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Discussion on

TULSION RESIN forWater and special application

By

Thermax Limited - India

South Korea South Korea

World Water Scenario• Three quarters of earth is filled with water

• Estimated water ~ 1.3 X 10 9 km3

• 97.5 % constitute the Ocean (saline water) which is unfit for use.

• Out of 2.5 %, major portion locked in glacier.

• Only 0.5 % is available for human use.

10 countries share 60% of the reserves,

while 29 (in Africa, and the Middle East)

face chronic shortages

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Topics for DiscussionTopics for Discussion� WATER CHEMISTRY

� DIFFERENT TECHNIQUES OF WATER

TREATMENT

� TYPES OF ION EXCHANGE RESIN

� APPLICATIONS OF ION EXCHANGE RESIN

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Water Chemistry • Source• Impurities• Method of Measurement• Units of Measurement• Typical Analysis• Interpretation• Checking of analysis

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Water Sources1.RAIN2.SURFACE3.UNDERGROUND4.SEA

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Water Impurities1.SUSPENDED /

DISSOLVED

2.INORGANIC

3.ORGANIC

4.GASEOUS

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Carbon DioxideTurbidity & SiltAnionicCationic

Oil & corrosion products

Organic matter

Bacteria & PlanktonSilicate &Manganese

Micro OrganismPhosphate Iron

Colloidal SilicaChloride Ammonium

Organic MatterSulphate Potassium

ChlorineColorHydroxideSodium

Methane OxygenOther Suspended Matters

CarbonatesMagnesium

Hydrogen SulphideMud , Dirt and BicarbonatesCalcium

GaseousNonionic and Un-dissolved

Ionic and Dissolved

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Water parameter and its problems

OrganicsCOD (ppm)

OrganicsBOD (ppm)

SilicateSilica (ppm)

SulphateSulphates (ppm)

ChloridesChlorides (ppm)

CO3, OHP - Alkalinity (ppm)

OH, CO3, HCO3M-Alkalinity (ppm)

Dissolved solidsConductivity (ms/cm)

Total dissolved solidsTDS (ppm)

Acidity, AlkalinitypH ( 0 - 14)

Suspended, Colloidal MatterTurbidity NTU

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Units of Measurement• ppm = mg / ltr = gm / m 3

• All parameters in resin applications are measured i n ppm as CaCO3.

• All Chemical react in their equivalent weight.Conversion to CaCO 3

– CaCO3 Eq. Wt. = 50– e.g. ppm of ion in water (71 ppm Cl)

Eq. Wt. (35.5 Eq. Wt. Cl)– ppm as CaCO 3 = Gram eq of ion x 50 ppm as CaCO 3

(Gram eg of ion = Weight of substance ÷÷÷÷ Eq. Wt)

– (71ppm Cl) = 100 ppm as Ca CO 3.

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How to Check Analysis ?• Cation - Anion balance

–Total Cations = Total Anions

–pH Alkalinity e.g. OH or P alkalinity is above 8.2 pH

•

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Why Water Analysis?Water analysis serves following functions

1. Anticipation of problem.

2. Diagnose the problem.

3. Evaluate a change in water treatment.

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Parameters

Conductivity meter. Expressed as micromho/cm

corrosion tendency increases.

2. Conductivity

1. pH paper2. pH indicator

solution.3. pH meter

pH varies accordingto acidic or alkalinecontent. water showscorrosive or scaling tendency.

1. pH

METHOD OF ANALYSIS

SIGNIFICANCEPARAMETER

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Parameters contnd….

Titration with EDTA soln. Expressed in ppm as CaCO3

Chief source of Types : Ca,Mg and total. scale in pipe lines etc

5. Hardness

alkalinity. Analysed after titration with std. acid. Expressed in ppm as CaCO3

Combines with divalent Types : p & m

4. Alkalinity

• Gravimetric analysisDeposits in the water line, heat exchanger etc

3. Suspended solids

METHOD OF ANALYSIS

SIGNIFICANCEPARAMETER

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Parameters

Analysis onColorimetric spectrophotometer

Evaluation of phosphate levels in cooling water. Classified as ortho, poland total phosphates

7. Phosphates

Titration with AgNO3 with chromate indicator, expressed in ppm as chlorides.

Adds to solid content & increase corrosive character of water.

6. Chlorides

METHOD OF ANALYSIS

SIGNIFICANCEPARAMETER

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Parameters

Colorimetric analysis on spectrophotometer. Expressed in ppm as SiO2.

Very hard silicate scale are formed.

9. Silica

Colorimetric analysisspectrophotometer.

expressed in ppm as CaC03.

Adds to solid content & combines with calcium on to form calcium sulfate scales.

8. Sulfates

METHOD OF ANALYSIS

SIGNIFICANCEPARAMETER

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Parameters

Titration with FAS activity. or with chlorotexreagent.

Chlorine demand & biocidal12. FRC

Titration with EDTA with dithizone indicator .

Evaluation of our treatment program.

11. Zinc

Colorimetric analysis On Spectrophotometer

Expressed in ppm as Fe.

Discoloration of water. Deposits in low velocity area and inpipelines

10. Iron

METHOD OF ANALYSIS

SIGNIFICANCEPARAMETER

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SamplingThe sample should be

Representative

Sufficient in quantity

Properly packed and labeled

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Sampling

1. Collect sample in previously sterlised

and closed bottles or containers.

2. Fill sample without rinsing.

3. Sample quantity should be minimum

250 ml.

4. Sample should reach lab within 24 hrs.

5. Label the sample properly.

Sample forAnalysis

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Different Techniques of water Treatment. ????

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Different Techniques Of Water Treatment• Pre-treatment Coagulation ,Chlorination

• Filtration: Sand Filter, Activated Carbon Filter etc.

• Membrane

• Thermal

• Ion exchange

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Different Techniques contd…..

Pretreatment:Extra Hardness by Precipitation� Chemical Coagulation/ Chemical

Precipitation– Hardness and alkalinity removal by

lime soda process (hot or cold)– Iron removalRemoval of Suspended solids

Inorganic Coagulant :# Alum, Iron Salts, etc.# Organic flocculent :-Cationic, Anionic, Nonionic, Polyelectrolyte

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Different Techniques Contnd....Suspended solids

removal contd ….� Gravity settling� Filtration

Different Media :- Sand, Anthracite- Activated Carbon- Polymer Bead- Multimedia Filters- Iron Removal Filters

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Different TechniquesDissolved solids1. Membrane technique Electro dialysis & Reverse

Osmosis

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2. Thermal Desalination

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• A Ion exchange resin is a Insoluble solid polymer having exchangeable ions on which reversible interchange of ions between a solid (IXR) and a liquid takes place.

• A reversible stoichiometric process. Every ion which is removed from the solution is replaced by equivalent amount of another ion of same sign.

• After the ion exchange, the exchanger material can be brought back to original form by suitable reaction, called regeneration.

WHAT ARE ION EXCHANGE RESIN?

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Ion ExchangersInsoluble solid material carrying exchangeable

cations or anions

WAC SAC

Cation Exchange

WBA

Type I Type II

SBA

Anion Exchange

Ion Exchange Resins

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Advantages of Ion -Exchange Technique� Ambient temperature

operation

� Instantaneous treated water

� Take care of fluctuation of load

� Easy waste disposal

� Cheaper to operate

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Cation Resin Manufacturing

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Weak Acid Cation Manufacturing..

• Polymerisation of methacrylic acid and DVB yield a weakly acidic cation exchanger

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Weak Base & Strong Base Anion Manufacturing..

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Type I & WBA

CH3OCH2ClCHLOROMETHYLETHER

N(CH3)3/Catalyst

CH-CH2-CH-CH2-

-CH-CH2CH-CH2

CH2 N(CH3)3 Cl

-CH-CH2

CHLOROMETHYLATED BEADS

CH-CH2-CH-CH2-

CH-CH2

CH2CL

Styrene

CH=CH2

+

CH=CH2

CH2=CH2

DVB

N(CH3)2/Catalyst

CH-CH2-CH-CH2-

-CH-CH2CH-CH2

CH2 N(CH3)2Cl

Weak Base Anion Strong Base Anion

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Anion Type II

-CH-CH2

Styrene - DVB Copolymer

CH-CH2-CH-CH2-

CH-CH2

NCH3CH2OH (CH3)2/Catalyst

CH3OCH2ClCHLOROMETHYLETHER

-CH-CH2

CHLOROMETHYLATED BEADS

CH-CH2-CH-CH2-

CH-CH2

CH2CL

-CH-CH2

TYPE II RESIN

CH-CH2-CH-CH2-

CH-CH2

CH2 NCH3CH2OH (CH3)2

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Resin structure: Cation

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Structural classification• Since about 1935 organic ion exchangers have been

developed in large scale. Contrary to inorganic exchangers their properties can be varied in a much wider range due to the possibilities of polymer chemistry.

• In general the organic ion exchangers consists of a polymer matrix with functional groups. These functional gro ups may be part of the organic monomers or are introduced by o ther means. The final material has the properties of a r esin and, as a consequence, organic ion exchanger are often design ated as ion exchange resins .

• ON STRUCTURE BASIS IT HAS BEEN CLASSIFIED IN TWO TYPES GEL AND MACROPOROUS

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What is Macroporous resin ?• Also referred to as Macro-reticular resins. • Manufactured using a solvent process that

leaves a network of pathways throughout the beads.

• This sponge like structure allows the active portion of the bead to contain a high level of DVB cross -linking without affecting the exchange kinetics.

• There is an increase of approximately 30-40 % in porosity, which may results in proportionate decrease in exchange capacity due to lowering of the actual exchange sites.

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Gel resins are homogenous cross linked polymers with exchange sites distributed evenly across the bead. The amount of DVB crosslinking used during the synthesis of a bead determines the relative strength of the bead. These resins generally have higher operating efficiency and cost less

What is Gel type resin ?

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Gel and Macroporous structure

WATER

(Moisture)

GEL

Macro porous

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Properties of Tulsion IXR

1. Particle Size2. Effective Size3. Uniformity Coefficient4. Moisture5. Swelling6. Total Exchange capacity7. Kinetics 8. Bulk Density9. Stability

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Properties of Ion Exchange Resins1. Particle Size :

Purely hydraulic and kinetic influence on the ion e xchange process. 0.3-1.2 m size is satisfactory for industr ial applications

0.3mm 1.2mm

2. Effective size = Sieve (mm) on which 90% of beads a re retained.

3.Uniform Coefficient = ratio of sieve size on which 40% retainedto the sieve size on which 90% maintained. .

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4. Moisture Content :It is bound water related to cross linking. About 45 - 55 °C depending on type of resin. Gives valuable information on resin under use

WATER (Moisture)

Properties of Ion Exchange Resins

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5. Swelling :� It is volume change due to change in surrounding

medium.� Depends upon medium, resin matrix.� Ionic group present and type of counter ions� e.g. SAC Na and H form

→→→→←←←←

Form Na Form H

Properties of Ion Exchange Resins

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6. Total Exchange Capacity :

It is the capacity obtained from the total quantity of counter ions that is capable of exchange per unit weight or volume of either dry or swollen resin.

Properties of Ion Exchange Resins

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7. Kinetics (speed of exchange reaction) :It is influenced by cross linking, functional groups, particle size, properties of the influent and temperature.

8. Bulk Density: Bulk density, shipping weight, true wet density•The bulk density is the weight of wet resin per unit volume. This de nsity is measured in a calibrated glass column after back washing the resin, allowing it to settle and draining off the water. T his density is specific for each resin and is dependent on the type of resin an d ionic form. For each wet resin, Thermax has set a value of bulk density, called shipping weight.9. Stability : During service and regeneration resin is subjected to expansion and contraction. Oxidizing agents attack the resin. There is mechanical attrition. All these influence resin life and economics of operation

Properties of Ion Exchange Resins

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Role of Ion Exchange Resin

• Strong Acid Cation : Removes all cation

• Strong Base Anion : Removes all anion

• Weak acid Cation : Remove hardness associated with Alkalinity

• Weak Base Anion : Removes Organic Acids and FMA (Cl, SO4 & NO3)

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Different application of Ion exchange technique.

- Water Softening. - Demineralization.- CPU - Nitrate Removal- MEG - Heavy metal removal- Sugar - Bio Diesel- Nuclear - Brine

Decalcifications

- Pharma-resin

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1.SOFTENING By TULSION Resin

Nacl

CaCO3

MgCl2Water

SO3Na +

Regenerated resin

SERVICE CYCLE

Na cl

RegenerantCa/Mg +

Exhausted Resin

Ca/Mg +

Na cl

Na2CO3

2NaCl

EffluentExhausted Resin

SO3Na

Regenerated resin

CaCl2MgCl2

NaCl

Effluent

Regeneration

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Tulsion Resins for Softening

Tulsion ® T 40 Tulsion ® T 42

Softmax

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SO3H +

Ca ) HCO3Mg) ClNa ) SO4SiO2Regenerated Cation Exhauted Cation

Ca

SO3 +Mg

Na

H2 ) CO3H) ClH2 ) SO4H2 )SiO3Cation Effluent

CH2NH(CH3)3 OH+

Regenerated anion

H2 ) CO3H) ClH2 ) SO4H2 )SiO3

Cation Effluent

CH2NH(CH3)3

Exhausted Resin

CO3ClSO4SiO3

H2O

2. DM Service cycle

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Regeneration of cation in DM

Regeneration of Anion

Ca

SO3 +Mg

Na

HCl

Exhauted Cation

SO3H +

Ca Cl2MgCl2NaCl

CH2NH(CH3)3

Exhausted Anion Resin

+ NaOH

CO3ClSO4SiO3

CH2NH(CH3)3 OH+

Regenerated anion

Na2CO3

NaClNa2SO4

Na2SiO3

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Tulsion Resins : There are 500 Types of resin

Tulsion T 42 Tulsion 52Tulsion T 50Tulsion T 56MP

Cations Tulsion A 23 Gel, Tulsion A 27MP

Strong Base Anion Type I

Tulsion A 36MP, Tulsion A 36 gel

Strong Base Anion Type II

Tulsion A 2XMP,Tulsion A 10 XMP, Tulsion A 8XMP

Weak Base anion

Tulsion Resins

TypeTulsion Resins

Type

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3. What is Condensate Polishing ?(CPU)• The term 'condensate purification' is normally

applied to the treatment of condensed steam from turbines and processes operating in the power, petrochemical chemical and other industries

• Treatment StandardsSodium : less than 5 µg/l as Na+Silica : Less than 5 µg/lConductivity : Less than 0.1 µs/cm at 25 0CIron : total iron < 5 µg/lCopper : Total copper < 2 µg/l

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Why is Condensate Polishing Required ?

• Traces of soluble impurities present in the feed water entering a high pressure boiler can be concentrated within the system

– The degree to which this occurs depends on the design of boiler, heat flux, oxide thickness at heat transfer surfaces, and the level of insoluble impurities

• In a once-through type of boiler all the water entering a tube is evaporated in a single pass and salt concentration occurs at thewater/steam transition point.

• The result of these concentration mechanisms is that there is a risk of corrosion of boiler tubes by ions such as chloride and sulphate, and if failures occur the economic penalties are very severe.

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Why is Condensate Polishing Required Contnd…. ?• In once-through boilers operating under supercritical conditions, i.e.

such that the critical pressure and temperature is exceeded and a single phase fluid exists rather than two phase water/steam conditions all the impurities in the boiler fluid will be present as the fluid enters the turbine.

• Consequently, there is a risk of substances depositing within the turbine. At the temperatures and pressures involved this includes metallic elements like copper and iron which have an appreciablesolubility under the boiler conditions which reduces rapidly as the fluid passes through the high pressure section of the turbine and can lead to the formation of hard, tenacious deposits(CURD) , resulting in deterioration in output from the turbine.

• It also minimizes consumption of make-up water. • It is also applied if the risk of contamination of return condensate is

persistent.

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Impurities Removed by Condensate Polisher…..• Corrosive Impurities:

– Oxides of iron, copper and nickel are the major cor rosive products Cartridge or pre-coat filters can be used for filte ring

• Dissolved Salts– Sometimes due to leakage of cooling water the impur ities

caused by dissolved salts arise – For low-contamination levels mixed-bed ion exchange rs are

commonly used. – Separate cation and anion exchangers can be used on ly

when there is higher level of mineral contamination .

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Factors Affecting The Performance Of Condensate Purification Plant

• Flow rate• Regeneration procedures and conditions• Composition of water to be treated (Inlet

water)• Quality and quantity of treated water to be

produced

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Cycle Termination Is Depending On Following Parameters

• High pressure drop across the resin bed

• High cation conductivity if Cation tower precede MB .

• High effluent silica leakage from MB.

• Total volume of condensate treated (OBR)

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CONDENSATE FLOW DIGRAM

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CONDENSATE POLISHING

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Tulsion ® Resins For CPU

• Tulsion ® T 50 Tulsion ® A 21• Tulsion® T 52 Tulsion ® A 21

MP• Tulsion ® T 42 MP

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4.MEG What is MEG?

Mono-ethylene Glycol (MEG) is a fiber intermediate product. Major raw material for the manufacture of polyester fiber, filament and yarn.

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pH adjustmentCycle water ���� SAC���� DGT ���� WBA

EO Gas Scrubber Stripping Column

GlycolAbsorptionColumn

DI Unit= SAC+ WBA+ CO2 Removal Unit

Evaporator

Drying Column

MEG Conc

NaOH

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Measurement of MEG Purification• Improvement in pH value . Improvement in Conductivity• Improvement in Transmission

>99> 95> 922 -56.5 – 7.8Outlet

99- 10092 - 94 75 - 8075 – 100 3.4 – 3.5Inlet

350 nm275 nm225 nm

Transmission %ConductivitypHSample

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TULSION Resins in MEG Purification• Tulsion T 56MP

•TEC = 1.7meq/ml.in Hydrogen form.•Macroporous catalytic grade•Can take Cations associated with organic acids.•Good Regeneration efficiency.•Regeneration by HCL •Reg. by 4 - 6 % HCl•High operating capacity. pH range 0 - 14•Max. op. temperature 80 °C•Swelling Na --> H 7 %

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TULSION Resins in MEG Purification• Tulsion A 8XMP HP

•TEC = 1.3 meq/ml.in free base form.•No salt splitting capacity in OH- form.•High reg. efficiency.•Reg. by 120% of stoichiometric qty.•Reg. by 1-5% NaOH•High operating capacity. pH range 0 - 9•Max. op. temperature 80 °C•Swelling OH Cl 18 %

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5.Brine Decalcification

It’s a ion exchange process in which hardness from brine is removed to the required level.

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Tulsion CH 90 Tulsion CH 93

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Critical Impurity limits in Brine Decalcification

• Cationic impurities Ca2+, Mg2+Present in all brines Harmful > 20 ppb

• Sr 2+ Common in rock salt. Harmful if Sr > 100 ppb

• Ba2+Common in rock salt. Harmful if Ba > 500ppb

• Al 3+Common in rock salt. Harmful if > 100 ppb,

• SO42+ Common in rock salt. Harmful if > 10g/l

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6. Glucose DeashingLiquid glucose (LG) and dextrose are obtained from starch,

which in turn is derived principally from maize. Starch is also produced from potatoes, rice, taro etc. When starch is hydrolyzed with mineral acids or enzymes, it is converted to glucose. This glucose contains objectionable impurities such as ash, color bodies and proteinaceous materials. In order to meet specifications laid down by many end-users of LG / dextrose, it is necessary to remove these impurities. Normally glucose is supplied as liquid glucose having concentration of 85 % w/w while dextrose is supplied as white crystalline powder.

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GLUCOSE SYRUP 85 % W/W

FILTER ONCE USED CARBON

STARCHSLURRY

ACID / ENZYME HYDROLYSIS

“BREAK POINT”TANK

Na2CO3

CENTRIFUGE

I CARBON AT 60 °°°°CFILTER

SPENT CARBON DISCARDED

T42GEL

SAC

A 2X MP

WBA

II CARBON AT 60 °°°°C

VACUUM EVAPORATION

PAN BOILING TO CRYSTALLIZE DEXTROSE

MARKET

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Tulsion ® Products for Glucose Deashing

• Tulsion T 42• Tulsion A2XMP• Tulsion T 46MP• Tulsion A 2XMP-R• Tulsion T 52

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7. Nuclear

A nuclear power plant is much similar to a coal fir ed thermal plant except the way heat is produced to raise steam. At the heart of a nuclear power plant is the fission reaction in the nuclear fuel,usually uranium, takes place in the reactor core. T o be simplistic, in a nuclear fission, a neutron hits the nucleus of an atom of the uranium fuel and splits it, in which two or three n eutrons are released and used to cause fission in other uranium atoms. Fission of a single atom of uranium yields energy e qual to 200 MeV (million electron volts) in comparison to only 4 eV in the oxidation of one carbon atom. Therefore, on equal w eight basis the total energy from the nuclear fission of 1 tonne of uranium is about as much as that produced from 2.5 million ton nes of coal combustion.

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Tulsion ® Products for Glucose Deashing

• Tulsion® T 46

• Tulsion® A 33

• Boron Enrichment resin

• Chelating Resin

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8. Nitrate Removal• Nitrates have no detectable color, taste or smell at the

concentrations involved in drinking water supplies, and they do not cause discoloration of plumbing fixtures, so they remain undetectable to our senses. Nitrate removal processes must be either foolproof or include extensive monitoring of the treated water to detect breakthrough or determine the need for regeneration.

• Infants are particularly susceptible to nitrates because their digestive systems do not operate in the exact same manner as adults. Nitrates are converted by bacteria in the stomach of infants to toxic nitrites. At levels that would not cause harm to adults, nitrates can cause methemoglobinemia in infants, a condition also known as "blue baby" syndrome.

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Nitrate removal ResinTulsion ® A 62MPThe term "nitrate selective" refers to resins that retain nitrates more

strongly than any other ions including sulfates. A variety of functional groups can and have been placed into anion exchange resins that are nitrate selective. The affinity relationship for ni trate selective resins in drinking water is

Nitrate > Sulfate > Chloride > BicarbonateFunctional Group : Quaternery AmmoniumParticle Size : 0.3 to 1.2 mmpH range : 0 to 14

Regenerant : NaCl

Use Industrial water and Domestic waterOutlet Limit < 1 ppm.

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9. Heavy Metal removal• Iron Removal Resin

From : Sulphuric acid

; Water: Solvent

• Copper Removal from PCB waste.• Zinc Removal rayon manufacturing.• Nuclear heavy metal removal from reactor water.• Barium , Lead • Arsenic• Gold• Chromium from plating Industry

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There are mainly four steps for bringing resin in process

1. Backwash

2. NaOH injection

3. Slow Rinse

4. Fast Rinse

5. Service

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Back Washing

Back washing is done for :

� Loosening the bed

� Re classifying the bed

� To remove dirt and filtered matter

By back washing, more uniform distribution of fluid is obtained in subsequent down-flow operation.

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Back WashingInjecting water in upward direction to expand the bed to about 50%. DM water used for backwash. Can carry out for 15-20 minutes Service Flow

Outlet

Nozzle Plate

Resin Bed

Before Backwash After Backwash

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Regeneration Process

�The process to bring back the exhausted resin to original or usable form is regeneration.

�The reaction is opposite to service reaction.

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Regeneration by Co-flow

Regenerant inlet.

Regeneration outlet.

RESIN BED

Service inlet

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Counter - Current regeneration.(CCR)

Service inlet

Regeneration inlet.

Regeneration Outlet.

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•Slow Rinse:It is extended regeneration. Hence at regeneration flow rate generally by 2-4 BV of water – DM water

Fast Rinse :To remove traces of regenerant.Done at service flow rate. – DM water

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• TROUBLE SHOOTINGSouth Korea

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Troubleshooting• Ion exchange units may experience problems during

operation• For effective troubleshooting consideration should

be given to the following areas:-– Flow rates– Pressure drop– Resin– Backwash :- Pressure drop– Regeneration :- Concentration, Quality– Water quality :- Ion concentration (Ionic load)– Design criteria :- Original design and operating cond ition

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Troubleshooting• Problems generally encountered

–High pressure drop –Decrease in pressure drop–Reduction in capacity (Output)–Poor Quality of treated water

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Major causes in general for less OBR :

� Insufficient regeneration� Increased load� Over running in previous run� Fouling� Resin loss (quantity & quality)� Malfunctioning of up-stream unit/s� Excessive rinsing

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Trouble ShootingMajor causes in general for poor quality :

� Mechanical problem� Chemical precipitation, silica precipitation.� Improper separation and improper mixing

(MB)� Wrong or misleading analysis hence

apparent poor quality

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MBService/Alkali/Down/

Alkali Rinse

Regenerant Effluent

Acid flow/Acid RinseTreated water

Free BoardResin bed Anion and

Cation

Distributor

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THANK YOU

(NOT)

THE END