Lipid Manual

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Book No: MA 0901 00-02-11 13

Application Manual
14 00-02-11 Book No: MA 0901

Application Manual
08/7,0,;
Process by
Alfa Laval Separation AB
For Alkali Refining of Oils & Fats
Book No: MA 0901 00-02-11 15

Application Manual
16 00-02-11 Book No: MA 0901

Application Manual
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The results in the continuous refining of vegetable and animal fatsare highly
dependent on the working conditions, as for instance the quantity of lye used
and the lye concentration. Usually, the highest losses occur in the neutraliza-
tion stage, but also the losses in the degumming, the re-refining and the wash-
ing stages may in certain cases be of decisive importance for the yield, special-
ly when treating oils with a low free fatty acid content. Therefore, the quantity
of the lye and its concentration should be correctly calculated and carefully
checked during processing. This applies also to the other working conditions
in the different refining stages.
For an exact determination of the yield, the crude as well as the dried refined
oil should be weighed, suggestively by the Loss Monitoring System.
However, the losses may also be found by determining the total quantity of fat
in the soapstock from the neutralization or the refining stage, as well as in the
water discharged from the washing and degumming stages. In this case the to-
tal quantity of soapstock and water is treated with sulphuric acid, and the total
amount of acid oil determined. The losses in each stage may also be determin-
ed separately, according to “Methods for the analysis of vegetable oils” - ALS
4031. In the latter case the quantity of soapstock and that of water should be
determined in each stage and the fat content of the different soap solutions be
determined by analysis.
The determination of the total loss and of the losses in the different refining
stages allows a complete control of the refining process, but is rather time con-
suming. When starting the refining of an unknown oil the working conditions
must therefore be chosen by simpler means.
The following general instructions, based on practical experience, allow an es-

timation of the best working conditions from the very beginning of the refining
operation. Some special recommendations for treating various oils are also gi-
ven, in ALS4041 E 111, 112, 113, etc. However, as is well known to all refin-
ers, fats have very different properties, and general recommendations are not
necessarily valid for special cases.
The ALS MM all-hermetic plant has hermetically sealed separators which

work under pressure and during the whole refining procedure the oil is kept in
a closed system under pressure, which excludes air from coming in contact
with the oil. This protects the oil from oxidation, which has a bad effect on the
flavour and stability of the oil.
Book No: MA 0901 00-02-11 17

Application Manual
18 00-02-11 Book No: MA 0901

Application Manual
'HJXPPLQJVWDJH
The gums are dissolved in the crude oil and have to be precipitated before sep-
aration can take place. This is done by adding water, which flocculates and
precipitates the gums. Some oils contain gums which cannot be precipitated
and removed by water degumming. Cf. under “Phosphoric acid pretreatment”.
The quantity of water required depends on the gum content of the crude oil.
For hydrating a certain quantity of gums, approximately the same quantity of
water is normally reckoned with. Most oils have a gum content between .5 and
2 per cent and, consequently, the equivalent amount of water should be added.
If too little water is used the precipitation of the gums will be incomplete. On
the other hand, if more water is added than the amount with which the gums
can react, the mixture will then contain free water, which tends to emulsify the
neutral oil and cause great losses in the degumming.
The degumming temperature should preferably be approximately 65-75°C. At

lower temperatures, the viscosity of the oil is high and the separation efficien-
cy low; at higher temperatures the precipitation of the gums will be incomplete
and more of them will remain dissolved in the oil. It is recommended to add
some flushing water in the separator bowl to prevent the gums from clogging
up the bowl.
1HXWUDOL]DWLRQVWDJH
The quantity of lye theoretically required for a complete neutralization of the
fatty acids is at first calculated as follows:
P = L x d x FFA x 1000 litres per hour

100 x M x n
L = Oil flow in the neutralization stage l/h
d = Specific gravity of the oil at neutralization temperature
FFA = Content of free fatty acids in the crude oil in per cent
M = Molecular weight of the fatty acids
n = Normality of the lye
Normal throughput = 2 000 l/h
Supposed specific gravity d = .9
Book No: MA 0901 00-02-11 19

Application Manual
Molecular weights:
Coconut oil, palm kernel oil and babassu M = 200

Palm oil M = 256
Rapeseed oil (high erucic acid type) M = 308
Most other oils (viz.: cottonseed oil,linseed oil, olive oil, M = 282
peanut oil,shea butter, soybean oil, sunflower oil)
If the concentration of the lye in degrees Bé is known, the normality can be

seen from the following table:
/\HFRQFHQWUDWLRQ%p 1RUPDOLW\
4 0.70
8 1.45
12 2.26
16 3.20
20 4.25
24 5.40
28 6.75
If refining, for instance, a groundnut oil using a lye of 20°Bé at a throughput

of 2 000 l/h, the quantity of lye required for neutralizing the fatty acids is:
2000 x 0.9 x FFA x 1000
P = = 15 x FFA l/h
100 x 282 x 4.25
The FFA is determined according to ALS 4031 E 101
Normally, the theoretically calculated amount of lye is not sufficient for ob-
taining an optimum result. Firstly, the oil does not always become neutral with
the stoichiometric quantity of lye and, secondly, the losses in the neutralization
stage depend highly on the excess and the concentration of the lye. For a clear
understanding of the factors influencing the yield, it should be noted that in the
neutralization of crude oils four different kinds of losses occur:
a) the free fatty acids
b) the mucilage and colouring matters as well as other impurities, which are
removed in the neutralization
c) the saponification losses, which arise through saponification of neutral

oil by the excess of lye
d) the neutral oil lost in the soapstock
a) and b) are the unavoidable so-called minimum losses. The losses c) and d)
should be avoided as far as possible. Therefore, it is of great importance to
know how great the different losses are exactly, and this is obtained by care-
fully analysing the soap. The losses can be calculated in the following way:
20 00-02-11 Book No: MA 0901

Application Manual
The designations used are:
FFA = free fatty acids in the crude oil in per cent

FFAR = " " " " " refined oil in per cent
FFASS = " " " " " split soapstock in per cent
X = loss in per cent
Provided that no saponification of neutral fat takes place, the amount of fatty
acids in the crude oil is equal to the sum of the amounts of fatty acids in the
soapstock and the refined oil. Thus, for 100 parts of oil the following equation
holds true:
FFA x 100 = FFAR (100 - X) + FFASS x X, or

100 x (FFA - FFAR)
X=
FASS - FFAR
When the refined oil is neutral the FFAR is 0, and the loss will be:
100 x FFA
X=
FFASS
The refining factor defined as the quotient of the neutralizing losses and the
FFA as per cent in the crude oil without any saponification would then be:
X 100
RN = =
FFA FFASS
The total loss in the neutralization stage can be calculated from the total fat
content in the soapstock. This is done in the simplest way by collecting and
weighing the total amount of soapstock formed during a certain period of time,
for instance, 1 or 2 hours, when working at a known and constant throughput.
The total fatty matter in the soapstock is determined by analysis and the loss
in per cent in the neutralization stage is then calculated. The following equa-
tion holds true even if saponification occurs:
(FFA + FFAV) x 100
FFASS =
FFA + FFAV + N
FFAV = The amount of fatty acid formed through saponification in per cent
of the crude oil
N = The neutral oil in the soapstock in per cent of the crude oil
If the refining factor obtained by weighing the soapstock is called RS, we have
FFA + FFAV + N
RS =
FFA
Hence,
FFAV RS N 1
= - 1 and = RS (1 - )
FFA RN FFA RN
Book No: MA 0901 00-02-11 21

Application Manual
From these two equations the saponification as well as the oil losses can be cal-
culated.
([DPSOH
2 000 1 of coconut oil with a specific gravity of .87 were refined during one
hour in a continuous refining plant. Thus, the amount of crude oil was 1 740
kgs. The soapstock obtained amounted to 458 kgs. By analysis the total fatty
matter in the soapstock was found to be 28.7 per cent, and the total loss in the
neutralization stage calculated to
458 x 28.7 x 100
= 7.6 per cent
100 x 1740
The FFASS in the soapstock was 91 per cent and the FFA of the crude oil 6.0
per cent.
From these values it was calculated::

100 100
RN = = = 1.10
FFASS 91
total loss 7.6

RS = = = 1.26
FFA 6.0
RS 1.26
FFAV = ( - 1) x FFA = ( - 1) x 6.0 = 0.9 per cent
RN 1.10
and
RS 1.26
N = (RS - ) x FFA = (1.26 - - 1) x 6.0 = 0.7 per cent
RN 1.10
Thus 0.9 + 0.7 = 1.6 per cent of the total loss of 7.6 per cent was to be attri-
butedto saponification and neutral oil losses.
It has been found by experience that approximately 50-75 per cent of the lye
excess is consumed in saponification of neutral oil. The saponification de-
pends, however, on the nature of the oil, the neutralization temperature, the
concentration and amount of the lye, the manner of mixing and the contact
time.
The losses under b) cannot normally be calculated exactly, because part of the
mucilages, by the splitting with sulphuric acid used in the analytical determi-
nation of the total fatty matter, are converted into water-soluble compounds
which are not accounted for in the calculation of the total loss. However, this
error is to be considered relatively small: firstly, because the amount of gums
is usually low and, secondly, because an essential part of the lecithin molecules
consists of fatty acids which are found in the split fat. It has been found by ex-
periments that normally the error in question does not exceed 0.1 - 0.3 per cent
of the crude oil.
22 00-02-11 Book No: MA 0901

Application Manual
The amount of neutral oil emulsified by the soapstock depends on the charac-
ter and the fatty acid content of the oil, as well as on the excessand the concen-
tration of the lye and the way of mixing.
Generally, the weaker the lye and the lower the excess, the lower the FFASS
(i. e., the greater the neutral oil content in the soapstock). This applies specially
to oils with a relatively high percentage of fatty acids. Therefore, as a general
rule it can be said that the higher the FFA of the oil, the higher the appropriate
concentration of the lye.
In most cases, oils with an acidity lower than 1 per cent can be neutralized with
a lye of 6-12 Bé without the loss of neutral oil, the soapstock being too high.
For oils with an FFA between 1 and approximately 5 per cent a lye of 20 Bé is
normally used. For oils having a still higher content of fatty acids a lye con-
centration between 20 and 30 Bé is often required, to reduce the amount of
neutral oil in the soapstock. Certain oils, specially crude oils with a high con-
tent of gums and palm oil, give relatively high content of neutral oil in the
soapstock and the FFASS rises only slowly when the excess of lye is increased.
Even if the loss of neutral oil in the soapstock is slightly reduced when a higher
excess of lye is used, the losses due to saponifications of neutral oil increase
at the same time. Therefore, the higher the lye excess the greater the total loss-
es. It is recommended to neutralize such oils with a lye excess of only 10-15
per cent. On the contrary, other oils, especially degummed oils such as ground-
nut, rapeseed, soybean and sesame oils, give a very rapidly rising FFASS with
increasing lye excess. The following results obtained when refining groundnut
oil are typical:
Groundnut oil - FFA = 2.5 per cent, refined with a lye of 20 Bé.
Excess of lye FFASS Refining Real refining

factor saponification
without included
saponification
per cent per cent 100/FFASS
5 55 1.82 1.86
40 75 1.33 1.61
80 80 1.25 1.81
From this table it can be seen that a certain excess of lye helps to break the
emulsion and to reduce the amount of neutral oil in the soapstock, even if a cer-
tain saponification of the neutral oil takes place at the same time. For this type
of oils an optimum yield is normally obtained if adding 40-50 per cent more
lye than required for the neutralization of the fatty acids. As a general rule it
can be said that strong lye produces a relatively strong break of emulsions,
while less concentrated lye has a weaker action. Therefore, the weaker the lye
the higher the excess to obtain the same FFASS. Furthermore, a weak lye pro-
duces less saponification, so that the saponification losses will be small even
if a rather high excess of lye is used.
For the majority of the oils the best neutralization temperature is between 70-
90°C.
Book No: MA 0901 00-02-11 23

Application Manual
Even if the fatty acid content of the oil has been carefully determined in the
beginning of the test and the required lye quantity and the lye concentration
have been correctly calculated, it happens often that changes in the fatty acid
content of the crude oil necessitates a new checking. The final refining result
can, of course, only be judged after the determination of the yield, but experi-
ence has shown that the proper excess of lye can be estimated by much simpler
means. For this purpose a checking of the free fatty acid content of the refined
oil as well as of the viscosity and the alkalinity of the soapstock may be used.
When lye of 20 Bé is used, the following applies to the majority of the oils:
If no lye excess then the refined oil will not be neutral. (Note:
is used, for red-coloured oils, as for instance, palm oil
and cottonseed oil, phenolphthalein is unsuit-
able as an indicator, because the end of the ti-
tration cannot be clearly noticed.) The oil has a
tendency to form emulsion, and the liquid seal
of the hermetic separator is easily broken. The
FFASS is often very low, 50 per cent or less.
If a lye excess the refined oil is completely neutral. The soap-
of 5-15 per cent stock, which is neutral to phenopthalein has a
is used, hard and smooth surface, similar to sausage
skin. The FFASS is normally between 60 and
70 per cent.
If a lye excess the soapstock gives a distinct alkaline reaction
of 15-30 per cent with phenolphthalein. Only a few seconds will
is used, elapse before the red colour appears. The soap-
stock is soft and the FFASS about 70 per cent.
If a lye excess the soapstock will give an instantaneous alka-
of 30-50 per cent line reaction with phenolphthalein. Further-
is used, more, the soapstock will be very soft. Soap-
stock from certain oils, especially oils with
high iodine number, may be completely fluid.
At the same time the FFASS is high: values be-
tween 80 and 90 per cent, and still higher, are
by no means uncommon. The refined oil is not
always bright but contains some soap.
If a lye excess salting-out takes place, the feed pressure in the
higher than 50 per cent separator gradually increases and the through-
is used, flow is reduced. The neutral oil contains much
soap, and the oil appears quite dark in the in-
spection glass. These separation difficulties
can be overcome by adding some flush water
into the separator bowl. (Cf. below)
The above applies when lye of 20 Bé is used. With other lye concentrations the
picture may change somewhat: when using a weaker lye the soapstock will
generally be softer and thinner, sometimes quite fluid. Because of the hydro-
lytic reaction between soap and water, diluted soapstocks always show alka-
line reaction with phenolphtalein, even when there is no lye excess.
24 00-02-11 Book No: MA 0901

Application Manual
On the other hand, when a stronger lye is used the soapstock will be much
harder and thicker. It is to be noted that soapstock from different oils has very
varying consistencies. Generally, the higher the iodine number the greater the
fluidity of the soapstock. For instance: the soapstock from linseed oil and soy-
bean oil is soft or fluid even when a relatively low excess of lye is used. Hard-
ened oils, for instance, always produce a very hard soapstock. Oils with a high
content of mucilage or of other emulsifying agents always give a low FFASS.
As stated in the Instruction Manual for the hermetic separator the position of
the boundary between the two liquids in the bowl is regulated by changing the
working pressure. If the counter-pressure in the outlet pipe of the separator is
increased by throttling the oil regulating valve, the position of the boundary in
the bowl will be displaced outwards. With this regulation the oil appears nearly
bright in the inspection glass of the discharge pipe. The soapstock is, however,
separated under relatively unfavorable conditions and has a relatively high
content of neutral oil. If the counter-pressure is too high, the liquid seal will be
broken and the oil will be lost in the soapstock. On the other hand, if the
counter-pressure is too low, the boundary will be situated nearer to the bowl
center. Under these circumstances the soapstock contains a minimum of oil,
whereas the oil may still contain a pretty large amount of soap and will there-
fore appear quite turbid in the sight-glass. A high content of soap in the oil may
cause difficulties in the subsequent refining stages and should therefore be
avoided. The oil should be so bright in the inspection glass that the outline of
a pencil can be clearly observed through the inspection glass. This is normally
attained at a counter-pressure of approximately 0.2 MPa. The pressure drop in
the separator depends on the throughput and the viscosity of the components.
Therefore, for a certain counter-pressure the higher the throughput the lower
the temperature, and the higher the lye concentration the higher the pressure in
the feed pipe.
With too high excesses of lye the separation process in the hermetic separator
may be disturbed. As is well known to all soap makers, electrolytes including
lye produces salting-out or graining, i.e., the soap separates into two phases,
spent lye and soap, of which the first has the highest specific gravity. When oil
is present, the separator will have to handle three different phases. Because of
the fact that the difference in specific gravity between the spent lye and the
soap is greater than between the soap and the oil, the soap outlet will be block-
ed by the heaviest layer, and the soapstock discharged with the neutralized oil
which appears very turbid in the sight-glass. No soapstock is discharged from
the soap outlet and the pressure in the separator rises. If this happens, the heavy
layer of spent lye must be removed. This can be done by adding some flush
water in the separator bowl. This water is mixed with spent lye to give a lighter
mixture which can be discharged together with the soapstock. The salting-out
phenomenon occurs most easily when oils which are difficult to saponify, as
rapeseed, are treated.
As mixing device for oil and lye the so-called disc mixer is usually used, which
gives a fairly mild mixing and a time of contact of the order 1 to 5 seconds.
Further, the speed of the mixer can be regulated according to the requirements
for different oils (cf. ALS 4041). In certain cases the better refining results
with lower neutralizing losses can be obtained by using the Ultra Short Mixer.
This mixing device is situated in the hollow spindle in the separator and gives
a fairly intensive mixing and a time of contact of less than .5 second.
Book No: MA 0901 00-02-11 25

Application Manual
3KRVSRULFDFLGWUHDWPHQW
As mentioned under “Degumming” some oils contain nonhydratable gums or
phosphatides, which cannot be removed from the oils by a water degumming.
Even an ordinary lye refining and water washing cannot in these cases remove
the gums completely. These compounds are often slightly basic and can be de-
tected very simply in washed oils by a “soap”-determination according to ALS
4031-131. They may, however, be distinguished from usual alkali soaps con-
tained in the oil as these are easily removed by further washing with water. Ac-
cordingly refined oils containing only alkali soaps are designated as washable
whereas oils containing residual phosphatides are designated as not washable.
Oils like coconut, palm, and olive oils are easily washed whereas linseed and
rapeseed are not. Peanut, sunflower seed, soybean and cottonseed oils are
sometimes washable and sometimes not.
It has been shown (cf. J.A.O.C.S.34, 293-99, 1957) that the compound res-
ponsible to this phenomenon are phosphatides (gums) containing calcium and
magnesium, which, if left in the oil after refining, give this an inferior quality
(flavour, stability, colour). However, a complete removal of the compounds in
question is obtained, if the oil is treated with a small amount of concentrated
phosphoric acid prior to the neutralization. The phosphoric acid can be of tech-
nical grade and the suitable strength is 75-85 per cent. The effect of treatment
with phosphoric acid on washability and on the phosphatide content of neu-
tralized oils is shown in the table below. The soap analyses are made according
to ALS 4031-131.
7DEOH,
Oil Amount of Soap content in part Phosphatide content
85 per cent per million in per cent
phosphoric
acid, in per after after wa- in the after wa-
cent of oil neutral- ter wash- crude oil ter wash-
ization ing ing
Rapeseed - 2300 1000 0.63 0.20
" 0.2 1300 30 0.63 0.005
Peanut - 1100 260 0.84 0.14
" 0.1 480 20 0.84 0.006
Soybean - 2700 1600 1.10 0.32
" 0.2 800 60 1.10 0.006
Sunflower - 2200 310 0.57 0.15
" 0.2 1100 80 0.57 0.011
Cottonseed - 5000 2100 0.70 0.30
" 0.2 1100 110 0.70 0. 012
26 00-02-11 Book No: MA 0901

Application Manual
With most oils an amount of 0.1 or 0.2 per cent by weight of concentrated
phosphoric acid is sufficient to give a good oil with low phosphatide and soap
content. When using this pretreatment, the amount of lye for neutralization
must be correspondingly increased. The simplest way to calculate the total
amount of lye required is to determine the total acidity FFA + phosphoric acid
of the crude oil according to ALS 4031-101. Consider this acidity as being fat-
ty acids and calculate the amount of lye as shown previously. It must be em-
phasized, that adding phosphoric acid to the crude oil without adding lye may
give rise to corrosion in the separator bowl and in other apparatuses in the
plant. In some special cases it may be advisable to carry out the phosphoric
acid treatment after the neutralizing and before the re-refining of the oil.
5HUHILQLQJVWDJH
The purpose of re-refining is to improve the quality of the oil, specially regard-
ing the colour and the flavor. Depending on the kind and quality of the crude
oil, it may be advantageousHLWKHU to treat the oil with phosphoric acid RU to
make a re-refining, RU to give the oil both these treatments. Hints for different
oils are given in ALS 4041-111, 112-113, etc. Specially when the neutralizing
is carried out in the Ultra Short Mixer it is recommended to re-refine the oil.
In the re-refining mixer the neutralized oil and the re-refining lye are mixed
very intimately for about 15 seconds. As the bulk of the free fatty acids are re-
moved in the neutralizing stage, there is less risk for saponification of neutral
oil, because saponification is catalyzed by soap.
A re-refining of an oil, as well as a phosphoric acid pretreatment, often im-

proves also its washability and its oxidative stability considerably. It has been
shown, that any lecithin content of the neutralized oil is detrimental to the ox-
idative stability and the flavor of the bleached and deodorized oil. This is
shown in table II, where a comparison of a rapeseed oil and a soybean oil is
made.
The sodium carbonate precipitates the calcium and magnesium compounds as

insoluble carbonates and reduces the losses of oil because of its emulsion-
breaking action. The amount of re-refining lye is normally 1-3 per cent by vol-
ume of crude oil flow and the strength may vary from about 6 Bé up to over
30 Bé. The re-refining losses are normally higher when stronger lye and larger
lye volumes are used.
As an example on re-refining losses the following figures can be considered

normal for cottonseed oils:
Strength of re-refining lye °Bé Re-refining loss, per cent of crude

oil
12 0.5 - 0.8
20 0.8 - 1.2
24 1.2 - 2.0
Book No: MA 0901 00-02-11 27

Application Manual
For other oils the re-refining losses are normally lower. As the heavy layer
formed has a fairly high specific gravity, it is normally necessary to flush the
separator bowl with some hot water, to facilitate the removal of excess lye and
soapstock from the bowl. The counter-pressure in the re-refining separator is
normally 0.2 MPa. The temperature should be approximately 70-90°C in the
re-refining stage.
28 00-02-11 Book No: MA 0901

Application Manual
7DEOH,,
Kind Treatment Peroxide Phos- Oxidative stability of Fla-
of oil besides value phatide bleached deodorized oil, vour
neutral- before content expressed as peroxide score
ization bleach- after value (milli-equiv./litre) *)
and ing milli- bleach- in oxidized oil after cer-
water equiv./ ing per tain time intervals
washing litre cent
H o u r s
100 200 300 500
Rape- None 4.35 0.111 22.8 40.5 - - 1
seed
Do Re- 5.20 0.011 7.1 16.5 20.3 - 3
refining
with lye
and
sodium
carbonate
Do Pre- 4.54 0.001 2.1 3.0 2.8 2.5 5
treatment
with conc.
phospho-
ric acid
Soy- None 2.05 0.108 30.0 - - - 1
bean
Do Re-refin- 2.46 0.001 2.3 5.7 13.4 39 5
ing with
mixture of
lye and
sodium
carbonate
Do Pretreat- 1.53 0.009 1.4 4.1 10.2 32.1 5
ment with
conc.
phospho-
ric acid
*) 1 is a bad score and 5 a very good one
Book No: MA 0901 00-02-11 29

Application Manual
:DVKLQJVWDJH
If all preceding operations have been correctly carried out, no difficulties will
be met with in the washing stage. A temperature of 85-90°C for oil and 90-95°
C for water, and an amount of 10-15 per cent wash water are recommended.
Normally, the loss amounts to 0.3 per cent of the crude oil. Abnormally high
losses are usually due to insufficient or incorrect treatment in the re-refining
stage. If for instance the oil from the re-refining separator contains great
amounts of soap, the losses in the washing stage will be high.
In the wash separator there is no need for bowl flush water, and the counter-
pressure is normally 0.3 MPa in this stage. The separated oil should be almost
clear as seen through the sight-glass.
3URFHVVZDWHU
Experience has shown that condense water or dehardened water should pref-
erably be used as process water (i.e. for the preparation of neutralization and
re-refining lye and as wash water). When using hard water as process water
the neutralization and the re-refining lye contain insoluble carbonates which
may clog the proportioning devices, the flow meters and the pumps. Further-
more, very hard deposits, which are extremely difficult to remove, are often
formed on the discs.
It has also been found that the use of hard water increases the soap content of
the refined oil, because calcium soaps soluble in the oil but insoluble in water
are formed. Practical experience has shown that dehardening should always be
carried out, if the hardness of the water is higher than 5 German degrees.
'U\LQJVHFWLRQ
The washed oil contains normally about 0.1 - 0.2 per cent dissolved water and
only traces of soap. After cooling to room temperature, the washed oil will be-
come turbid due to precipitated water, as the solubility of water is lower at low
temperatures. If the oil is stored for some time, the FFA in the washed oil in-
creases in some degree. Therefore, it is advisable to dry the oil in a vacuum
section connected to the plant after the wash separator. The oil is sprayed into
a drying tower and maintained under an absolute pressure of about 40 mm Hg.
Here the oil is dried to a moisture content less than 0.05 per cent.
30 00-02-11 Book No: MA 0901

Special Recommendations
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Book No: MA 0901 00-02-11 31

32 00-02-11 Book No: MA 0901

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Book No: MA 0901 00-02-11 33

34 00-02-11 Book No: MA 0901

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Book No: MA 0901 00-02-11 35

36 00-02-11 Book No: MA 0901

Book No: MA 0901
G U ID E VAL UES F OR A LK A L I R EF I N I N G OF OI LS / FAT S
PRE-TREATMENT N E U T R A L I Z A T I O N WAT E R WA SH IN G
weight
Molecular WITH CONCENTRATED
Fats
Oils
% by volume of oil
Amount of water
Counter-current double wash
% by volume of oil
Amount of water
Single wash
(speed)
Type of mixer
I N T E R M I X S H O R T- M I X R E - R E F I N I N G
PHOSPHORIC ACID
FFA ... <3%

Strength of lye
Strength of lye
(speed)
Type of mixer
FFA ...>3%
Strength of lye
(speed)
Type of mixer
% by volume of oil
Lye
Temperature .... °C
% by weight
Amount of acid
% over stoichiometric
Lye excess
FFA ... <3%

Strength of lye
% over stoichiometric
Lye excess
Temperature .... °C
(speed)
Type of mixer
(speed)
Type of mixer
Peanut, corn, ses- 282 85-95 0.1 Knife 3N-5N 40-60 Knife 4-5N 5-7N 25-40 Disc or 85-95 4N 0.5-1 Knife 10 Knife 3-5
ame, safflower, (high- (high) knife (low)
00-02-11
sunflower, lin- est) (high)

seed, rapeseed*
Rapeseed** 308 " " " " " " " " " " " " " " " " "
Palm 256 85-95 0.025- " - - - " " " " - - - - " " "
0.05 or external
USM***
Palm-kernel 200 " " " - - - 2N 2N 10-25 Disc (idle - - - - " " "
or low)
Coconut 200 " " " - - - " " " - - - - " " "
Hardened oils, - - - - - - - 1N - 0.5-2 " - - - - " " "
bleached oils
Fish, tallow, lard 282 85-95 0.025- - - - - 4-5N 5-7N 20-35 Disc - - - - " " "
and other realted 0.05
oils
Olive 282 " " " - - - " " 25-50 - - - - " " "
Rice bran 282 " 0.05- " - - - 4-5N 4-7N 25-40 Disc or 85-95 4N 0.5-1 Knife " " "
0.2 external (low or
USM***) high)
Cotton seed, 282 70 0.025- " 3-5N 40-70 Knife 3-5N 5-7N 30-50 Disc or " 4-7N " " " " "
kapok 0.1 (high) knife
(high)
*) = low euric acid rapeseed
**) = high euric acid rapeseed
***) = Ultra Short-Mix LOG SHEET 1 R.1
37
38 00-02-11 Book No: MA 0901

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Molecular weight of fatty acids: 282
3UHWUHDWPHQWZLWKSKRVSKRULFDFLG
With some cottonseed oils, pretreatment will improve the colour and the sta-
bility of the refined oil. In some cases, when separating difficulties occur,
pre-treatment may be helpful
Temperature: 65-75°C
Strength of acid: Concentrated
Amount of acid: About 0.1% of oil by volume
Mixing: Mixer at high speed
1HXWUDOL]LQJ
Strength of lye: FFA < 5%: lye of about 4 N
FFA > 5%: lye of about 7 N
Lye excess: 10-50% of stoichiometric quantity
Mixing: Knife or disc mixer at high speed
Bowl flush water: 25-100 l/h
5HUHILQLQJ
With some cottonseed oils, the best de-
colorizing in the re-refining stage is ob-
tained at a fairly low temperature, e.g.
70°C; in other cases a high temperature is
better. Therefore the optimum refining
temperature for a cot-tonseed oil should
to be determined by trials at the start.
Strength of lye: The strength of lye must be chosen with
reference to the crude oil quality and the
requirements as to colour of the refined
oil. Lye strengths of 2-7 N are normally
suitable. If a lye of 12 Bé is used, it is of-
ten advisable to add about 100 water-free
sodium carbonate per cu. m. in order to
minimize the losses.
Book No: MA 0901 00-02-11 39

Amount of lye: For weak lye (up to 4 N) 1-3% of oil by

volume.
For strong lye 0.5-2% by volume
Mixing: Knife mixer at high or medium speed
Bowl flush water: 5-10% of oil by volume
:DVKLQJ
Amount of water: 10% of oil by volume
Mixing: Mixer running at medium speed
40 00-02-11 Book No: MA 0901

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Molecular weight of fatty acids: for coconut oil: 200

for palm-kernel oil: 200
Normally not required.
1HXWUDOL]LQJ
Strength of lye: Use about 2 N. 3-7 N must be avoided
Mixing: Disc mixer immobile or at lowest speed.
When lye of 7 N is used, it is sometimes
advisable to use the Ultra-Short Mixer.
Lye temperature: The lye ought to be preheated to about
90°C.
When lye of 7 N is used it is advisable to
add about 70 kg of anhydrous sodium
carbonate per cu. m of lye in order to
minimize the losses In this case the lye
excess should be reduced.
5HUHILQLQJ
:DVKLQJ
Mixing: Mixer at low speed
Book No: MA 0901 00-02-11 41

42 00-02-11 Book No: MA 0901

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Molecular weight of fatty acids: 282 (except rapeseed oil) n n

Molecular weight of rapeseed 308 (high erucic acid type)
oil:
Treatment of the oil with phosphoric acid will in most cases improve quality
and at the same time minimize the losses.
Amount of acid: 0.05 - 0.20% of oil by volume
1HXWUDOL]LQJ
Strength of lye: FFA < 5%: lye of about 4 N
FFA > 5%: lye of about 7 N
Mixing: Knife mixer at medium or high speed
5HUHILQLQJ
Soybean and rapeseed oil are normally re-refined. Whether the other oils
should be re-refined or not will depend on the quality of the crude oil.
Strength of lye: 2 - 4 N is normally suitable. It is often ad-
visable to add about 100 kg anhydrous
sodium carbonate per cu.m lye in order to
minimize the losses.
Mixing: Knife mixer at medium or high speed
Book No: MA 0901 00-02-11 43

:DVKLQJ
Mixing: Mixer at medium or high speed
44 00-02-11 Book No: MA 0901

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The quality of crude linseed oil varies very much with the origin, the manner
of extraction, and other factors. The quality requirements of the refined oils
also vary according to the field of application. Therefore, the refining method
can be quite different in different cases.
For cold-pressed linseed oil, water degumming is recommended to obtain a

break-free oil, i.e. with no trace of precipitation in a sample of oil heated to
300°C.
In the case of hot-pressed or extracted oil, water degumming does not improve
the quality sufficiently with respect to beak test and colour. In this case treat-
ment of the oil with phosphoric acid followed by lye treatment to neutralize
the mineral acid and water washing will give a better degumming effect. If a
high quality linseed oil is desired, for example, for producing stand oil or alkyd
resin, degumming alone is generally not sufficient. The method to choose is
treatment with concentrated phosphoric acid followed by complete neutraliza-
tion of both the mineral acid and the free fatty acids and water washing.
The table below shows results obtained by the different treatments of hot-
pressed linseed oil.
Treatment Percentage of phos- Break test

phatides (P x 25.4)
Crude oil 1.3 Break
Degummed by water 1.0 Break
Degummed by phos- 0.15 No break
phoric acid
Neutralized without 0.6 No break
phosphoric acid
Treated by phosphoric 0.01 No break
acid and neutralized
:DWHUGHJXPLQJ:
Amount of water: 0.5 - 2% by volume, depending on the
phosphatide content.
Mixing: Mixer at medium speed.
Book No: MA 0901 00-02-11 45

'HJXPPLQJZLWKSKRVSKRULFDFLG
Amount of acid: 0.05 - 0.4% of oil by volume
Strength of lye: 0.5 - 0.7N. Lye of a higher strength can
be used but in that case it is necessary to
flush the separator bowl with water in or-
der to prevent clogging.
Amount of lye: To pH 5-6 (indicator paper) in the aque-
ous phase from the separator. Due to the
buffering effect of the phosphatides and
the varying amount of phosphoric acid
and lye concentration it is impossible to
give figures for the quantity of lye.
Mixing: Mixer at low speed or stopped.
The degummed oil is then washed with water in the same way as described
below.
1RWH
If too little lye is used for neutralizing the mineral acid (i.e. if the pH in the
aqueous phase is lower than 5), the removal of the gums will be incomplete,
and if too much lye is used (i.e. if the pH in the aqueous phase is higher than
6), some free fatty acids will be neutralized, which gives higher losses.
&RPSOHWHQHXWUDOL]DWLRQLQFOXGLQJSKRVSKRULFDFLGSUH
WUHDWPHQW
3KRVSKRULFDFLGSUHWUHDWPHQW
Strength of phosphoric acid: Concentrated
Amount of phosphoric acid: 0.05 - 0.20% of oil by volume.
Mixing: Mixer at high speed.
1HXWUDOL]LQJ
Strength of lye: About 20°Bé
Lye excess: 20-40%
Mixing: Mixer at low or medium speed
46 00-02-11 Book No: MA 0901

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Mixing: Mixer at medium speed
Book No: MA 0901 00-02-11 47

48 00-02-11 Book No: MA 0901

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Treatment of the oil with phosphoric acid will normally improve the oil
quality.
Temperature 85-95°C
Amount of acid: 0.05 - 0.2% by volume, depending on the
crude oil quality.
Mixing: Mixer at high speed.
1HXWUDOL]LQJ
Strength of lye: 4N, containing 80-100 kg anhydrous so-
dium carbonate per cu.m.
Lye excess: 5-15%
Mixing: The lye, heated to about 90°C, is intro-
duced with the mixer running at low
speeed.
5HUHILQLQJ
:DVKLQJ
Mixing: Mixer running at medium speed
Amount of water: 10% oil by volume
1RWH
If a tendency to emulsification occurs, the mixing intensity must be de-
creased. This can be done by removing some of the knives from the mixer
and running this at the lowest speed. In order to get a good washing effect,
the amount of wash water ought to be increased up to 30%.
Book No: MA 0901 00-02-11 49

50 00-02-11 Book No: MA 0901

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Treatment of the oil with phosphoric acid will in some cases improve the
quality and at the same time minimize the losses.
1HXWUDOL]LQJ
Strength of lye: FFA < 5%: lye of about 4N.
FFA > 5%: lye of about 7N.
Mixing: Ultra-Short Mixer. In some cases the disc
mixer can be used alternatively.
Lye temperature: The lye should be preheated to about
90°C when the Ultra-Short Mixer is used.
5HUHILQLQJ
:DVKLQJ
Amount of water: 10% of oil by volume.
Book No: MA 0901 00-02-11 51

52 00-02-11 Book No: MA 0901

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It is often advisable to alkali-refine fatty oils after the hardening operation.

The object of this alkali-refining is to remove traces of the catalysts used in the
hydrogenation and also to neutralize and remove some free fatty acids formed
during the hardening operation. Some oils, e.g. palm oil, are bleached with
large amounts of bleaching earth which also gives rise to a higher acidity.
Normally not used.
1HXWUDOL]LQJ
Strength of lye: 1-2N
Amount of lye: 0.5 - 2% by volume
5HUHILQLQJ
Not required:
:DVKLQJ
Mixing: Mixing at medium speed
Book No: MA 0901 00-02-11 53

54 00-02-11 Book No: MA 0901

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UHODWHGRLOV
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Treatment of the oil with phosphoric acid will in some cases improve the
quality and at the same time minimize the losses.
1HXWUDOL]LQJ
Strength of lye: FFA < 5%: lye of about 4N
FFA> 5%: lye of about 7N
Mixing: Disc mixer at medium or high speed. In
some cases the Ultra-Short Mixer will re-
duce the losses. When the Ultra-Short
Mixer is used the lye should be preheated
to about 90°C. Bowl flush water: 25-100
l/h
5HUHILQLQJ
Normally not required, but may be carried out to obtain a better quality.
Strength of lye: 12-20° Bé is normally suitable. If a lye of
12 Bé is used, it is often advisable to add
about 100 kg anhydrous sodium carbon-
ate per cu.m. lye in order to minimize the
losses.
Amount of lye: 1-3% of oil by volume
Mixing: Knife mixer at medium speed
Book No: MA 0901 00-02-11 55

:DVKLQJ
56 00-02-11 Book No: MA 0901

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FHVV
Book No: MA 0901 00-02-11 57

58 00-02-11 Book No: MA 0901

Book No: MA 0901
Notes: LOG SHEET FOR ALS

MULTI-MIX PROCESS
Capacity of oil (input) : ......................................................................................... Kind of oil :

Pretreatment with acid : Phosphoric acid litres/hour .............................................. Mixer .......... Speed .............. Date :
Neutralizing stage : Strength of lye ................................Lye excess............% Mixer .......... Speed ..............
Rerefining stage : Strength of lye ................................Lye........................... Mixer .......... Speed .............. Operator :
Washing stage : Water .............................................................................. Mixer .......... Speed .............. Operator :
Drying stage : ......................................... Operator :
S T A G E S
NEUTRALIZING REFINING WASHING DRYING
pressure .. kg/km2
Separator outlet
Temperature of lye
flush water
Flowmeter for
flush water
Flowmeter for
water
Temperature of
pressure .. kg/km2
Separator outlet
mm Hg
Vacuum
crude oil
Flowmeter for
FFA in crude oil %
phosphoric acid
pretreatment with
FFA in crude oil after
Temperature of oil
pressure .. kg/km2
Separator outlet
Temperature of oil
%
FFA in oil
Temperature of oil
wash water
Flowmeter for
%
Soap in oil
Time
Temperature of oil
Flowmeter for lye

Flowmeter for lye REMARKS
00-02-11
Max. RECOMMENDATIONS
(31 90 50 E) LOG SHEET 2 REV. 1
59
60 00-02-11 Book No: MA 0901

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 $SSOLFDWLRQ0DQXDO

Book No: MA 0901 00-02-11 13

14 00-02-11 Book No: MA 0901

Alfa Laval Separation AB

For Alkali Refining of Oils & Fats

Book No: MA 0901 00-02-11 15

16 00-02-11 Book No: MA 0901

The following general instructions, based on practical experience, allow an es-

The ALS MM all-hermetic plant has hermetically sealed separators which

Book No: MA 0901 00-02-11 17

18 00-02-11 Book No: MA 0901

The degumming temperature should preferably be approximately 65-75°C. At

P = L x d x FFA x 1000 litres per hour

L = Oil flow in the neutralization stage l/h

d = Specific gravity of the oil at neutralization temperature

M = Molecular weight of the fatty acids

n = Normality of the lye

Normal throughput = 2 000 l/h

Supposed specific gravity d = .9

Book No: MA 0901 00-02-11 19

Coconut oil, palm kernel oil and babassu M = 200

If the concentration of the lye in degrees Bé is known, the normality can be

If refining, for instance, a groundnut oil using a lye of 20°Bé at a throughput

The FFA is determined according to ALS 4031 E 101

a) the free fatty acids

c) the saponification losses, which arise through saponification of neutral

d) the neutral oil lost in the soapstock

20 00-02-11 Book No: MA 0901

The designations used are:

FFA = free fatty acids in the crude oil in per cent

FFA x 100 = FFAR (100 - X) + FFASS x X, or

Book No: MA 0901 00-02-11 21

From these values it was calculated::

total loss 7.6

22 00-02-11 Book No: MA 0901

Excess of lye FFASS Refining Real refining

Book No: MA 0901 00-02-11 23

24 00-02-11 Book No: MA 0901

Book No: MA 0901 00-02-11 25

26 00-02-11 Book No: MA 0901

A re-refining of an oil, as well as a phosphoric acid pretreatment, often im-

The sodium carbonate precipitates the calcium and magnesium compounds as

As an example on re-refining losses the following figures can be considered

Strength of re-refining lye °Bé Re-refining loss, per cent of crude

Book No: MA 0901 00-02-11 27

28 00-02-11 Book No: MA 0901

*) 1 is a bad score and 5 a very good one

Book No: MA 0901 00-02-11 29

30 00-02-11 Book No: MA 0901

Book No: MA 0901 00-02-11 31

32 00-02-11 Book No: MA 0901

Book No: MA 0901 00-02-11 33

34 00-02-11 Book No: MA 0901

Book No: MA 0901 00-02-11 35

36 00-02-11 Book No: MA 0901

G U ID E VAL UES F OR A LK A L I R EF I N I N G OF OI LS / FAT S

FFA ... <3%

FFA ... <3%

sunflower, lin- est) (high)

38 00-02-11 Book No: MA 0901

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