Fat fractionation

A vegetable fat is subjected to dry fractionation, i.e. without the use of solvents or detergents, with a view to obtaining a concrete fraction compatible with cocoa butter in one or two fractionation cycles. In each of these cycles, the fat melted beforehand is seeded with stabilized .beta. or .beta.' crystals thereof, the liquid is progressively cooled and the suspension obtained is pressed by the application of a progressively increasing pressure. The concrete fractions obtained may be used instead of cocoa butter as confectionery fats.

This invention relates to a process for the dry fractionation of a 
vegetable fat capable of crystallizing in several forms at temperatures 
around ambient temperature, to the fractions obtained and to their use. 
Natural fats are complex mixtures of triglycerides of which the composition 
includes solid saturated fatty acids and liquid unsaturated fatty acids 
having different chain lengths. The composition of the fatty acids and 
their distribution within the triglyceride molecules are particular to 
each fat and determine its properties and, in particular, its melting 
behavior. Since natural fats are mixtures, (eutectic) interaction 
phenomena occur within a certain temperature range, modifying the physical 
state of the constituents, the triglycerides being capable in addition of 
crystallizing in several forms. 
Vegetable fats, for example cocoa butter, generally show these crystalline 
polymorphism phenomena around ambient temperature is cases where the 
disaturated-monounsaturated and monosaturated-diunsaturated triglycerides 
are preponderant. Apart from cocoa butter, these fats are not directly 
used in foods because of their plastic character and it has been proposed 
to fractionate them to enable them to be used either as table oil or as 
confectionery fat, for example as a substitute for cocoa butter. 
The confectionery/chocolate industry uses large quantities of cocoa butter 
because of its unique physical properties which are highly valued in that 
industry: it is solid up to 25.degree. C., melts rapidly in a narrow 
temperature range between 35.degree. and 37.degree. C. (particularly in 
the mouth, which produces sensations of melting and taste) and hardens 
rapidly with controllable shrinkage on cooling (which enables it to be 
removed from moulds). Accordingly, consideration has been given to the use 
of other vegetable fats available in greater abundance as a substitute fat 
because the climatic zones in which cocoa can be grown are restricted and 
the supply of cocoa butter is limited. Fats of the type in question have 
to show physical behavior very similar to that of cocoa butter to be 
compatible therewith. With the object of producing such substitutes, 
vegetable fats, particularly palm oil, are industrially fractionated by 
various methods: 
A first method using solvents comprises cooling a solution of the fat in an 
organic solvent, for example acetone, hexane, isopropanol, 2-nitropropane, 
dichlorodifluoromethane, trichlorotrifluoroethane, separating the stable 
.beta. and .beta. crystalline forms required by filtration and eliminating 
the solvent by evaporation. This method may be applied to natural oil, for 
example as described in GB-PS No. 827 172, or to a concrete fraction 
obtained after a first dry fractionation step. To increase the yield of 
table oil whilst at the same time producing a fraction suitable for use in 
confectionery, this method has been applied to an oil that has undergone 
catalytic interesterification (or transesterification), i.e. an internal 
rearrangement of the fatty acids in the triglyceride molecule, for example 
as described in French Patent Application No. 2 427 386. Another process 
described, for example, in U.S. Pat. No. 3 431 116 comprises selectively 
hydrogenating a stearin obtained as by-product in the manufacture of table 
oils from cotton seeds to convert the linoleic acid into oleic acid before 
the fractionation treatment with solvents. Although all these known 
processes enable fractions suitable for use in confectionery to be 
obtained, they have the disadvantage of using chemical agents and/or 
solvents which have to be treated and recycled and also eliminated from 
the fats. This requires heavy installations which are not always available 
in the regions where the starting material is gathered and involves 
considerable energy consumption. 
A second method carried out in aqueous medium is based on the wettability 
of the crystals in the presence of a surfactant which enables an aqueous 
suspension of crystals to be separated from the liquid oil, the crystals 
being subsequently collected by centrifuging. This method has the 
disadvantage of producing a large volume of waste waters. 
A third method comprises dry fractionation. In this method, which is 
described for example in German Patent Application No. 29 16 604, the 
entirely liquid fat is treated in a controlled manner and, after the 
molten mass has been seeded with .beta. crystals of the fat at 45.degree. 
C., the melt is cooled and the crystals formed are filtered. The operation 
is carried out a second time at a lower temperature. This method does not 
prevent the occlusion of part of the liquid fraction in the crystal 
aggregates, which leads either to a fraction that does not have the 
required characteristics or to a low yield at the separation stage. This 
confirms the opinion generally held among experts that it has not hitherto 
been possible to obtain a concrete fraction compatible with cocoa butter 
by dry separation from palm oil in a yield comparable with that obtained 
where solvents are used. 
The present invention seeks to provide a process for the dry fractionation 
of vegetable fats capable of crystallizing in several forms at 
temperatures around ambient temperature which gives concrete fractions 
compatible with cocoa butter in a yield comparable with that obtained by 
fractionation with solvents without having any of the disadvantages 
attending the known processes of aqueous or solvent fractionation. 
The process according to the invention comprises the following steps: 
(a) the pre-refined fat is heated to convert it entirely into liquid form, 
(b) the liquid of step (a) is cooled to a temperature 3.degree. to 
10.degree. C. above its solidification temperature, 
(c) it is then seeded with .beta. or .beta.' crystals obtained from said 
fat or from cocoa butter and stabilized in the required form by storage, 
(d) the suspension of step (c) is progressively cooled at a rate of 
0.5.degree. to 1.5.degree. C. per hour to a fractionation temperature in 
the range from 15.degree. to 35.degree. C. and 
(e) the suspension of step (d) is filtered under a pressure of at least 20 
kg/cm.sup.2 at the fractionation temperature and a concrete fraction 
(C.sub.1) having an iodine value of at most 50 and a fluid fraction 
(F.sub.1) having a higher iodine value than the concrete fraction 
(C.sub.1) are collected, the difference between the iodine value of the 
fraction (C.sub.1) and that of the fraction (F.sub.1) being at least 10, 
and if necessary the sequence of operations from the fluid fraction 
(F.sub.1) is repeated until the desired concrete fraction is obtained. 
The vegetable fats capable of being fractionated in accordance with the 
invention are those which show a crystalline polymorphism around ambient 
temperature, i.e. between 20.degree. and 35.degree. C. Vegetable fats such 
as these, which are known generically as vegetable tallows, include shea 
butter (karite, Butyrospermum parkii or Bassia parkii), sal butter (Shorea 
robusta), Borneo tallow (Shorea stenoptera), kokum butter (Garcinia 
indica), mango kernel butter (Mangifera indica), mowrah fat (Madhuca 
latifolia and Madhuca longifolia), palm oil (Elaeis guineensis), etc. 
The expression "pre-refined fat" means that the fat has been subjected to 
the removal of mucilages to insolubilize the phospholipids, the 
polysaccharides, the gums, the resins, etc. . . . which are separated by 
centrifuging, 
neutralization to eliminate most of the free fatty acids in the form of 
soaps to a free fatty acid content of less than 0.2% and preferably less 
than 0.1% by weight. The fractionated fat is preferably refined in known 
manner by the following successive additional operations: 
decoloration by passage in molten form over active carbon or other 
adsorbents, for example bleaching earths based on activated aluminium 
silicate, such as montmorillonite or bentonite, and filtration to remove 
the chlorophyll and the carotenoid pigments and 
deodorization by stripping with steam in vacuo at a temperature below 
260.degree. C. and preferably at a temperature below 200.degree. C. 
All the pre-refining and refining steps have to be carried out in such a 
way as to avoid isomerization of the triglycerides.

SCHEME 1 
This embodiment comprises a single fractionation cycle and is particularly 
suited to vegetable tallows, such an mango butter, sal butter, mowrah fat 
or kokum butter, which are rich in saturated and monounsaturated acids and 
which have a particular configuration of the triglycerides characterized 
by a high percentage of 2-monounsaturates and a low percentage of 
trisaturates. This composition makes them fairly similar to cocoa butter 
from the chemical and physico-chemical viewpoints. 
As indicated in Table I below, which gives their composition in % of the 
fatty acids and their 2-monounsaturated triglycerides in % of the 
triglycerides, these fats contain more linoleic and oleic acid and, 
correlatively, more monosaturates-diunsaturates than cocoa butter. The 
fractionation described hereinafter reduces the content of these 
triglycerides in the concrete fraction (C.sub.1), bringing its 
physico-chemical properties into line with those of cocoa butter and 
making it compatible with cocoa butter. The fraction (1) may therefore be 
used as an ingredient of a cocoa butter substitute in chocolate. 
TABLE I 
______________________________________ 
Mango Sal Mowrah Kokum 
______________________________________ 
Palmitic acid 
8-9 6-7 16-24 2-3 
Stearic acid 
40-42 42-44 20-25 52-58 
Oleic acid 40-42 38-42 43-45 38-40 
Linoleic acid 
5-8 4-7 9-14 2-3 
2-monounsaturates 
46-50 64-79 26-30 73-78 
______________________________________ 
The fractionation cycle comprises the following steps: 
(1a) The refined fat is heated to convert it entirely into liquid form, 
i.e. to a temperature of from 60.degree. to 80.degree. C., depending on 
the fat used, for example to around 60.degree. C. for sal butter and to 
around 70.degree. C. for mango butter. 
(1b) The liquid fat is cooled to a temperature 5.degree. to 10.degree. C. 
above its solidification temperature, i.e. generally to 
30.degree.-45.degree. C. 
(1c) The cooled liquid fat is seeded with stabilized .beta. crystals to 
direct crystallization towards the formation of a concrete fraction 
(C.sub.1) of high melting point or stearin. The .beta. crystals consist 
essentially of saturated fatty acid triglycerides. They constitute the 
polymorphic form of those triglycerides which is stable and has a higher 
melting point or a higher melting range. The first seed crystals may be 
obtained by straightforward crystallization of the molten fat at 
30.degree.-35.degree. C. and filtration. 
Once production has started, .beta. crystals emanating from the stearin 
(C.sub.1) obtained during the fractionation of a preceding batch may be 
used for seeding a batch. These .beta. crystals may emanate from cocoa 
butter or preferably from fractionated fat. Fractionation may have been 
carried out by the dry method or using a solvent, the solvent having been 
subsequently eliminated. Whatever their origin, the .beta. crystals will 
preferably have been stored for at least 4 weeks at 30.degree.-35.degree. 
C. The crystals are added in a quantity of from 0.05 to 0.2% by weight 
either as such or in the form of a 5-15% by weight suspension in the 
corresponding fluid fraction (F.sub.1). The suspension is slowly stirred 
in order thoroughly to mix the crystals. 
(1d) The suspension obtained in step (1c) is progressively cooled at a rate 
of 0.5.degree. to 1.5.degree. C./hour and preferably at a rate of 
1.degree. C./hour to facilitate the formation of coarse crystals down to 
the fractionation temperature which is preferably in the range from 
20.degree. to 35.degree. C. Alternatively, the suspension may be left 
standing for 8 to 15 hours at the seeding temperature and then cooled 
under the conditions described above. The suspension may also be cooled as 
described above and then left standing for 8 to 15 hours at the 
fractionation temperature. The same operation may be carried out at an 
intermediate temperature by interrupting cooling. 
Crystallization is carried out either in tanks or on trays. 
(1e) Fractionation is carried out by means of a hydraulic press, for 
example a frame press. To this end, the suspension obtained in step (1d), 
which has assumed a paste-like consistency due to the crystal aggregates, 
is transferred to cloths or "press bags" which are arranged in stacks, 
each bag being separated from the adjacent bags by metal plates provided 
with drainage grooves. Alternatively, it is possible to use a 
semicontinuous automatic press of the type used for separating cocoa 
butter from the nibs, suitably modified for example, by replacing the 
metal filters by cloths having a mesh width of at most 2 microns. 
In this step, the pressure should be applied in stages and should reach a 
level of at least 20 kg/cm.sup.2 to obtain as complete as possible an 
expulsion of the fluid fraction. Preferably, the pressure is increased in 
stages of around 6-7 kg/cm.sup.2, the pressure applied being maintained 
for at least 5 minutes, to at least 30 kg/cm.sup.2, for example to 45 
kg/cm.sup.2, the maximum pressure being maintained for 1-2.5 hours. The 
operation lasts at most 1.5 to 3 hours. 
Depending on the composition of the fat used, the concrete fraction 
(C.sub.1) obtained represents from 10 to 90% by weight of the starting fat 
and its iodine value is in the range from 18 to 50. The iodine value 
depends upon the degree of unsaturation of the fatty acids contained in 
the triglycerides and is the number of grams of iodine fixed by 100 g of 
fat. In the present case, it indicates the degree of separation of the 
concrete fraction from the fluid fraction. The fluid fraction (F.sub.1) or 
olein has an iodine value of from 45 to 70. 
The fluid fraction (F.sub.1) may be used in foods either as such or after 
slight hydrogenation, for example as table oil. 
SCHEME 2 
This embodiment comprises two successive fractionation cycles and is 
particularly suited to palm oil which has a comparatively higher content 
of triunsaturated triglycerides having a high melting range. Table II 
below gives its composition in % of the fatty acids and also the number of 
2-monounsaturated and trisaturated triglycerides in % of the 
triglycerides. 
TABLE II 
______________________________________ 
Palmitic acid 41-49 
Stearic acid 4-6 
Oleic acid 27-53 
Linoleic acid 5-10 
2-monounsaturates 
40-45 
Trisaturates 6-9 
______________________________________ 
In this case, the fractionation of step 1e) of the first cycle (according 
to scheme 1) makes it possible to separate a concrete fraction (C.sub.1) 
having an iodine value of 18-24 in a yield of 10 to 12% by weight. This 
fraction (C.sub.1) has a melting range of 45.degree.-55.degree. C. It may 
be used for hardening shortenings or margarines or may even form part of 
cosmetic or pharmaceutical products. 
The fluid fraction (F.sub.1) undergoes a second fractionation cycle under 
the following conditions: 
(2a) The fluid fraction (F.sub.1) having an iodine value of greater than 55 
and preferably from 56 to 56.5 represents from 90 to 93% by weight of the 
starting fat. The starting fat is heated to a temperature of from 
40.degree. to 60.degree. C. and preferably to a temperature of 
approximately 45.degree. C. to convert it completely into liquid form. 
(2b) The liquid obtained in step (2a) is cooled to a temperature around 
30.degree. C. which is 3.degree.-5.degree. C. above the solidification 
temperature of the fraction (F.sub.1). 
(2c) The cooled liquid is seeded with stabilized .beta.' crystals to direct 
crystallization towards the formation of a desired intermediate concrete 
fraction (C.sub.2). The .beta.' crystals consist essentially of 
2-monounsaturated triglycerides which may be obtained by the 
crystallization of a fraction (F.sub.1) heated to approximately 45.degree. 
C. and cooled to a temperature of 20.degree.-30.degree. C., followed by 
filtration. Once production has started, .beta.' crystals emanating from a 
fraction (C.sub.2) of a preceding batch will preferably be used for 
seeding a batch. Preferably, these crystals will have been stabilized by 
storage for at least 4 weeks at 20.degree.-30.degree. C. They are added as 
such in a quantity of from 0.05 to 0.2% by weight or in the form of a 
5-15% by weight suspension in the corresponding fluid fraction (F.sub.2) 
with slow stirring. 
(2d) The suspension obtained in step 2c) is cooled at a rate of 
0.05.degree.-1.5.degree. C./hour and preferably at a rate of 1.degree. 
C./hour to 15.degree.-20.degree. C., preferably after it has been left 
standing for 8 to 15 h at the seeding temperature. 
The suspension is then left standing for 72-120 hours at 
15.degree.-20.degree. C. and preferably at 15.degree.-18.degree. C. 
(2e) The suspension is fractionated as indicated above in reference to 
scheme 1 under the following particular conditions: the pressure is 
increased in stages of 6-7 kg/cm.sup.2, the pressure applied in each stage 
being maintained for at least 5 minutes and preferably for 10 to 15 
minutes. The maximum pressure is at least 30 kg/cm.sup.2 and preferably 45 
kg/cm.sup.2 and is maintained for at least 1 h and preferably for around 2 
h. 
In the present case, it is important to ensure that the temperature does 
not exceed 18.degree. C., particularly at the beginning of fractionation. 
This is because excessive heating during pressing could result in partial 
melting of the crystals which would in turn result in a reduction in yield 
and would promote the subsequent appearance of undesirable crystal forms. 
The foregoing procedure gives a concrete fraction (C.sub.2) having 
physico-chemical characteristics very similar to those of cocoa butter in 
a global yield of around 30% by weight, based on the fat used, and a fluid 
fraction (F.sub.2) having an iodine value of 65-68. 
In one preferred embodiment, it is possible to improve the global yield of 
concrete fraction (C.sub.2) to 33% by leaving the fluid fraction (F.sub.2) 
to crystallize for 2 to 3 days at approximately 15.degree. C. and 
recovering a concrete fraction (C.sub.3) by pressing under the conditions 
applied to the fraction (F.sub.2); the fraction (C.sub.3) may be added to 
the following batch (F.sub.1) in step 2e). 
The concrete fraction (C.sub.2) melts at body temperature and, accordingly, 
has many uses in confectionery and biscuit manufacture as a substitute for 
cocoa butter, in cosmetics, for example as a cream, lotion or lipstick 
base, and in the pharmaceutical field as a medicament support, for example 
as a suppository. In chocolate manufacture, it may be used on its own or 
in combination with a vegetable tallow in a fat composition intended as a 
substitute for cocoa butter. In a fat composition such as this, the 
vegetable tallow will preferably be in the form of one or more concrete 
fraction(s) (C.sub.1), for example sal butter or mango butter. The 
concrete fraction(s) (C.sub.1) will advantageously represent from 10 to 
60%, for example 50%, by weight of the composition. 
The fluid fraction (F.sub.2) may be used as table oil, more particularly as 
frying oil. 
The invention is illustrated by the following Examples in which the 
percentages are percentages by weight. In the Examples, I.V. is the iodine 
value as determined by titration with sodium thiosulfate of the iodine 
released by the addition of potassium iodide to a solution containing the 
fat and iodine chloride (reagent) by comparison with a reference solution 
of the reagent without the fat (Method 2.205, I.U.P.A.C. "Standard Methods 
for the Analysis of Oils, Fats and Derivatives", Pergamon Press, 6th 
Edition, 1979). 
In the following Comparison Example, an iodine value balance was made. This 
operation comprises comparing the I.V. of the starting fat with the 
weighted sum of the I.V.'s of the concrete fraction (C) and the fluid 
fraction (F) obtained: 
I.V.=I.V.sub.C..times.C+I.V.sub.F..times.F, C and F being, respectively, 
the percentages of concrete fraction and fluid fraction obtained by 
fractionation. 
The suitability of a concrete fraction (C.sub.1) or (C.sub.2) to be mixed 
with cocoa butter is verified 
by studying its behavior on cooling, giving its solidification point, under 
clearly defined conditions (Shukoff's method, reference temperature 
0.degree. C., I.U.P.A.C., Method 2.132), 
by determining its melting curve, giving the solid fat index (S.F.I.) or 
the percentage of solid fat present in the partially melted fat at a given 
temperature, by pulsed NMR (nuclear magnetic resonance of the proton) 
(I.U.P.A.C., 1st Supplement, 1982, Method 2.323) or by dilatometry 
(I.U.P.A.C., 6th Edition, 1979, Method 2.141), 
by its use in chocolates in conjunction with cocoa butter either on its own 
or in admixture with another concrete fraction. 
The following Comparison Example shows the yields and I.V.'s obtained for 
the fraction (C.sub.2) of palm oil in accordance with the present 
invention (A) by comparison with the fractionation of palm oil with hexane 
(B) and acetone (C), respectively, under the following conditions: 
(B) The fluid fraction (F.sub.1) emanating from fractionation in accordance 
with scheme 2 above is heated to 45.degree. C. and dissolved in hexane in 
a ratio by weight of hexane to olein of 3:1, after which the solution is 
cooled to -10.degree. C. and left to crystallize for 24 h at -10.degree. 
C., the suspension is stirred for 5 minutes at 3-4 r.p.m. 4 h before the 
separation of the crystals and the crystals are filtered using a frame 
filter. The crystals are collected and melted and the solvent evaporated. 
(C) The procedure is as in (B) except that a ratio by weight of acetone to 
fluid fraction (F.sub.1) of 6:1 is used and the suspension is crystallized 
for 24 h at 5.degree. C. 
Where solvents are used, as in (B) and (C) above, separation of the 
crystals may be carried out in any apparatus suitable for liquid/solid 
separation without the application of pressure, for example in a filter or 
a centrifugal separator. 
EXAMPLE 1 
Preparation of palm olein (F.sub.1) 
100 kg of palm oil freed from mucilages and neutralized (containing at most 
0.1% of free fatty acids), I.V. 53, are heated to 60.degree. C. and then 
cooled to 45.degree. C. 
The oil is seeded at 45.degree. C. with 100 g (0.1%) of .beta. crystals of 
concrete palm fraction (stearin) prepared as described hereinafter. After 
it has been transferred to a tank, the suspension is progressively cooled 
to 30.degree. C. in 12 h. The suspension of the crystals formed is 
filtered in a frame press. The pressure cycle used is 2 h at 30.degree. 
C., the maximum pressure of 30 kg/cm.sup.2 being reached in 35 mins. at 
intervals of 7 mins. 90 kg of clear fluid fraction (olein F.sub.1) having 
an I.V. of 56-56.5 and 10 kg of a concrete fraction (stearin C.sub.1) 
having an I.V. of 22-24, representing 10% of the oil used, are collected. 
The iodine value of the stearin (C.sub.1) depends upon the separation 
efficiency: thus, a low iodine value is indicative of a high separation 
yield. A precise iodine value for the olein (F.sub.1) is merely indicative 
of orientation of the crystallization process without detriment to the 
yield. 
Preparation of the concrete fraction (C.sub.2) 
90 kg of the preceding fraction (F.sub.1) are heated to 45.degree. C. and 
seeded with 90 g (0.1%) of stabilized .beta.' crystals (fraction C.sub.2) 
prepared as described above. After the crystals have been mixed with the 
liquid, the suspension is cooled for 10 h to 26.degree.-27.degree. C. It 
is then transferred in batches of 25 kg onto trays at that temperature, 
cooled to 18.degree. C. in 8 h and left to crystallize for 4 days at 
18.degree. C., care being taken to ensure that the temperature of the 
trays stays between 17.degree. and 19.degree. C. 
The suspension is then transferred to press bags which are stacked in a 
hydraulic press and collectively subjected to a pressure increasing 
progressively in stages of 6-7 kg/cm.sup.2 every 15 minutes to 20 
kg/cm.sup.2, i.e. in 45 minutes, which corresponds to a reduction of the 
charge of around 30%. The duration of the increase in pressure naturally 
depends upon the type of press used and its geometry. The pressure is then 
increased in stages of 6-7 kg/cm.sup.2 every 15 minutes to 45 kg/cm.sup.2, 
i.e. in 1 h and pressing is continued at that pressure for 2 h. A concrete 
fraction (C.sub.2), I.V. 36-38, yield 30%, and a fluid fraction (F.sub.2) 
having an I.V. of 65-67 are obtained. 
Preparation of .beta. and .beta.' crystals of palm stearin 
The .beta. seed crystals are prepared by tempering the palm oil for 2 weeks 
at 30.degree.-35.degree. C. The crystals formed are separted by filtration 
and left standing for 2 weeks at 30.degree.-35.degree. C. 
To prepare the .beta.' seed crystals, the fluid fraction (F.sub.1) is 
tempered for 2 weeks at 20.degree.-28.degree. C. The crystals formed are 
separated by filtration and left standing for 2 weeks at 
20.degree.-28.degree. C. 
Once production has started, part of the stearin fractions (C.sub.1) and 
(C.sub.2), respectively, may be removed from the following batches and 
tempered as indicated above for at least 2 weeks in order to collect 
stabilized .beta. and .beta.' crystals, respectively, the crystals then 
being left standing for 2 weeks. 
Comparison Example 
A refined palm oil having an I.V. of 53 is fractionated 
(A) by the method of Example 1, 
(B) as previously described, the last step using hexane, 
(C) as previously described, the last step using acetone, 
(D) in accordance with Example 1 of German Patent Application No. 29 16 
604. 
The yields based on the fat used and the I.V's of the various fractions are 
shown in Table III below: 
TABLE III 
__________________________________________________________________________ 
A B C D 
I.V. 
Yield % 
I.V. 
Yield % 
I.V. 
Yield % 
I.V. 
Yield % 
__________________________________________________________________________ 
Starting palm oil 
53 53 53 53.sup. 
1st pressing 
or filtration for D 
Stearin (C.sub.1) 
22-24 
10 22-24 
10 22-24 
10 31.sup.1 
16.7 
Olein (F.sub.1) 
56.5 56.4 56.5 58.sup.2 
2nd pressing 
or filtration for B, C & D 
Stearin (C.sub.2) 
36-38 
33 38-40 
35 36 40 33.sup.3 
52 
Olein (F.sub.2) 
65-67 68 70 60.sup.3 
48 
Global yield .sup. 30.sup.4 
32 36 43 
__________________________________________________________________________ 
Legend: 
.sup.1 The I.V. of the stearin is too high and shows that a certain 
quantity of olein (F.sub.1) is still present due to the poor separation 
.sup.2 On the basis of the yields indicated, evaluation of the I.V.'s 
gives an I.V. of 58 for the olein (F.sub.1). 
.sup.3 On the basis of the I.V.'s indicated, the I.V. balance gives: 58 = 
33 .C + 60 .F with C + F = 1, i.e. C = 0.07 In fact, only 7% of stearin 
(C.sub.2) having an iodine value of 33 is obtained. 
.sup.4 The global yield may be increased to 33% if the olein (F.sub.2) is 
left to crystallize for 2 to 3 days at 15.degree. C. A concrete fraction 
(C.sub.3) (I.V. 52-53, yield 15%) and a fluid fraction (F.sub.3) (I.V. 
67-68, yield 85%) are thus recovered by pressing under the conditions 
described in Example 1 in reference to the preparation of the concrete 
fraction (C.sub.2). The concrete fraction (C.sub.3) may be added to the 
following batch (F.sub.1). 
Table IV below shows the S.F.I. the Shukoff values of the concrete 
fractions (C.sub.2) obtained by methods A, B and C compared with those 
obtained for cocoa butter. 
TABLE IV 
__________________________________________________________________________ 
Concrete 
Concrete 
Concrete 
fraction 
fraction 
fraction 
(C.sub.2) acc. 
(C.sub.2) acc. 
(C.sub.2) acc. 
Cocoa 
to A to B to C butter 
__________________________________________________________________________ 
I.V. 38 38-40 
36 36 
S.F.I. (%) at temperature (.degree.C.) 
25 54 52 62 63 
30 32 25 35 41 
35 5 2 5 0 
40 0 0 0 
Shukoff cooling curve (0.degree. C.) 
Minimum temperature (.degree.C.) in time (mins) 
18.0 
27 
14.7 
37 
18.4 
30 
17.7 
39 
Maximum temperature (.degree.C.) in time (mins.) 
20.6 
50 
18.3 
70 
22.1 
52 
20.6 
60 
.DELTA. temperature (.degree.C.) 
2.6 3.6 3.7 2.9 
.DELTA. time (mins.) 23 33 22 21 
.DELTA. temperature/.DELTA. time (.degree.C./mins.) 
0.11 0.11 0.17 0.14 
__________________________________________________________________________ 
EXAMPLES 2-3 
The analytical values for these Examples (S.F.I., yield, I.V., Shukoff 
cooling curve) are set out in Table V below. 
2. 100 kg of refined sal butter are heated to 60.degree. C. and, after 
cooling to 30.degree. C., are seeded with 1 kg of a suspension containing 
10% of .beta. crystals of sal stearin in liquid sal olein, these crystals 
having been stabilized as indicated in Example 1. The suspension obtained 
is left standing for 12 h at 30.degree. C. and cooled to 26.degree. C. in 
4 h. The suspension is fractionated in 2 h as described in Example 1 in 
reference to the preparation of the fraction (F.sub.1), except that the 
operation takes place at 26.degree. C. and the maximum pressure is 35 
kg/cm.sup.2. 80 kg of a concrete fraction (C.sub.1) are obtained. 
3. 1 kg of refined mango kernel butter is heated to 68.degree. C., cooled 
to 30.degree. C. and seeded with 1 g (0.1%) of .beta. crystals of mango 
stearin stabilized as described in Example 1. The suspension is cooled for 
5 h to 23.degree. C. and then kept for 15 h at 23.degree. C. The 
suspension is fractionated in 2 h as described in Example 1 in reference 
to the preparation of the fraction (F.sub.1), except that the operation 
takes place at 23.degree. C. and the maximum pressure is 36.5 kg/cm.sup.2. 
670 g of a concrete fraction (C.sub.1) are obtained. 
TABLE V 
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Example 2 3 
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S.F.I. at 
25 (.degree.C.) 74 45 
30 69 37 
35 41 9 
40 0 0 
Yield of stearin (%) 78 70 
I.V. stearin 33 42 
olein 45 61 
Shukoff cooling curve (0.degree. C.) 
Minimum temperature (.degree.C.) in time (mins.) 
18.8 43 18.0 32 
Maximum temperature (.degree.C.) in time (mins.) 
25.1 51 26.4 44 
.DELTA. temperature (.degree.C.) 
6.3 8.4 
.DELTA. time (mins.) 18 12 
.DELTA. temperature/.DELTA. time (.degree.C./mins.) 
0.35 0.7 
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EXAMPLE 4 
4 chocolate masses are prepared from the following ingredients. 
The foreign fat consists of: 100% of concrete fraction (C.sub.2) of Example 
1 (I); 10% of concrete fraction (C.sub.1) of Example 2/90% of concrete 
fraction (C.sub.2) of Example 1 (II) and 40% of concrete fraction 
(C.sub.1) of Example 2/60% of concrete fraction (C.sub.2) of Example 1 
(III). 
______________________________________ 
Milk Plain 
Ingredient, % by weight 
chocolate 
chocolate 
______________________________________ 
Sugar 43.3 48.7 
Nibs (Ghana) 12.0 45.2 
Milk powder (26% fat, based on 
27.5 -- 
dry matter) 
Cocoa powder (12-14% cocoa butter, 
-- 0.7 
based on dry matter) 
Deodorized cocoa butter 
11.8 -- 
Foreign fat (corresponds to approx. 
5.0 5.0 
16-18% of the total fat) 
Lecithin 0.4 0.4 
Vanillin (traces) -- -- 
______________________________________ 
The various ingredients, except the lecithin, the vanillin and some of the 
fat, are mixed at 40.degree. C. in such a way that the mixture contains 
from 27 to 29% by weight of fat, after which the mixture is finely ground 
in a roll mill. The ground mixture is then conched for 24 h at 55.degree. 
C., the remainder of the fat being added in portions. The vanillin and 
then the lecithin are added just before the end of conching. After 
conching, the milk chocolate is cooled to 27.degree. C. and the plain 
chocolate to 29.degree. C., followed by tempering at 29.degree. C. and at 
30.degree.-31.degree. C., respectively. 
The compatibility of the foreign fat with the cocoa butter is evaluated by 
the following tests: 
Mould releasability 
Metal moulds are filled with 100 g of the tempered chocolate and placed in 
a refrigerated chamber at 4.degree. C. After about 5 mins, the moulds are 
inverted and vibrated and the time (mins.) which the chocolate takes to 
separate from the mould is recorded. 
Fat bloom 
Fat bloom is the appearance of a whitish layer of fat at the surface of the 
chocolate. This undesirable phenomenon occurs more readily the more the 
foreign fat interacts with the cocoa butter. It is thus a good indication 
of its compatibility. The chocolate is subjected to 30 tempering cycles 
comprising 12 h at 15.degree. C., then 12 h at 28.degree. C. and finally 
another 12 h at 15.degree. C. and the results obtained are recorded on a 
scale of 1 to 5 as follows: 
1=no change (shiny appearance) 
2=slightly clouded 
3=clouded 
4=fat bloom 
5=considerable bloom 
The number of tempering cycles after which there is a change of 1 unit on 
the scale is also noted. 1/18, 2/6, 3/6 for example signifies that, after 
18 cycles, the sample has a rating of 2, after 6 more cycles it moves onto 
3 and remains at 3 after 30 cycles. 
The results are shown in Table VI below: 
TABLE VI 
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Milk chocolate Plain chocolate 
Mould Mould 
separation separation 
Sample 
Whitening time (mins.) 
Whitening 
time (mins.) 
______________________________________ 
I 1/30 26.5 1/24;3/6 19.3 
II 1/30 31.3 1/24;3/6 21.6 
III 1/30 27.9 1/18;2/6;3/6 
20.6 
Cocoa 1/30 25 1/20;2/4;3/6 
20 
butter 
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