33.42 m3/hr or equivalent to 147.14 gal/min gives

NPSHR of 25.0 ft or 7.62 m. Therefore, NPSHA> NPSHR. The pump is applicable.

Step 6: Actual motor power

381

The efficiency of the motor is determined in the graph above. From the graph, volumetric flow

rate of 33.42 m3/hr or equivalent to 147.14 gal/min and total head of 6.7998 m or equivalent to

14.0487 ft gives the efficiency of 0.50. Thus the actual power motor of the pump is:

Actual power:3018.385W

In terms of horsepower= 4047.65 hp

Step 7: Type of pump

(A) Normal operating range of pumps (to find the type of pump suitable), (B) Total Head versus

Flow Rate (to find the speed of pump)

Type of pump chosen = Diaphragm Speed of pump = 3500 rpm (Coulson & Richardson’s Chemical Engineering)

REFLUX PUMP (P-103)

DESIGN BASIS:

INLET and OUTLET

Molar Flow Rate (kmol/hr) 719.95

Mass Flow Rate (kg/hr) 3350.15

Volumetric Flow Rate (m3/hr) 28.38

382

DESIGN PARAMETERS:

Pump

Nozzle size

Total Head

NPSH

Motor Power

DESIGN CRITERIA:

Inlet Temperature 33 OC=306.1K

Pressure 100 kPa to 120 kPa

Length of suction side, L1(m) 5.00

Length of discharge side, L2(m) 5.00

Total length of pipe,L(m) 10.00

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

Density (kg/m3) 803.12

Pv(Pa) 100000

Viscosity (Pa.s) 0.00045

Step 1: Nozzles design:

Liquid Inlet and Outlet

The Harker equation (1978), modified for SI unit, for the optimum pipe (and nozzle) diameter:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Dopt = 8.41 ×20576.9740.45

803.120.31= 92.33mm = 3.63in = 4.0 in

Where: W in kg/hr and in kg/m3

W = Mass Flow Rate = 20576.974 kg/hr

ρ = 803.12 kg/m3

383

Based on Schedule 40 pipe dimension, the pipe size to be chosen is 4 in nominal size.

For nominal size of 4 in, internal diameter is 4.026 in or 0.1022 m

Therefore, area of pipeline (based on internal diameter):

A =πD2

4=

π×0.10222

4=0.1023 m2

Step 2: Velocity of Liquid

Based on area of the pipeline, the velocity of the liquid flow:

Fluid volumetric flow rate =mass flow

density=

20576.974kghr

803.12kgm3

=25.62m3

hr×

1hr

3600s

Q = 0.00712m3/s

Q = Av

Rearrange, v =Q

A=

0.00712m3/s

0.0082 𝑚2=0.866 m/s

Step 3: Friction in pipe

In calculating the friction in pipe, the whole length of the pipe is taken into account which is the

summation of length in suction side and discharge side. Friction in pipe is determined based on

the following equation:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔

384

In determining the value of friction factor, f, the value is taken based on Moody diagram as in

below with known Reynolds number, Re and relative roughness, 𝜀/D;

Reynolds Number is determined based on the following equation;

𝑅𝑒 =𝜌𝑣𝐷

𝜇= 216286.63

Taking the type of the pipe used as commercial steel pipe, the roughness, ε is 0.046 mm. Thus, the

relative roughness is: 𝜀

𝐷 =0.00045

Therefore, based on the Moody diagram, the friction factor is 0.02. Thus, the friction loss in pipe

is:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔

= 0.1048m

Step 4: Total Head

The velocity flow in both suction and discharge side is the same. Thus through the

rearrangement of Bernoulli’s Equation, the total head is:

ℎ𝑝 = (𝑃2−𝑃1

𝜌𝑔) + (𝑧2 − 𝑧1) + ℎ𝑓 = 6.2433𝑚 = 14.049 𝑓𝑡

Step 5: Power Required

Power required by the pump is based on the following equation:

385

𝑃𝑜𝑤𝑒𝑟 = �̇�𝑔ℎ𝑝 = 1260274.01 𝑊

Step 6: NPSHA

NPSHA only involves the suction side. Thus the length of pipe involved is only the suction side.

NPSHA is calculated with the following equation:

𝑁𝑃𝑆𝐻𝐴 =𝑃1−𝑃𝑣

𝜌𝑔+ 𝑧1 − ℎ𝑓1

Friction loss is calculated only on the suction side

ℎ𝑓 =8𝑓𝐿1

𝐷

𝑣2

2𝑔= 0.05238𝑚

Thus, NPSHA = 3.1476m

For a pump to operate without cavitation, NPSHA > NPSHR. This requirement is checked for the

suitability of the pump. NPSHR is determined by using the following graph.

From the

graph,

volumetric

flow rate of 25.62

m3/hr or

equivalent to

112.81 gal/min gives NPSHR of 25 ft or 7.62 m . Therefore, NPSHA> NPSHR. The pump is t

applicable.

Step 6: Actual motor power

The efficiency of the motor is determined in the graph above. From the graph, volumetric flow

rate of 25.62 m3/hr or 0.00712 m3/s or equivalent to 112.81 gal/min gives and total head of

6.24m or equivalent to 14.05 ft gives the efficiency of 0.55. Thus the actual power motor of the

pump is:

Actual power: 2520548.013kW

In terms of horsepower= 3380.05 hp

386

Step 7: Type of pump

(A) Normal operating range of pumps (to find the type of pump suitable), (B) Total Head

versus Flow Rate (to find the speed of pump)

Type of pump chosen = Diaphragm

Speed of pump = 3500 rpm (Coulson & Richardson’s Chemical Engineering)

DISTILLATE PUMP (P-104)

DESIGN BASIS:

INLET and OUTLET

Molar Flow Rate (kmol/hr) 643.55

Mass Flow Rate (kg/hr) 20576.974

Volumetric Flow Rate (m3/hr) 25.62

DESIGN PARAMETERS:

Pump

Nozzle size

Total Head

NPSH

Motor Power

387

DESIGN CRITERIA:

Inlet Temperature 33OC=306.15K

Pressure 100 kPa to 150 kPa

Length of suction side, L1(m) 1.00

Length of discharge side, L2(m) 20.0

Total length of pipe,L(m) 21.0

Inlet elevation, Z1 (m) 3.20

Outlet elevation,Z2(m) 6.80

Density (kg/m3) 803.12

Pv(Pa) 100000

Viscosity (Pa.s) 0.0005

Step 1: Nozzles design:

Liquid Inlet and Outlet

The Harker equation (1978), modified for SI unit, for the optimum pipe (and nozzle) diameter:

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

Dopt = 8.41 ×20576.9740.45

803.120.31= 92.33mm = 3.63in ≈ 4 in

Where: W in kg/hr and in kg/m3

W = Mass Flow Rate = 20576.974 kg/hr

ρ = 803.12 kg/m3

388

Based on Schedule 40 pipe dimension, the pipe size to be chosen is 4 in nominal size.

For nominal size of 4 in, internal diameter is 4.026 in or 0.1023 m

Therefore, area of pipeline (based on internal diameter):

A =πD2

4=

π × 0.10232

4= 0.00821m2

Step 2: Velocity of Liquid

Based on area of the pipeline, the velocity of the liquid flow:

Fluid volumetric flow rate =mass flow

density=

20576.974kghr

803.12kgm3

=25.62m3

hr×

1hr

3600s

Q = 0.0071m3/s

Q = Av

Rearrange, v =Q

A=

0.0071m3/s

0.0082m2= 0.866m/s

Step 3: Friction in pipe

In calculating the friction in pipe, the whole length of the pipe is taken into account which is the

summation of length in suction side and discharge side. Friction in pipe is determined based on

the following equation:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔

389

In determining the value of friction factor, f, the value is taken based on Moody diagram as in

below with known Reynolds number, Re and relative roughness, 𝜀/D;

Reynolds Number is determined based on the following equation;

𝑅𝑒 =𝜌𝑣𝐷

𝜇= 216286.63

Taking the type of the pipe used as commercial steel pipe, the roughness, ε is 0.046 mm.Thus the

relative roughness is:

𝜀

𝐷= 0.00045

Therefore, based on the Moody diagram, the friction factor is 0.0035. Thus, the friction loss in

pipe is:

ℎ𝑓 =8𝑓𝐿

𝐷

𝑣2

2𝑔= 0.220𝑚

Step 4: Total Head

The velocity flow in both suction and discharge side is the same. Thus through the

rearrangement of Bernoulli’s Equation, the total head is:

ℎ𝑝 = (𝑃2−𝑃1

𝜌𝑔) + (𝑧2 − 𝑧1) + ℎ𝑓 = 10.17𝑚 = 14.05 𝑓𝑡

Step 5: Power Required

Power required by the pump is based on the following equation:

𝑃𝑜𝑤𝑒𝑟 = �̇�𝑔ℎ𝑝 = 2052180.925 𝑊

390

Step 6: NPSHA

NPSHA only involves the suction side. Thus the length of pipe involved is only the suction side.

NPSHA is calculated with the following equation:

𝑁𝑃𝑆𝐻𝐴 =𝑃1−𝑃𝑣

𝜌𝑔+ 𝑧1 − ℎ𝑓1

Friction loss is calculated only on the suction side

ℎ𝑓 =8𝑓𝐿1

𝐷

𝑣2

2𝑔= 0.0105𝑚

Thus, NPSHA = 3.19m

For a pump to operate without cavitation, NPSHA > NPSHR. This requirement is checked for the

suitability of the pump. NPSHR is determined by using the following graph.

From the graph, volumetric flow rate of 25.62 m3/hr or 0.00712 m3/s or equivalent to 104.04545

gal/min gives NPSHR of 25 ft or 7.62 m. Therefore, NPHSA> NPSHR. The pump is applicable.

Step 6: Actual motor power

The efficiency of the motor is determined in the graph above. From the graph, 25.62 m3/hr or

0.00712 m3/s or equivalent to 112.81 gal/min gives NPSHR of 25 ft or 7.62 m the efficiency of

0.55. Thus the actual power motor of the pump is:

Actual power: 3731238.05 W

In terms of horsepower= 5003.59 hp

391

Step 7: Type of pump

(A) Normal operating range of pumps (to find the type of pump suitable), (B) Total Head

versus Flow Rate (to find the speed of pump)

Type of pump chosen = Centrifugal

Speed of pump = 3500 rpm (Coulson & Richardson’s Chemical Engineering)

BOTTOM PUMP, P-105

Step 1: Design Calculation

Parameters (Inlet & Outlet)

Molar flow rate (kmol/hr) 1068.64

Mass flow rate (ton/hr) 192.4808

Volumetric flow rate (𝑚3/hr) 20.0908

Design criteria

Inlet temperature (K) 373.15

Inlet Pressure, 𝑃1 (bar) 1.0

Outlet Pressure, 𝑃2 (bar) 1.2

Length of suction side, 𝐿1(m) 6.00

Length of discharge side, 𝐿2 (m) 7.00

Total length of pipe, L (m) 13.00

Inlet elevation, 𝑍1 (m) 5.00

Outlet elevation, 𝑍2 (m) 5.00

Density (kg/𝑚3) 958.0561

Viscosity (Ns/𝑚2)(Pa.s) 0.0208

392

Volumetric flow rate, ѵ(𝑚3/s)

𝑣 =�̇�

𝜌

𝑣 =19248.08 𝑘𝑔/ℎ𝑟

958.0561 𝑘𝑔/𝑚3 𝑥

1 ℎ𝑟

60 𝑚𝑖𝑛 𝑥

1 𝑚𝑖𝑛

60 𝑠

𝑣 = 0.005581𝑚3

𝑠

Step 2: Nozzles design

𝐷𝑜𝑝𝑡 = 8.41𝑊0.45

𝜌0.31

= 8.4119248.080.45

958.05610.31

𝐷𝑜𝑝𝑡 = 84.82798 𝑚𝑚 = 3.3397 𝑖𝑛

Based on Table 38.the pipe size to be chosen is 4 in nominal size.

From Table 38. Internal diameter, ID is = 4.026 in = 0.1023 m

𝐴𝑟𝑒𝑎 = π𝐷2

4

𝐴𝑟𝑒𝑎 = π 𝑥 0.10232

4

𝐴𝑟𝑒𝑎 = 0.008219 𝑚2

Table 38 – Schedule 40 Pipe Dimensions

393

Step 3: Velocity of liquid

𝑄 = 𝐴𝑣 → 𝑣 =𝑄

𝐴

𝑣 =0.005581 𝑚3/𝑠

0.008219 𝑚2

𝑣 = 0.6790𝑚

𝑠

Step 4: Friction in pipe

Relative roughness:

From Table 5.2 (Coulson Richardson): Absolute roughness for cast iron pipe = 0.26 mm

ɛ

𝐷=

0.26 𝑚𝑚

102.3 𝑚𝑚= 0.002542

Reynolds Number:

𝑅𝑒 =𝜌𝑣𝐷

µ=

958.0561𝑘𝑔𝑚3 𝑥 0.6790 𝑚/𝑠 𝑥 0.1023 m

0.0208 Ns/𝑚2

𝑅𝑒 = 3199.301

394

The Moody Diagram

From The Moody Diagram:

As the Re is too small, use: 𝑓 =64

𝑅𝑒,

𝐹𝑟𝑖𝑐𝑡𝑖𝑜𝑛 𝑓𝑎𝑐𝑡𝑜𝑟, 𝑓 = 0.020004

Assume Length of pipe = 13 m,

ℎ𝑓 =8𝑓

𝐷 𝐿 𝑣2

2𝑔

ℎ𝑓 =8 𝑥 0.020004

0.1023 𝑚 13 𝑚 𝑥(0.6790

𝑚𝑠 )2

2 𝑥 9.81 𝑚/𝑠2

𝐹𝑟𝑖𝑐𝑡𝑖𝑜𝑛 𝑙𝑜𝑠𝑠 𝑖𝑛 𝑝𝑖𝑝𝑒, ℎ𝑓 = 0.4779𝑚

Step 5: Total head, 𝒉𝒑

ℎ𝑝 =(𝑃2 − 𝑃1)

𝜌𝑔+ (𝑍2 − 𝑍1) + ℎ𝑓

ℎ𝑝 =20000 𝑃𝑎

958.0561𝑘𝑔𝑚3 𝑥 9.81 𝑚/𝑠2

+ (5.0 − 5.0)𝑚 + 0.4779𝑚

ℎ𝑝 = 2.6059 𝑚 = 8.5484 𝑓𝑡

395

Step 6: Power required

𝑃𝑜𝑤𝑒𝑟 = 𝑚𝑔ℎ𝑝

𝑃𝑜𝑤𝑒𝑟 = (19248.08𝑘𝑔

ℎ𝑟) 𝑥 9.81

𝑚

𝑠 𝑥 2.6059 𝑚

𝑃𝑜𝑤𝑒𝑟 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 = 492055.5881𝑊 = 492.0556𝑘𝑊

Step 7: NPSH

𝑁𝑃𝑆𝐻𝐴 =(𝑃1 − 𝑃𝑣)

𝜌𝑔+ (𝑍1 − ℎ𝑓1)

𝑁𝑃𝑆𝐻𝐴 =(100000 − 100000)

958.0561𝑘𝑔𝑚3 𝑥 9.81 𝑚/𝑠2

+ (5 − 0.4779)𝑚

𝑁𝑃𝑆𝐻𝐴 = 4.5221𝑚

Volumetric flow rate = 20.0908𝑚3

ℎ= 88.45115

𝑔𝑎𝑙

𝑚𝑖𝑛

Graph Pump efficiency

396

From graph pump efficiency:

𝑁𝑃𝑆𝐻𝑅 = 1𝑚 = 3.2804 𝑓𝑡

Therefore, NPSHA> NPSHR. The pump is applicable.

Step 8: Actual motor power

From graph pump efficiency:

Efficiency, ƞ =0.4

Thus the actual power motor of the pump is:

𝐴𝑐𝑡𝑢𝑎𝑙 𝑃𝑜𝑤𝑒𝑟 =𝑃𝑜𝑤𝑒𝑟 𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑

𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦

=492055.5881𝑊

0.4= 1230138.97 𝑊 = 1230.1390 𝑘𝑊 = 1649.6410 ℎ𝑝

Step 9: Type of pump

Normal operating range of pumps Total Head versus Flow Rate

Type of pump chosen = Diaphragm

Speed of pump = 3500 rpm

(Coulson & Richardson’s Chemical Engineering)

397

MINUTE MEETINGS (1)

Date: 17th

November 2015 (Tuesday)

Time: 9.00pm – 11.00pm

Venue: Cafe Lembaran

Attendance:

1. Syed Zulfadli Syed Putra

2. Nurul Ezati Bt Mat Sidek

3. Syafiqah Binti Mad Zin

4. Elaine Ooi Chin Wen

5. Soon Kah Aik

Agenda:

1. First of all, we discuss and try to understand about the task 3 given by lecturer.

2. We start to distribute part of the task which mainly on the design of unit operations that

involves in our plant design which are reactor, distillation column, absorber, heater,

reboiler, condenser and pump.

3. Set the date for our next group meeting.

Prepared by,

………………………….

(Syed Zulfadli Syed Putra)

398

MINUTE OF MEETINGS (2)

Date: 23th

November 2015 (Monday)

Time: 4.00 pm – 5.15pm

Venue: Anjung Ilmu in School of Chemical Engineering

Attendance:

1. Syed Zulfadli Syed Putra

2. Nurul Ezati Bt Mat Sidek

3. Syafiqah Binti Mad Zin

4. Elaine Ooi Chin Wen

5. Soon Kah Aik

Agenda:

1. Discuss on what we understand on the design of each unit operations.

2. Report any potential problems that will encounter when doing the design later.

3. Plan to meet our supervisor to discuss on effective ways to solve the potential problems.

4. We identified that we need to do mechanical design for all mass and energy transfer equipment.

Since, it is quite similar, we must go back and study then share with each other on next coming

meeting.

Prepared by,

………………………….

(Nurul Ezati Bt Mat Sidek)

399

MINUTE MEETINGS WITH SUPERVISOR (3)

Date :30th

November 2015 (Monday)

Time :3.00 pm – 5.00pm

Venue: Lecturer’s Office in School of Chemical Engineering

Attendance:

1. Prof.Madya Dr. Norashid Aziz

2. Syed Zulfadli Syed Putra

3. Nurul Ezati Bt Mat Sidek

4. Syafiqah Binti Mad Zin

5. Elaine Ooi Chin Wen

6. Soon Kah Aik

Agenda:

1. We had asked Dr that is there any problem in our Task 2 because it will determine whether

we are going to continue our job in Task 3.

2. All the designed unit operations must come out with logic and appropriate scale so that they

are practically/feasible to install in industry.

3. Dr ask us to try our best to design and understand on the design method, perhaps it is useful

in our career in the future.

Prepared by,

………………………….

(Syafiqah Binti Mad Zin)

400

MINUTES OF MEETING (4)

Date : 7th

December 2015 (Monday)

Time: 9.30 pm –11.00 pm

Venue: Cafe Lembaran

Attendance:

1. Syed Zulfadli Syed Putra

2. Nurul Ezati Bt Mat Sidek

3. Syafiqah Binti Mad Zin

4. Elaine Ooi Chin Wen

5. Soon Kah Aik

Agenda:

1. Beginning of the meeting, we review back what we have done so far to check for any

correction or modification of the works.

2. Meantime, we do all the design in spreadsheet (EXCEL) by key in all the important

formula so that will ease our calculation next time.

3. After that, we had continued with our discussion on the mechanical part for every unit

operations.

4. We will discuss with each other immediately through social networking when we face any

problem when doing it.’

5. Start to do the compilation for task 1 and task 2 so that we won’t are able to

complete/submit the final report on time.

6. Plan to meet dr again to update our progression.

Prepared by;

-------------------------

(Elaine Ooi Chin Wen)

401

MINUTES OF MEETING (5)

Date :11th

October 2015 (Friday)

Time: 3.00 pm –4.30 pm

Venue: Café lembaran

Attendance:

1. Syed Zulfadli Syed Putra

2. Nurul Ezati Bt Mat Sidek

3. Syafiqah Binti Mad Zin

4. Elaine Ooi Chin Wen

5. Soon Kah Aik

Agenda:

1. Since dr are busy, so we couldn’t make the las meeting together with dr in his room.

2. Start to do all the compilation.

3. Help those who still not complete their task.

Prepared by;

-------------------------

(Soon Kah Aik)


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