Exp 1 Physical Refining of Crude Palm Oil _v4_.pdf

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EXPERIMENT No: 1

PHYSICAL REFINING OF CRUDE PALM OIL

1

JAN

2015

1.0 INTRODUCTION

All crude fats and oil obtained after rendering, crushing or solvent extraction inevitably

contain variable amount of non tryglycerides, components such as fatty acids, mono and

diglycerides, phospatides, sterols, tocopherols, hydrocarbons, pigment(gossypol,chlorophyll),

vitamins(carotene), sterol glucosides and glycolipids.

Physical refining was utilized as early as 1930 as a process for the preneutrallization of

products with a high initial FFA content. In this case, preneutralization was followed by caustic

refining. Later, it was found possible to physically refine lauric oils and tallow if the proper

pretreatment was applied before steam distillation. Physical refining became a reality in the

1950s for processing palm oil, which typically contains high FFAs and low gum contents. The

palm oil process subjected the crude feedstock first to pretreatment and then to deacidification.

The pretreatment consisted of a degumming step and an earth bleaching step, which together

remove certain nonvolatile impurities by filtration. Volatile and thermally labile components are

removed during the conditions of steam distillation under vacuum, which originally gave the

process its name of steam refining. However, for vegetable oils, such as soybeans, that containrelatively low levels of FFA

The traditional edible oil processing system consists of caustic neutralization, bleaching,

and deodorization. Caustic neutralization of vegetable oils with high phosphatide contents

delivers a soapstock that is a mixture of sodium salts of fatty acids, neutral oil, water, unused

caustic, and other compounds resulting from the reactions of the caustic with various impurities

in the oil. Disposal of this soapstock or the waste streams from soapstock processing systems has

become increasingly more expensive. A second problem associated with chemical neutralization

is the loss of neutral oil, which reduces the overall yield from the crude oil. Elimination of the

caustic refining step is economically attractive, but it means that degumming or some other

pretreatment process or system must assume all the functions of the alkali refining process,

except for FFA removal



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2.0 METHODOLOGY

The experiment can be divided into 3 main parts:

1. Removal of free fatty acids, phospholipids and impurities.

2. Removal of pigments, oxidation products, metals and soup.

3. Removal of free fatty acids and fatty acids, mono & diglycerides, oxidation products,

pigments and decomposition products.

The main objective of this experiment is to operate pilot scale experiment of refine,

bleach and deodorize processing of crude palm oil. The experiment starts with identification of

optimal parameter for degumming, bleaching and deodorization processes. The optimal

parameter is identified in range as below:

.

Parameters Degumming and

Bleaching(Range)

Deodorization(Range)

Temperature (oC) 80-110 220-260

Pressure (mmHg) 60-90 5-20

Contact time (minutes) 20-50 30-60

After the operating parameters have been identified, a pilot scale experiments facilities

will be set up based on the operating parameter. There are two physical pilot will be used which

are pre-treatment consists of degumming and bleaching stage and deodorization stage. The

neutralization/the pre-treatment stage is done by using the portable container unit. Then analysis

is done for the oil before and after the experiment.



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2.1 Operating Parameter

In this experiment, students need to identify the optimal operating parameters of refining

process. Based on the range of operating parameters given in the previous table process, students

need to select different value of each trial.

Table 2.1: Operating parameter data sheet

Parameters Degumming Bleaching Deodorization

Temperature (oC)

Pressure (mmHg)

Contact time (min)



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2.2 Crude Palm Oil Sample

The crude palm oil (CPO) samples used in this research study were obtained from Kilang

Sawit Hutan Melintang Perak. The quality of the CPO sample is good which is the free fatty acid

content of this sample is less than 2.5 % and the moisture content of the sample is about 0.15 %.

2.3 Phosphoric Acid and Bleaching Earth

Bleaching earth used is neutral bleaching earth and phosphoric acid used is phosphoric

acid 85% concentrated. The dosage of bleaching earth is 1.0% - 3.0% by weight of oil and the

phosphoric acid dosage is 0.5%- 2.0% by weight of oil depends on the FFA % at initial stage.

2.4 Degumming and Bleaching Experiment

The degumming and bleaching experiment are set up according to the optimal parameter

identified, which are ___ oC, under vacuum of ___mmHg and contact time of ____ minutes. The

equipment set up for this experiment is as shown in Figure 2.1 next page.



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Figure 2.1 Bleaching Unit

Control panel

Vacuum gauge

Stirrer rotor

Bleaching Filter



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2.4.1 Experimental Procedure for Degumming and Bleaching

In this study, the CPO sample used for degumming and bleaching processes is 10000

gram ± 10 gram for each trial. The phosphoric acid used is about 0.1 % w/w and the

bleaching earth used is about 1 % w/w. Heating element for this experiment is silicon oil.

The CPO is initially heated up to 65-90 oC using water bath. After heating up for 30

minutes, CPO will be transferred to main vessel body T 141 at Bleaching Pilot Plant Unit. The

procedure must be doing through the hose given with initial vacuum condition in T141. Start

stirrer and set the rotation speed accordingly with low rpm. Once the CPO has fully charged into

the vessel, prepare the Phosphoric Acid (PA) with the calculated volume based on the theory

given in the previous page. Transfer PA into T141 slowly through with the same inlet of CPO

previously. Set the time of 30 minutes with constant speed of stirrer. The process can be done in

atmospheric pressure.

Once the degumming process completed, set the vacuum to ____ mmHg. At the same

time, the mixture is heated up to 90oC by manipulating ball valve S141 BV 1555. Once the

vacuum reading is consistent, prepare the bleaching agent based on the weight % provided. After

achieve 30 minutes of degumming, slowly add bleaching powder through suction hose attached

at small tank T 142 similar to CPO and PA charge in process. Let the temperature reach at desire

state and reserve it for one hour or extra another 30 minutes.

Stop the stirrer after that and check the filtration unit to ensure the tightness of thee filter

frame. Run the filtration pump and same time bleed for 10 seconds to reduce vacuum condition.

Open the bottom valve to allow the flow of mixture. The process may be sluggish due to small

diameter of pipe and also the size of the filter cloth which is between 0.5-3.5 micronmeters.

Collect the bleach oil in plastic pale and ready to transfer to deodorization pilot plant unit.

2.5 Deodorization Experiment

The deodorization experiment is set up according to the optimal parameter identified,

which are ____ oC, under vacuum of ___ mmHg and contact time of _____ minutes. The

equipment set up for this experiment is as shown in Figure 2.2 next page.



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Figure 2.2 Deodorization Unit



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2.5.1 Experimental Procedure for Deodorization

After the oil has undergone degummed and bleached process, the oil is then will be

prepared to deodorization process.

Place a new filter bag in polishing filter F08I and close the filter. Start vacuum system

V08I following the procedure outlined in the instruction manual and evacuate deodorizer D08I to

a vacuum of about 6.7 mbar.

Start pump P704 (located at the storage tank area) and feed oil from the storage tank to

deodorizer D08I. At high level HLA08I, stops pump P704. Switch on electrical heating element

HT08I. Set the deodorization temperature (normally 250°C) at temperature controller TIC08I.

Use the metering valve to set the flowrate of sparging steam to deodorizer D08I (see

Appendix 1). Maintain the oil in deodorizer D08I at the deodorization temperature and under

steam sparging for the desired deodorization time. At the end of the deodorization time, switch

off electrical heating element HT08I and stop temperature controller TIC08I.

Start cooling water flow to the internal cooling coil of deodorizer D08I to cool down the

oil to less than 90°C. Stop cooling water flow and the temperature controller, close the sparging

steam valve and shut down vacuum system V08I. Open the vent valve of deodorizer D08I to

break the vacuum. Starts pump P08I and discharge the oil to storage tank T082 through polishing

filter F08. When deodorizer D08I is empty, stop pump P08I. Empty the pipelines by opening the

drain valve at the pump.

3.0 Analysis

The experiments for CPO and RBDPO qualities are conducted based on the standard

method by MPOB. The following analysis should be done to determine the quality of oil (before

and after the process):

a) Free Fatty Acid (FFA) content

b) Moisture content

Sampling standard must be followed and data must be taken at least 3 trials. Data analysis

should be conducted to find mean and median. For crude palm oil, sample should be taken from

bottom, middle and top drum. The sample are mixed and taken for analysis.



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For process oil, sample should be taken uniformity at sampling valve. Sample should be taken

for the first time after processing.

3.1 Free Fatty Acids (FFA) Content

Theory:

Acidity or free fatty acid (FFA) in the palm oil is calculated as palmitic acid from the

equation:

% Free Fatty Acid as palmitic acid =.××

Where,

M is the molarity of standard NaOH or KOH solution

V is the volume of the standard NaOH or KOH solution used (ml)

m is the mass of the test sample (g)

Apparatus:

Burette, 25 ml capacity graduated in 0.05 ml subdivisions

Conical flasks, 250 ml and 500 ml Hot plate, with magnetic stirrer and temperature control

Analytical balance

Reagents:

1. Standard potassium or sodium hydroxide, 0.1M

Potassium or sodium hydroxide of approximate 0.1M should be standardized with

potassium hydrogen phthalate.

Dry potassium hydrogen phthalate in an oven at 120 oC for 2 hr and allow

cooling in a desiccators before use.

Weight 0.4g ± 0.02g to 0.1 mg accuracy of the potassium hydrogen

phthalate directly into a conical flask.

Add 50 ml of water and a few drop of phenolphthalein indicator.

Place on a hot plate and swirl till the salt has completely dissolved and

titrate with potassium or sodium hydroxide to the first appearance of a

permanent pink color.

Molarity of the alkali =×

×.



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2.

Phenolphathlein indicator solution, 1% in isopropanol (or in 95% ethanol)

3. Neutralized isopropanol

Place 50 ml isopropanol in a flask and bring the solution to the boil over

hot plate.

Add about 0.5 ml of phenolphthalein and neutralized by drop-wise

addition of 0.1M potassium hydroxide or sodium hydroxide till a faint but

permanent pink color is obtained.

Experimental procedures:

1. Prepare the sample for the analysis by melting the sample at 60 to 70 oC and

thoroughly homogenize it before sampling.

2. Keep the sample in a clean and dry flask with stopper or screw cap to prevent

contact with humidity.

3. Weigh 5 to 6 g of sample into a conical flask.

4. Add 50 ml of the neutralized solvent.

5.

Place the flask on the hot plate and regulate the temperature to about 40oC.

6. Shake the sample gently while titrating with standard alkali until the appearance

of the first permanent pink color. The color must persist for 30 sec.

3.2 Moisture Content

Theory:

The moisture content can be calculated by the equation below:

% Moisture and volatile matter =

×100%

Where,

m is the mass of the dish (g)

m b is the mass of the dish and test sample (g)

md is the mass of the dish and test sample after drying (g)



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Apparatus:

Air oven

Analytical balance

Petri dishes

Desiccator

Experimental procedures:

1. Dry cleaned petri dishes in the oven at 103oC for at least 15 min and allow

cooling in desiccators. Weigh the dish to the nearest 0.001g.

2. Weigh approximately 10g of the molten oil (test sample) to the nearest 0.001g

into the dish. Return to the desiccators until the oil has thoroughly cooled. Weigh

the dish plus the oil to the nearest 0.001g and place the dish in the middle shelf of

the oven at 103oC for exactly 2.5h.

3. Remove the dish and allow it to cool to room temperature in the desiccators (30 to

45 min) before reweighing to the nearest 0.001g.

4.

If the moisture exceeds 0.3%, continued drying (at 30 min interval) to constant

weight is recommended. In this case, the difference between two successive

weighing should not exceed 0.002g. Carry out two determinations of test portions

taken from the same test sample.



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Table of Data:

Table 1: Result for analysis (CPO)

Analysis Crude Palm Oil (CPO)

Sample 1 Sample 2 Sample 3 Average

Free Fatty Acid

content (%)

Moisture content (%)

Table 2: Result of analysis (RBDPO)

Parameters Refined Bleached Degummed Palm Oil (RBDPO)

Sample 1 Sample 2 Sample 3 Average

Free Fatty Acid

content (%)

Moisture content (%)

Analysis

Find mean and standard deviation of each data.



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4.0 Discussion

Compare the value of free fatty acid and moisture content of sample obtained with the standard

value of refinery quality of RBDPO (refer Appendix 1).



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APPENDIX 1

Table A1: Desired quality of pretreated and RBD Palm Oil

Table A2: Palm oil specification for Malaysia (taken from MPOB, 2002)

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