Process for the extraction of fats and oils

Abstract:

A process for the extraction of fats and oils from natural substances using
liquid propane as the solvent is described in which the extraction is carried out at a
pressure of 10 to 30 bar and a temperature of 10° to 55° C. and the separation of the
extracted fats and oils from the solvent is carried out by means of pressure reduction
or/and temperature increase to ≤80° C. High quality products are isolated in this way
in a good yield and under mild conditions.

A process for the extraction of fats and oils from natural substances using
liquid propane as the solvent is described in which the extraction is carried out at a
pressure of 10 to 30 bar and a temperature of 10° to 55° C. and the separation of the
extracted fats and oils from the solvent is carried out by means of pressure reduction
or/and temperature increase to ≤80° C. High quality products are isolated in this way
in a good yield and under mild conditions.

Edible Oil

The extraction of oil and fat for food has always been an important part of
human nutrition and culture. There is evidence that oil fruits such as poppies, rape
and flax were cultivated as far back as the Neolithic period. The first oil mills
appeared in the Minoan culture in 3500 bc while Chinese sources from 2800 b.c
already mentioned soy and hemp as oil plants.

The rapid growth in the population in europe in the 18th and 19th centuries
was due solely to the industrial extraction of oils from plant seeds. Edible vegetable
oils is one of the nutritional foundations on which western civilization is historically
based.

Current Trends

18.5 million tons of oil were produced from plants in 2004.Demand will rise
quickly due to this oil's additional advantage as a substitute for mineral oil.

The world's most important oil seed are now the soy bean, palm fruit, rape,
sunflower, cottonseed and maize. Sunflowers, rape and maize are primarily
cultivated, processed and consumed in Europe. Olives are also processed, but on the
either small scale compared with other fruits, and are intended for direct
consumption.

Constituents, processing and origin

Edible oil contributes unsaturated fatty acids to people's diet. The

recommended daily intake of these fatty acids is 10 grams. Oils contains vitamins E,
D, K and A. In particular, vitamin E is important as an antioxidant. Since these oil
constituents are very sensitive, the process must be controlled very precisely.
 A large number of products, for example palm oil, must be processed directly
after harvesting in order to prevent spoilage. This leads to very harsh conditions for
the plantations which are often located in inhospitable areas close to the Equator.
Since harvesting is a seasonal business, the installed machines must be able to
readily cope with these burdens on production and the difficult climatic conditions.

Oil can not only be extracted from plants, but also from marine animals such
as whales, herring or the liver of other fish. This oil is rich in unsaturated fatty acids.
However, it is not sold commercially as a pure fish oil of waltran for use as edible oil.
For this reason this will be not mentioned any further.

Types of edible oil

Commercial edible oils come from one specific plant or are a mixture of
several plant oils. If oils have a specific plant name, they must stem from the pure
unmixed oil of this plant. Mixed oils are called table oil, edible oil or vegetable oil.
Mixed oils are mostly sold under a brand name. References to the utilized plant oils
are only permissible if their type and proportion are shown on the label.

Mixed oils are normally cheaper and more heat resistant than oils from a
single plant. They can be easily used for all kitchen processing methods such as
frying, baking or deep drying.

The best known edible oil

>Cottonseed oil >Maized oil >Special oils

>Dietary edible oil >Rapeseed oil >Wheatgerm oil
>Thistle oil >Saflor oil
>Peanut fat >Sesame oil
>Linseed oil >Sunflower oil

Edible oils can be produced either through cold processing (up to 40 °C) or hot
pressing with extraction from oil seeds or fruits.

The fruits and seeds from which the oil is extracted (oil fruits) are first cleaned
and then crushed in rollers. The mush created during this process is then normally
heated. The addition of chemical solvents finally "washes" the oil out of the heated
mush, thus producing the raw oil.

The raw oil contains unwanted substances which make it cloudy and spoil it,
and may have a negative effect on taste. These substances include plant residues,
sludge, slime and free fatty acids. In order to separate these substances from the oil,
it is refined. During refining, different chemical and mechanical processes are used to
clean, de-lime, de-acidify and de-color the raw oil and free it from unwanted odors.
The edible oil thus produced is stable, which means that no solid constituents settle
during storage. Refined oil is also clear and light, and ha a much more neutral taste
and smell than untreated raw oil. Refining has no adverse effect on the valuable
polyunsaturated fatty acids. Refined oils are suitable for the preparation of warm
meals in the kitchen, like frying.
Presses or beaten: Differences in oil quality

Cold-pressed or cold beaten oil is obtained solely through pressing and

subsequent filtering of the oil fruits. Pressing of the oil fruits may produce heat which
has an unfavorable effect on the quality of the oil. The oil press is therefore cooled to
ensure high quality oil. The oil is only cleaned in special filter systems.

The quality of cold pressed oil is very high since all the valuable substances
originally contained in the oil fruit are preserve due to the gentle production method.
Cold-pressed oil is characterized by a strong taste and intensive color. It can be called
"natural" or "natural pure". Cold-pressed oil is suitable for the preparation of cold
meals and salads. Since it does not contain any preservatives, it should be used up
quickly. Cold-pressed oils are not suitable for frying. From an ecological viewpoint,
cold pressing uses less energy but only has a yield of between 10 % and 30 %. By
comparison, hot pressing uses a great deal of energy but has a yield of 99.5%.

Principles of oil extraction

Oil is extracted from a number of fruits, nuts and seeds for used in cooking
and soap making or as an ingredient in other foods such as baked or fried goods. Oil
is a valuable product with universal demand, and the possible income from oil
extraction is therefore often enough to justify the relatively high cost setting up and
running a small-scale oil milling business.

Raw material preparation

Oil seeds and nuts should be raw materials (like groundnuts,

properly dried before storage, and cleaned sunflower seeds) need dehusking (or
to remove sand, dust, leaves and other decorticating). Small manual machines
contaminants. Fruits should be harvested are available to give higher production
when fully riped, cleaned and handled rates than manual dehusking.
carefully to reduce bruising and splitting. All
raw materials should be sorted to remove
stones etc. and especially moldy nuts, which
can cause aflatoxin poisoning. When storage
is necessary, this should be in weatherproof,
ventilated rooms which are protected
against birds, insects and rodents. Some

Dehusking is important to give high yields of oil and reduce the bulk of
material to be processed but in groundnut oil extraction about 10% by weight of husk
should be added back to the nuts to allow oil to escape more freely from the press.
 Coconut is dehusked and split the oil yield. Other oilseeds and nuts
by skilled operators as this is faster are usually processed cold provided
than the available small-scale that their moisture content is below
machines. Most nuts need grinding about 70%.
before oil extraction to increase the
yield of oil. Small mills are available for
grinding copra, palm kernels and
groundnuts.

Some seeds (like groundnuts) are

conditioned by heating to 80-90 °C
using a seed scorcher and all oil-
bearing materials need to have the
correct moisture content to maximize

Methods of Extraction

These are basically three methods of removing oil from the raw materials:
solvent extraction, wet processing or dry processing. Solvent extraction is not
suitable for small-scale processing because of high capital and operating costs, the
risk of fire and explosions from solvents and the complexity of the process.
Equipment for wet or dry processing is available at different scales of operation from
household to industrial scale. Traditional methods of extraction are described below,
followed by higher output manual machines and mechanized extraction.
Traditional methods

Oil is extracted from fresh coconut, olives, palm fruit sheanut etc. by
separating the flesh and boiling it in water. Salt is added to break the emulsion and
the oil is skimmed from the surface. In palm oil processing the fruit is first heated in a
digester.

Manual methods.

Oil can be extracted by pressing softer

soil seeds and nuts, such as
groundnuts and shea nuts, whereas
harder, more fibrous materials such as
copra and sunflower seed are
processed using ghanis. Pulped or
ground materiall is loaded into a
manual or hydraulic press to squeeze
out the oil-water emulsion.This is more
efficient at removing oil than
traditional hand squeezing,allowing
higher production rates.

Fresh coconut meal is removed from

the shell using a manual reamer or a
motorised reamer. The fine particles
are pressed in a similar wayto extract
the oil emulsion. The emulsion is
broken and the oil is then separated
and clarified
Presses =
have a number of different designs, hydraulic types are more expensive,
which can be grouped into screw or need more maintenance, and risk
hydraulic press operation. Both types contaminating oil with poisonous
can be manual or motor driven. In all hydraulic liquid.
types, a batch of raw materials is
placed in a heavy-duty perforated
metal 'cage' and pressed by the
movement of a heavy metal plunger.
The amount of material in the cages
varies from 5-39 kg with an average of
20 kg. Layer plates can be used in
larger cages to reduce the thickness of
the layer of raw material and speed up
removal of oil. The pressure should be
increased slowly to allow time for the
oil to escape. Srew types are more
reliable than hydraulic types but are
slower and produce less pressure.
Exept where a lorry jack is used,

Ghanis = are widely used in asia but less so in other areas. A heavy wooden or
metal pestle is driven inside a large metal or wooden mortar. The batch of raw
material is ground and pressed and the oil drains out. They have relatively high
capital and maintenance costs and need skilled operators to achieve high oil yields.

Mechanised Extraction

Motorised presses are faster than

manual or animal types but are more
expensive. Motorised ghanis are also
available, but their higher capital and
operating costs require a larger scale
of production for profitability.

Expellers = are continous in operation and work by grinding and prssing the raw
materials as it is carried through a barrel by a helical screw. The pressure inside the
barrel, and hence the yield of oil,are adjusted using a 'choke' ring of the outlet. The
equipment has higher production rates than similar sized presses but is more
expensive to buy and operate.

Although manual expellers are available, small scale oil millers more often
use powered equipment to reduce the time and labour involve in processing. Some
designs also have an electric heater filted to the barrel to increase the rate of oil
extraction.
 The production rate using
prsses and ghanis depends on the size
of the equipment and the time taken
to fill,press and empty each batch. The
production rate of expellers depends
on the size of the equipment, the
speed of the screw and the setting of
the choke.

Determination of unsafonifiable matter

The unsafonifiable matter is defined as the substance soluble in

an oil which after saponification are insoluble in water but soluble in
the solvent used for the determination. It includes lipids of natural
origin such as sterols, higher aliphatic alcohols, pigments, vitamins and
hydrocarbons as well as any foreign organic matter non-volatile at 100
degree celcius (like mineral oil) which maybe present. Light petroleum
or diethyl ether is used as a solvent but in most cases result will differ
according to the solvent and generally the use of diethyl ether will give
a higher result.

Apparatus:

1. Flat bottom flask or connical flask with a ground glass joint,250 ml.
2. Air condenser 1 m long to fit the flask
3. Separating funnel, 500 ml

Reagents:
1. Alcoholic potassium hydroxide solution: dissolve 7-8g of potassium
hydroxide in an equal quantity of distilled water and add sufficient
aldehyde free ethyl alcohol and make up to 100 ml.
2. Ethyl alcohol:95 percent
3. Phenolphthein indicator solution: Dissolve one gram of
phenolphthlein in 100 ml of ethyl alcohol.
4. Petroleum ether(40-60 degree celcius): analytical reagent grade
5. Aqueous alcohol:10 percent of ethyl alcohol in water
6. Standard sodium hydroxide solution: approximately 0.02N
7. Acetone: analytical reagent grade
8. Anhydrous sodium sulphate

Procedure:

Weigh accurately 5 g of well mixed oil/fat sample into a 250 ml

conical flask. Add 50 ml of alcoholic potassium hydroxide solution. Boil
the content under reflux air condenser for one hour or until the
saponification is complete (complete saponification gives a
homogeneous and transparent medium). Take care to avoid loss of
ethyl alcohol during the saponification. Wash the condenser with about
10 ml diethyl alcohol.

Transfer the saponied mixture while still warm to a separating

funnel, wash the saponification flask first with some diethyl alcohol and
then with cold water, using a total of 50 ml of water to rense the
flask,cool to 20-25 degeree celcius,add to the flask 50 ml petroleum
ether,shake vigorously and allow the layers to separate.

Transfer the lower soap layer into another separating funnel and
repeat the ether. Some oils high inunsaponifiable matter like marine
oils,may require more than three extractions to completely remove
unsaponifiable matter.

Wash combined ether extract three times with 25 ml portions of

aqueous alcohol followed by washing with 25 ml. portions of distilled
water to ensure ether extract is free of alkali (washing are no longer
alkaline to phenolphthlein).transfer ether solution to 250 ml
beaker,rinse separator with ether and rinsings to main
solution.Evaporate to about 5 ml and transfer quantitatively using
several portions of etther to 50ml erlenmeyer flask previously dried
and weighed. Evaporate ether.When all ether has been removed add 2-
3 ml acetone and while heating on steam or water bath completely
remove solvent under a gentle air. To remove last traces of ether,dry at
100 degree celcius for 30 min tll constant weight is obtained. Dissolve
residue in 5o ml of warm ethanol which has been neutralised to a
phenolphthlien end point.Titrate with 0.02 N NaOH.
Calculation:

Weight in g of the free fatty acids in the extracts as oleic acid=0.282

VN

Where V=Volume in ml of standard sodium hydroxide solution

N=Normality of standard sodium hydroxide solution

Unsaponifiable matter= 100(A-B) / W

where A=weight in grams of the residue

B= weight in grams of the free fatty acids in the extracts
W= weight in grams of the sample.

Determination of Acid Value

Definition:

The Acid Value is defined as the number of mg of potassium

hydroxide required to neutralized the free fatty acid present in one
gram of fat. It is a relative measure of raincidity as free fatty acids are
noemally formed during decomposition of oil glycerides. The value is
also expressed as percent of free fatty acids calculated as oleic acid.

Principle:

The acid value is determined by directly titrating the oil/fat in

an alcoholic medium against standard potassium hydroxide/sodium
hydroxide solution.

Analytical Importance:

The value is a measure of the amount fatty acids which have

been liberated by hrdrolysis from the glycerides due to the action of
moisture,temperature and/or lypolytic enzyme lipase.
Apparatus:

250 ml conical flasks.

Reagents:

1. Ethyl alcohol -95 % alcohol or rectified spirit neutral to

phenolphthlein indicator.
2. Phenolphthelein indicator in solution=Dissolve one gram of in 100
ml of ethyl alcohol.
3. Standard aqueous potassium hydroxide solution 0.1 or 0.5 N. The
solution should be colorless and stored in a brown glass bottle.

Procedure:

Mixed the oil or melted fat thoroughly before weighing. Weigh

accurately about 5-10 g of cooled oil sample in a 250 ml conical falsk
and add 50 ml -100 ml of freshly neutralised hot ethyl alcohol and
about one ml of php indicator solution. Boil the mixture for about five
minutes and titrate while hot against standard alkali solution shaking
vigorously during the titration. The weight of the oil/fat taken for the
stimation and the strength of the alkali used for titration shall be such
that the volume of the alkali required for the titration does not exceed
10 ml.

Calculation:

Acid Value=56.1 VN / W

where
V= Volume in ml of standard potassium hydroxide or
sodium hydroxide used
N= Noemality of the potassium hydroxide solution or sodium
hydroxide solution
W= weight in g of the sample

The acidity is frequently expressed as free fatty acid for which

calculation shall be
Free Fatty Acids as oleic acid %/wt= 28.2 VN / W
Acid Value=% fatty acid (as oleic)x 1.99