Fat Splitting (Fatty

Acid Isolation) and

Glycerine Recovery
CHAPTER 4
Learning Outcomes
To define the terms such as fat splitting, glycerine and others
To rectify and comprehend the method of fat splitting
To classified the process parameter such as enzymes and etc
To acknowledge and summarize the principle of production of glycerine.

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Introduction
The importance of fatty acid and glycerine in chemical industry is well
known and they are used in a very wide range of applications such as:
Fatty acid: soap & detergents, cosmetics, lubricants, paint industry,
rubber chemicals, textile chemicals & emulsifier.
Glycerine: toothpaste, alkyd resins, explosive, cosmetics, food &
beverages, pharmaceutical

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Fat Splitting
Fat splitting or hydrolysis is the main reaction step in fatty acid
technology.
Fat splitting is the process to split or hydrolyzed the triglyceride
molecules of fats and oils in the presence of water to yield glycerine and
a mixture of fatty acids.
It can be carried out by chemical modification (catalyzed or uncatalyzed)
or enzyme modification.

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Fat Splitting

Esterification
Glycerol + Fatty acids Triglyceride + 3H 2O
Splitting

Splitting agents (Reverse process)

 Water= hydrolisis
 Methanol= methanolysis
 Caustic soda=saponification
 Amines = aminolysis

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Fat Splitting
Natural fats consists of mainly glycerol ester of fatty acids or
triglycerides.
Fats normally means material of solid consistency, whereas liquid
materials are referred to as oil
Terms depends on parameter
◦ State
◦ Temperature
Fat posses a characteristic of fatty acid

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Fat Splitting: Chemical
Modification
Chemical modification:
◦ Transesterification
◦ Hydrolysis
◦ Aminolysis
◦ Saponification

Splitting agent:
 Water = hydrolysis
 Methanol = transesterification
 Caustic soda = saponification
 Amines = aminolysis

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Fat Splitting: Chemical
Modification
Fatty acid (Methyl
Transesterification ester+ glycerol

Fatty acid + glycerol

Triglyceride Hydrolysis
Fatty acid (soap)+
Saponification glycerol

Fatty acid (amides) +

Aminolysis glycerol

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Fat Splitting (Hydrolysis)
Principle:
◦ Homogeneous reaction between fat and small amount of
water dissolved in fats
◦ Fatty acids and glycerol will be discolored and may have
to be distilled
◦ Reversible process in equilibrium with esterification
◦ Endothermic reaction
◦ Uncatalyzed or added catalyst such as lipases
(bioenzyme) and zinc oxide (dibasic metal oxides)

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Type of Fat Splitting Process
◦ Twitchell process
◦ Batch autoclave process
◦ Continuous process
◦ Enzymatic process

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11

Type…..
Twitchell Process
◦ Advantages: have low initial cost and simplicity of installation and operation
◦ Disadvantages: long reaction period, high energy consumption and
discoloration of fatty acid.
◦ The process make use Twitchell reagents and sulfuric acid to catalyze the
hydrolysis.
◦ The reagents is a sulfonated mixture of oleic or other fatty acid and
naphthalene.
◦ Batch time : 12-24 hours
◦ Degree of splitting almost 80-85%
◦ Normally based in wooden container

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Type…..
Batch autoclave process
◦ Oldest commercial method for splitting higher grade stock to produce light
colored fatty acids.
◦ More rapid than Twitchell process, take 6 to 10 hours.
◦ Distillation normally performed to remove glyceride esters.
◦ This process use catalyst such as zinc, magnesium or calcium oxides. Zinc is
most active.
◦ 2 – 4% catalyst is used, a small amount of zinc dust is added to improve color
of fatty acid.
◦ Conversion more than 95%
◦ The autoclaves are tall cylinders, made of corrosion-resistant alloy and fully
insulated.

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Method of Fat Splitting
Batch autoclaves process
◦ An injection of live steam provides the agitation although in addition use
mechanical agitator.

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Method of Fat Splitting
Continuous process
◦ High pressure fat splitting known as Colgate-Emery process.
◦ High pressure (5000 kPa) and temperature (250 – 260 oC) used permit short
reaction time.
◦ Full countercurrent flow of oil and water produces a high degree of splitting
without the need of catalyst.
◦ The crude fat passes as a coherent phase from the bottom of tower whereas
the heavier splitting water travels downward as a dispersed phase.
◦ Degree of splitting more than 99%.
◦ Reaction time only 2 to 3 hours.
◦ Advantages: short reaction time, low energy consumption, little discoloration
of fatty acids.

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Type…..
Enzymatic splitting
◦ Use lipolytic enzymes such as Candida Rugosa, Aspergillus Niger and
Rhizopus Arrhizus.
◦ Crude fatty acid is predried and degassed under vacuum and fed to
distillation unit.
◦ Operated at vacuum of 1.2 kPa or less and a temperature approximately 200 o
C.
◦ The distilled fatty acid has an almost water white color and is free of
impurities.
◦ The bottom ends are charred viscous polymerized material.

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 16
Type…..
Enzymatic splitting
◦ Hydrolytic reaction is brought about by the action of lipolytic
microorganisms acting on the triglyceride molecule in the presence
of water.
◦ It survive through with certain moisture and dirt level.
◦ Amount moisture required for the survival is relatively 0.8 (ratio
between vapor pressure of water in the oil to the vapor pressure of
free water at the same temperature.)
◦ Range 0.16 to 0.32 % of moisture in the temperature range for
handling product.
◦ Dirt level more than 0.15%

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Fat Splitting
In fat splitting or hydrolysis, vegetable or animal fats are
split into fatty acid and glycerine, merely by addition of
water. One-tower fat splitting process employs highly
innovative and advanced technology for continuous fat
splitting without a catalyst.

The splitting takes place at a high (55 bar) pressure in

presence of water. The fat and water flow in opposite
directions, resulting in high glycerine-water concentration
and low-steam consumption.

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 Fat Splitting
One-tower splitting plant is totally continuous, designed so that
the fat is pumped in and the fatty acid and glycerine water
pumped out-continuously.
The plant is totally automated and its operation switch-button
simple. All control instrumentation is connected to the
switchboard making it possible for just one operator to supervise
the splitting plant.

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Fat Splitting
Advantages:
◦ Minimum steam consumption (approx. 200 kg/ton of fat)
achieved by heat exchange in the splitting tower.
◦ High glycerine-water-concentration (with a FFA-content of
5% in the crude fat, the glycerine-water-concentration is
approx. 20%) made possible by the specially designed water
distribution system inside the tower top.
◦ Discharge of fatty acids from the plant at approx. 80°C.
◦ Switch-button simple and continuous operation

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Fatty Acid Distillation
The fatty acid produced from the various fat splitting process are purified
and separated into fraction or even individual fatty acids by distillation and
fractionation.
Distillation of crude fatty acids removes both the low and high boiling
impurities such as unreacted partial glycerides, soaps, glycerol, sterols,
phosphatides, pitch water aldehydes and methyl ketones as well as odors.
Fatty acids are extremely sensitive to heat, oxidation and corrosion effect
due to reactive acid group at the end of carbon chain.

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Fatty Acid Distillation
Distillation of heat sensitive fatty acids is a highly complex and difficult
operation requiring specialized process and equipment.
It is specially designed to obtain premium quality fatty acids, free from
odors and low molecular weight components and minimum color
contaminants, with the help of a pre-run column.
The process involves stripping the maximum amount of unwanted volatiles
from the fatty acids.

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Fatty Acid Distillation
Distillation is carried out under high vacuum and lower temperatures
with the shortest residence time allowable.

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Fatty Acid Distillation
EQUIPMENT
The plant consists of a de-gassing and de-watering stage,
complete with a condenser/gas cooler and a condensate
receiver, two pumps, a pre-run column with falling film
evaporator, a product pre-heater, one reflux condenser, two
other condensers.
The main distillation column with a falling film evaporator
and a residue stage falling film evaporator, a condenser
serving as a product pre-heater for the de-gassing and de-
watering stage, a final condenser, a gas cooler, a residue
cooler, a distillate receiver and three pumps

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Fatty Acid Distillation
PROCESS DESCRIPTION
The color and odor carriers of split crude fatty acids-
secondary components,
Created by oxidation and decomposition with a much lower
boiling point - are drawn off together with the fatty acids in
the de-gassing / de-watering stage, mainly with the
stripping steam added to the bottom.

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Fatty Acid Distillation
PROCESS DESCRIPTION
The fatty acids are then continuously fed to the pre-run
column, where most of the remaining secondary components,
the odour and colour, are removed by steam distillation. The
deodorisation of fatty acids, and the separation of odour and
colour components is effected by the addition of steam to the
bottom.

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Fatty Acid Distillation
The fatty acids from the bottom are pumped back partially to
the column through a falling film evaporator, where the
temperature is raised to above 200°C by heating with thermal
fluid. The reflux is brought about by the reflux condenser.
The control is effected via circulation water. The odor and color
material moves to the next condenser due to initial cooling by
the reflux condenser. The vapors entering the next two
condensers help obtain maximum recovery from the first
running separated in the liquid phase separation tank

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 Fatty Acid Distillation
The fatty acids from the pre-run column are fed into the distiller
column. The acids from the bottom of this column are then pushed
back partially through the column via the falling film evaporator,
where the appropriate temperature to achieve the maximum rate of
evaporation inside the distiller column is maintained.

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Fatty Acid Distillation
The distilled fatty acid vapors leaving the column transfer
heat partially to the crude fatty acid in a condenser and then
enter the next condenser, where the maximum recovery of
the distilled fatty acids is effected.
These are then collected in the distillate receiver. The
necessary reduction in the temperature of the distilled fatty
acids is achieved with the help of the distillate cooler.

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Fatty Acid Distillation
As the level inside the distiller column increases the fatty acids from the
bottom of the column are pumped into the residue falling film
evaporator, which are then fed back to the distiller column.
With an increase in the falling film evaporator level, the accumulated
residue is then discharged and after proper cooling in the residue
cooler, conveyed to residue storage

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Production of Glycerine
Glycerine is a tribasic alcohol occurring in nature in the form
of triglycerides which are glyceryl esters of fatty acids.
It is an important high value by product obtained from the
processing of oils and fats.
Also can be synthesized from petrochemical.

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Production of Glycerine
Over the years, the demand for glycerine in the world, has continued to
grow, far outstripping the supply. It's a highly strategic chemical, used in
the manufacture of explosives, pharmaceuticals, foods, paints,
chemicals and dyes.
All-out efforts are therefore being made to bridge this gap between
supply and demand by increasing the present fatty acid industry
capacity, and also to step up the production of glycerine in globally.

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Production of Glycerine
Steps in production:
◦ 1. Pre-treatment:
◦ Objectives: to prepare feedstock for glycerine recovery
(remove impurities)
◦ Can cause fermentation produce trimethylene glycol
and acids
◦ How to remove:
◦ Cooling and settling
◦ Skimmed and settling
◦ Adding Coagulant: AlSO3 or Fe(11) chloride

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 Production of Glycerine
2. Evaporation
◦ Concentrated to 80-88%
◦ Two types :
◦ Natural circulation
◦ Forced circulation
◦ Entrainment separation:
◦ To reduce losses of glycerine in the vapor stream.
◦ Salt removal;
◦ Fat settling

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Production of Glycerine
3. Refining glycerine
◦ Distillation: using steam under high vacuum (5-6mm
Hg)and temperature(290°C). Certain reactions occur:
◦ Nitrogen formation
◦ Volatile components such glycerol esters
◦ Polyglycerols
◦ Acrolein
◦ Recovery

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# BMF Support

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