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Патент USA US3052710

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Sept. 4, 1962
Filed June 24, 1959
IL _ _
@ugm ‘DMZ-few
Patented Sept. 4, 1962
possible, and also, as few liquid component particles as
possible are to be occluded by the crystals. As is well
known, fatty materials possess a substantially poorer
crystallization capacity than many other organic com~
Hans Waldmann, Dusseldorf-Ellen and Werner Stein,
pounds. The higher melting compounds, present in a
Dusseldorf-Holthausen, Germany, assignors to Henkel
molten mixture of fatty materials having different melt
& Cie. G.rn.b.H., Dusseldorf-Holthausen, Germany, a
corporation of Germany
ing points, crystallize out very slowly and at that they
Filed June 24, 1959, Ser. No. 822,663
have the tendency to a higher degree than many other
Claims priority, application Germany July 3, 1958
organic compounds to build into the crystal structure 10W
8 Claims. (Cl. 260-419)
10 er melting materials or to incorporate mechanically such
particles in the course of the crystal growth.
This invention relates to improvements in the separa
An object of this invention is an improved vprocess
tion of mixtures of fatty acids. It more particularly re
for the separation of fatty acid and fatty acid ester mix
lates to the separation of these mixtures into components
tures into components of different melting points.
of different melting points.
The foregoing, and still further objects of the inven—
Fatty acids of natural or synthetic origin are usually 15
tion, will become apparent from the following description
obtained by way of mixtures of fatty acids, the individual
read in conjunction with the drawings, in which
components of which differ from one another by their
FIG. 1 is a diagrammatic vertical section of an em
melting points. Separation of these fatty acids from
bodiment of a cooling apparatus, useful in the practice
their mixtures has hitherto entailed certain difficulties, dis
of the invention;
advantages and drawbacks. Such separation was usually
FIG. 2 is a diagrammatic vertical section of a further
embodiment of a cooling apparatus, useful in the prac
by filtering, use of hydraulic presses, etc.
tice of the invention; and
It has additionally been suggested in US. Patent No.
FIG. 3 is a diagrammatic vertical section of a further
2,800,493 to e?ect the separation of fatty acid mix
tures into their components or component cuts by form 25 embodiment of a cooling apparatus, useful in the practice
of the invention, in which the cooling vessels also serve
ing a dispersion of the fatty acid material in an aqueous
accomplished by the use of organic solvents, separation
solution containing a surface-active material at a tem
as intermediate containers.
In accordance with the invention it has now been found
perature at which the mixture contains solid and liquid
that in the process of separating mixtures of ‘fatty acid
components. In this dispersion, the surface-active ma
terial serves to wet the surface of the particles of the 30 materials, the components of which differ from one an
other by their melting points by forming a dispersion of
solid fatty acid or ester and displace the liquid acid or
the fatty acid material in an aqueous solution containing
ester therefrom, so that there results a continuous aqueous
a surface-active material at a temperature at which the
phase with discrete separate particles of the solid and
mixture contains solid and liquid components and where
liquid components. Thereafter, the dispersion is sepa
rated by a layer formation into a speci?cally heavier phase 35 after the dispersion is separated by a layer formation into
a speci?cally heavier phase composed of the aqueous so~
composed of the surface-active material containing sus
lution of the surface-active material containing suspended
pended particles of the solid component and a speci?cally
particles of the solid component and a speci?cally lighter
lighter phase composed of the liquid components. The
separation of the dispersion into the two phases is then
phase composed of the liquid components, particularly
effected by centrifugal action, as for example in a cen
trifugal separator of the imperforate type.
When the dispersion is subjected to centrifugal action
favorable dispersion mixtures of solid and liquid com
ponents are obtained if the starting fatty acid material
is cooled from a higher temperature to the separation
in an imperforate centrifuge, the aqueous phase contain
ing the suspended solid fatty particles pass over as the
once interrupted by an intermediate stage in which sub
temperature in stages, said cooling stages being at least
speci?cally heavier fraction, and the liquid fatty particles 45 stantially no cooling takes place.
Separate as a speci?cally lighter fraction.
The advantages of the aforesaid procedure is that the
separation is extremely clean-cut with the solid fatty
particles being substantially free from the liquid fatty
component. In addition, the physical effecting of the
process is highly e?icien-t and economical, being excel
lently suited for commercial operation with high through~
put efficiency and low cost. The disadvantages encoun
The ratio ‘of the time of stay, i.e. duration, of the ma
terial in the intermediate stage to the ‘time of stay of vthe
material in the cooling stage, in accordance with the in
vention, may within wide limits vary within ‘the range of
about 200:1 to 1:200.
In many cases, fatty material mixtures are ‘to be proc
essed, whose higher melting components still possess, for
fatty materials, good crystallization ‘tendencies. These
maybe processed according to the usual separation proc
tered with the liquid or solid separation, as for example
55 esses for liquid and solid ‘materials. Such mixtures are,
with ?ltration, etc., are thus avoided.
However, the separation as above described suffers
for instance, mixtures of stearin and olein from ‘which the
from the drawback that it does not afford the possibility
olein may be pressed off after crystallization of the stearin.
other than by varying certain operating conditions, i.e.
According to Bailey: “Industrial Oil and Fat Products,"
the cooling rate, the separating temperature, the nature
1945, New York, page 873, paragraph 4, the components
and quantity of liquid organic compounds or their mix 60 of such a mixture may be separated by effecting the crys
tures added, to alter or in?uence the consistency of the
tallization of the higher melting component. In proces
mixture to be separated and the composition of the solid
sing such mixtures, whose higher melting components
and liquid components. In other words, the use of the
have good crystallization tendency, it is recommended
aqueous phase to effect the separation does not have
in accordance with the invention that the length of the
any effect on the dissemination of the substances of dif 65 time of stay of the materials in the intermediate stage
fercnt melting points in the solid and liquid phases inter
should be at least as great as in the preceding cooling
mixed in the starting material. This distribution is very
stage, and preferably the time of stay of the material in
important with respect to the separation effect achieved
the intermediae stage should amount to a multiple of the
and above all, the composition, i.e. state, of the solid
time of stay in the preceding cooling stage. The ratio
fatty particles is critical with respect to this effect. That 70 of the time of stay of the material in the intermediate
is, in the crystal lattice of the solid components there
state to the time of stay of the material in the cooling
are to be inserted as few liquid component particles as
stage may, for example, lie within the range of 4:1 to
200:1 and preferably lies within the range of 10:1 to 50:1.
For the cooling of the fatty acid mixtures, heat ex
change-rs are used, in which the walls which serve to ef
fect the heat exchange are kept free from deposits of solid
fatty materials. This is accomplished by passing the fatty
ester mixes mentioned above. The esters may be split
with the aid of water or steam or may be saponi?ed with
the aid of caustic, while the fatty acids may be liberated
from the resulting soaps with the aid of acid. Fatty acid
mixtures of synthetic origin may ‘be those obtained, for
acid material adjacent and in contact with walls serv
example, by the oxidation of natural or synthetic para?ins
ing for the heat exchange at a high ?ow speed rate or
and the isolation of the fatty acids from the oxidation
mixture, or may be obtained by the oxidation of alcohols,
such as is for example practiced in the hydrogenation of
posits which are formed are torn away. There are par 10 carbon monoxide. Furthermore, the synthetic mixtures
may be obtained by the oxidation of products which are
ticularly preferred as heat exchange units the so-called
obtained from the addition of carbon monoxide and hy
“scraper coolers.” Here one deals with cylindrical cool
drogen to ole?ns, resulting in fatty acid mixes well suited
ing devices, in which ‘the cooling surfaces, which come
to separation by the application of the process in accord
into contact with the fatty material mixture, are kept the
free from deposits of solid fatty materials by means of 15 ance with the invention.
The fatty acid mixtures to be processed according to
moving scrapers or shavers.
this invention may preferably contain as main compo
The depositing of solid fatty materials on the cooling
nents fatty acids of 6-36, preferably 10-28, carbon atoms
surfaces may also be decreased or in fact entirely pre
in their molecule. If the ester mixtures are containing
vented if the fatty materials are passed through the cool
ers in form of a dispersion in aqueous phase and, if nec 20 as carboxylic acid components fatty acid radicals, these
under conditions of high turbulence, so that through the
shearing forces occurring at the cooling surface any de~
essary, in an aqueous wetting agent solution.
In this
radicals may be derivated from fatty acids of the same
molecular size.
All the above mentioned materials are generally ob
tained as mixtures containing components of varying melt
materials with the cooling surface is strongly decreased. 25 ing points. These materials are of industrial importance,
situation, the fatty materials are present in form of small
droplets which are entirely surrounded by aqueous phase,
and thus the possibility of a direct contact of the fatty
In order to avoid in the heat exchanger, at the lower
temperatures, freezing of the aqueous phase or a separa
tion of the substances dissolved therein, it is desirable to
add materials to the aqueous phase which reduce the
freezing point of water. Suitable for this purpose are in
organic salts and above all organic Water-soluble solvents,
and it is generally necessary to separate the mixtures into
components of different melting points ‘for further use.
The invention, however, is not limited to the speci?c,
above enumerated mixtures, but is applicable to all simi
lar mixtures regardless of their source of procedure for
obtaining the same, as would ‘be obvious to the skilled
artisan, since the separation is physical in nature.
The drawings exemplify illustrated embodiments of
cooling apparatus usable in the practice of the process
glycerin, propylene-glycol, butyleneglycol, polyglycolene, 35 in accordance with the invention, without it being in
tended, however, to limit the application of the novel
polyglycerines, etc.
particularly if the latter are only di?icultly volatile. Ex
amples of such solvents are the polyvalent alcohols or
their water-soluble ethers, as for example ethyleneglycol,
Suitable raw materials for the practice of the invention
are carboxylic acid ester mixes and fatty acid mixes of
both natural or synthetic origin.
Natural carboxylic acid esters are predominantly fatty
‘acid esters and particularly glycerides, such as are ob
tained from the fat of vegetable and land and marine ani
~ mals. Examples of the various types of vegetable fats in
method to the particular heat exchanger or heat ex
changer storage container arrangement there depicted.
Referring to the diagrammatic representation of the
40 cooling arrangement, as illustrated in FIG. 1, in opera
tion, the starting material to be cooled enters into the
cylindrical heat exchanger 11 at the connection 15. The
cooling agent enters into the exchanger at 14 and leaves
the cooling jacket at 13. The starting material to be
clude coconut oil, palm oil, olive oil, soya bean oil, linseed
oil, wood oil and rapeseed oil. Examples of the various 4-5 cooled passes through the cylinder 11, whose inner wall
is kept free of deposits by means of a rotating scraper
types of fats obtained from land animals include beef fat,
12, which takes the form of a screw in the embodiment
hog fat andv bone fat. Examples of the various differ
shown in FIG. 1. After the desired cooling has been
ent types of fats of marine animals include whale oil, men
effected, the starting material passes through the pipe
haden oil, cod liver oil and herring oil.
Among the natural carboxylic acid esters, which con- I50 line 16 into the intermediate container 17, from which
it leaves at 18 and passes from there into the next cool
tain alcohols other than glycerine as the alcohol compo
ing stage. As the intermediate container 17 may serve
.nent, there may be mentioned, for example, sperm oil,
any desired container. It may be provided with guide
which in addition to glycerides also contains fatty acid
aliphatic alcohol esters as well as the wax esters.
plates or other immovable or mova-ble interior structures,
if desired.
In the embodiment shown in FIG. 1 there
In connection with the esters of fatty acids, the alcohol 55 is provided a movable screw, by means of which the
> component thereof may be derived from mono- and poly
material is stirred thoroughly. The stirring gives rise
valent,>preferably from .mono- to tri-valent, alcohols.
to shearing forces which serve to promote the crystalli
.The mono-, di- ‘and tri-glycerides and the esters of fatty
zation. In place of the container 17 there may also be
_ acids and fat alcohols are of particular technical interest.
used the construction which is shown in ‘FIG. 2. This
However, esters of fat alcohols and mono- or poly-basic
construction consists of a cylindrical container 20 provided
carboxylic acids having from 1-5 carbon atoms in their
with inlet and outlet connections 21 and 22, respectively.
molecules may be used as starting materials in accordance
In the container, stationary plates 23 are arranged per
with the invention.
pendicular to the cylinder shaft, which plates are pro
In addition to glycerides, any other desired ester com
vided with an opening in the middle thereof, through
bination may be used, such as for example are used as 65 which the revolving shaft 24 passes' On the revolving
softeners, which may be produced synthetically.
shaft 24 there are arranged circular discs 25, so as to
When the ester mixtures contain solid as well as liquid
alternate with the stationary plates. The fatty material
components at a given temperature, it is often of indus
is forced between the revolving and the stationary plates
trial importance to separate the mixture into components
and ‘thereby exposed to particularly strong shearing
of different melting points, as for example in the winteriz 70 forces. However, the method can also be effected em
ing of edible oils, the separation of hardened fats, the re
ploying in the intermediate containers very simple stir
moval of solid constituents from softeners and the sep
aration of isomeric phthalates, etc.
Fatty acid mixes of natural origin are those which are
ring devices. Such an arrangement is shown in FIG. 3.
Additionally, the containers 31 and 32 in FIG. 3 serve
simultaneously as intermediate containers and storage
obtained from the naturally occurring carboxylic acid 75 containers and are provided with the simple stirring de
vices 34 and 35. Finally, one may employ as the inter
there via the distributor system 37 consisting of pipe
mediate containers pipe lines of suitable volume, which
lines and valves back to the storage vessel 31. When
the material in storage vessel 31 has reached the desired
temperature, then the material is conducted by changing
for instance may even [be ccastructed as pipe coils.
If the temperature of the starting material as supplied
lies very much above the temperature at which the crystal 5 over of the valves of the distributor system 36 via the
lization begins, then the cooling down of the starting
pipe line 38 for ‘further processing.
material to the temperature at which crystallization
the storage vessel 32 is ?lled with the material, which is
begins may be effected in any manner desired. The
process in accordance with the invention starts with the
beginning of crystallization. The heat extraction during
the course of the cooling process may take place in
‘any manner desired. Thus, for instance, the heat extrac
tion may be, except ‘for the intermediate stages, uniform~
1y distirbuted over the entire cooling process. However,
the heat extraction may be regulated so as to be particu
larly great at the beginning or at any point in the course
of the cooling process, or at the end of same. The par
ticular variation or sequence used depends mainly on the
In the meantime
conducted in a circular course via the distributor system
36, the heat exchanger 30 and the distributor system 37,
and is thereby cooled oil.
Insofar as the screw worms, shown in the cooling and
intermediate vessels according to FIG. 1, do not suf?ce
‘for the transportation of the material, special conveyor
devices, such as for instance pumps of the most varied
constructions, are to be provided. This is advisable,
above all, in the apparatus according to FIG. 3, where
pumps may be arranged ‘for instance between the two
storage vessels 31 and 32 and the distributor system 36,
type and the crystallization characteristics of the mate
between this distributor system and the heat exchanger
rial to be processed.
20 35) and/or between this heat exchanger and the dis
The start of the crystallization is initiated earlier if the
tributor system 37.
starting material contains small amounts of crystals,
Conveniently, the size of the storage vessels and the
which have either been left in the starting material be
capacity of the heat exchanger 1and/or the temperature
of the cooling agent passing through the heat exchanger
tals have been recycled from- later cooling stages into 25 is so regulated that there is always required for the
the container or vessel containing the material.
reaching of the separation temperature as much time
Because of the low crystallization velocity of fatty
as for the emptying of the other vessel, whose material
materials, the crystallization in general is not completed
content is to be passed to the ?nal separation. If the
when the material leaves the heat exchanger. 'It is com
storage vessel running without load is then ?lled with
cause of an incomplete melting of same, or if some crys
pleted in the intermediate stage, in which no further heat
extraction takes place. The vessel, in which the mate
rial to ‘be cooled is maintained during the intermediate
stage, may be insulated against any possible heat ex
change with the suroundin-gs. In the intermediate stage
there may occur through the liberation of heat of crystal
lization a heating of the material. This increase in tem
perature is not, however, in any way attributable to heat
absorption from the environment. The material in the
newly supplied starting material, ‘then the small quanti
ties of solid carboxylic acid ester particles, which still
adhere as a residue of the previous charge to the walls
of the storage container or which are still in the lines
and in the heat exchanger, act as seed crystals and thus
promote, i.e. accelerate, the crystallization of the higher
melting constituents of the newly fed charge.
Of course the heat exchanger and storage vessel may
be arranged for a longer time of stay of the material in
intermediate container may under certain circumstances
the cooling step than in the intermediate stage. The time
be supplied with heat. In that instance, the quantity 40 of stay of the material in the cooling step may, for in
of heat supplied is preferably so regulated that it is smaller
stance, amount to ‘the 4~20O fold, preferably 10-50 fold,
than the heat quantity drawn o?c in the preceding cool
the time of stay in the intermediate stage. It is also pos
ing step. However, it is also possible to supply in the
sible that heat may be supplied in the intermediate stage.
intermediate stage more ‘heat than was drawn 01f in the
This variation of the ?rst described process is, above
preceding cooling step.
This special situation should 45 all of advantage for the processing of dil'iicultly crystal
arise, generally speaking, only when the heat balance of
the remaining cooling steps has to be regulated so that
the starting material is not cooled off to below the sepa
ration temperature.
The number of cooling steps to be connected in series
should be ‘at least two, but it may be considerably higher
and may be, ‘for instance, up to 5—200 series-connected
lizable fats, particularly for some fatty acid triglycerides.
Through the increased time of stay in the cooling step,
the formation of the ?rst crystals is accelerated. There
fore, it becomes advisable, with the crystallization just
starting, to slowly withdraw heat. The slow heat-with
drawal may be attained through a correspondingly weak
cooling in the cooling step and/ or when the material is
steps. After the last cooling step, no further intermediate
passed through the intermediate stage, supplying in the
stage need be arranged.
intermediate stage a part of the heat which has been
It has been expressly shown, and this is an essential 55 withdrawn in the cooling step.
object of the invention, that the cooling of the starting
The cooling of the starting material, employing a longer
material to be separated may be attained both as to
time of stay in the cooling step than in the intermediate
apparatus and process when the starting material is led
stage, may be employed when a relatively ‘narrow range
through a series of stages, in which the material is passed
of the total temperature decrease is to be effected. This
in a circular course from a storage container, which si 60 range may, for instance, amount to less than 1° C. but
multaneously serves as intermediate stage, through a
it may also extend to 5, 10 or 20° C.
heat exchanger and back into the storage container.
If, however, a part, preferably 10-50%, of the ma
Just as in the device, shown in FIG. 1, the ratio ‘of the
terial to be separated from the starting material as higher
capacity of the heat exchanger and intermediate vessel
melting component has solidi?ed, then one may switch
has to be proportional to the ratio ‘of the duration of 65 to the mode of ‘operation in which the time of stay in the
stay, so also in this device the volume ratio of the ma
intermediate stage is greater than in the cooling step.
terial present in .the storage vessel to the capacity of the
The mixtures thus obtained of solid and liquid con
heat exchanger must correspond to the ratio of the
stituents of the starting material are now further proc
duration of stay.
essed in the manner known per se. Insofar as these mix
A device suitable for the carrying ‘out of this variation
tures were not already during the cooling dispersed in
of the process in accordance with the invention is shown
an aqueous phase, they must be dispersed in a manner
in FIG. 3. The material to be cooled is in the storage
known per se and then the dispersion separated into the
vessel 31, which is provided ‘with the stirrer 34. A pipe
two phases.
line leads via the distributor system 36 consisting of pipe
The separation of the dispersion of the fatty acid mix
‘lines and valves to the heat exchanger ‘30, and from 75 ture may be effected, for example, in certain cases merely
by allowing the dispersion to stand, whereby the upper
phase of the liquid portion of the fatty acid mixture forms
along with a lower phase containing the aqueous solution
When the same starting material was continually cooled
down over a period of 8 hours, but otherwise under the
same conditions as above described, there was obtained
with the dispersed particles of the solid component of the
a clearly recognizable slower separation of the oil drop
lets from the dispersions in the centrifugation step.
Example 2
fatty acid mixture.
By decanting the layers, products
may be very simply recovered. Preferably the disper
sion is separated into layers by centrifugal action, em
As starting material there was employed a Sumatra
palm oil (iodine number=50.4), from which there _had
been removed small amounts of free fatty acids by a
vacuum-steam distillation. (This process has been de
ploying therefor centrifuges of the imperforate type.
The process of the invention makes possible for the
?rst time a slow crystallization and one which is, above
all, adjustable to any speci?c fatty acid mixture. As a
result of the process there is avoided any undesirable
after-crystallization which would otherwise occur in the
further processing of the mixture and which would act
to change in uncontrollable manner the composition of 15
the solid and of the liquid components of the mixture.
The results of the process are very surprising insofar as
scribed by Wecker, German Patent No. 397,332). 50
kg. of the treated palm oil were cooled under substan
tially the same conditions as described in Example 1
(volume ratio 1:13). The cooling took place over a
period of 6 hours, the fat ‘being cooled from 50 to 20° C.
Thereafter, the mixture of solid and liquid fat components
thereby obtained was dispersed in the manner described
the same results are not obtained even with slow cooling,
in Example 1. The following fractions were obtained:
employing the same cooling period as in the process in
accordance with the invention. A further and very sur 20 40 kg.=80
weight-percent lower-melting components
prising advantage of the process in accordance with the
(iodine number 56.8)
invention consists therein that in the centrifuging of the
10 kg.=20 weight-percent higher-melting components
dispersions obtained in accordance with the invention there
(iodine number 25.0).
is observed an essentially easier transition of the oil drop
was repeated, but in this case the starting ma
lets dispersed in the aqueous phase into the coherent oil 25
terial was slowly and continuously cooled from 50 to
phase than is the case in dispersions in which the cooling
20° C. The following fractions were separated:
of the starting material supplied was effected in another
80 weight-percent lower-melting components (iodine
number 53.6)
20 weight-percent higher-melting components (iodine
The following examples are given for the purpose of
illustration and not limitation:
number 39.7).
Example 1
80 kg. technical lard (iodine number=63.4) were
Example 3
melted down in a vessel equipped with stirrer of stainless
40 kg. Congo palm oil (iodine number=51.3) were
steel by heating to 50° C. Thereafter the fat was cooled 35 incompletely molten in a vessel equipped with a stirrer
by pumping the same through a circular course, which
by heating to 35° C. Thereafter the material was passed
consisted of a storage container and a scraper cooler hav
within 2 hours through the scraper cooler arrangement de
ing a 4~liter capacity and an 0.17 m.2 cooling surface.
scribed in Example 1 and thereby cooled down to 20° C.
The volume ratio of fat in the ‘scraper cooler and fat
The ratio of the fat material in the scraper cooler and/ or
in the storage container including the pipe line amounted 40 storage vessel, respectively, amounted to 1:10. Upon
to about 1:20. The scraper cooler was cooled with tap
reaching the temperature of 20° C., the fat material was
water having a temperature of 13° C. The temperature
left at this temperature for 2 hours and then emulsi?ed in
of the fat was measured in the storage container, and
an equal volume quantity of a wetting agent solution,
there was recorded the following cooling curve:
which contained 1 weight percent of a sodium soap of soy
Temperature, ° C.
fatty acid and 3 weight percent of sodium sulfate. The
Hours after start of cooling:
dispersion was further treated as described in Example 1,
and the following fractions were obtained:
33.2 kg.=83 weight-percent lower-melting components
(iodine number 57.5)
6.8 kg.=17 weight-percent higher-melting components
‘(iodine number 24.1).
Example 4
After reaching the lowest temperature, the fat was left
for two hours at 20° C. and then dispersed in an aqueous
wetting ‘agent solution, which contained dissolved in so
lution 0.3% alkylbenzolsulfonate (alkyl from tetrapro
pylene) and 4 weight-percent sodium sulfate. The weight
35 kg. of a somewhat solidi?ed olive oil (acid number:
0.9; saponi?cation number=l91; iodine number=70.8;
transcontent=65%) was heated to 80° C. and then
ratio of fat to wetting agent solution was 1:15. The
emulsion was then slowly passed through a stirring vat,
in which it was kept in motion by rotating a worm, and
was passed from the vat into the centrifugal separator
pumped through the apparatus described in the preceding
examples. It was rapidly cooled, the temperature falling
of the imperforate type. In the centrifuge, the dispersion
was separated into a lighter oil phase and into a heavier
down so that within 10 hours a temperature of 28° C.
was reached. During this time more and more crystals of
aqueous phase having therein dispersed the solid fatty
the higher-melting components of the starting material
within one hour from 80 to 40° C. In this cooling no
crystal separation took place. The cooling rate was slowed
particles. The aqueous phase was heated in ‘a heat ex 65 were separated out. The temperature of the starting mate
changer to a temperature at which the solid particles were
rial in the next four hours was further decreased to 20° C.
completely molten, and thereafter the liquid higher-melt
There was added to the fat material, which was being
ing fat fraction was separated from the aqueous phase
stirred continually in the storage vessel, 42 liters of wetting
in a plate centrifuge. There were obtained
agent solution having a temperature of 20° C. The
70 wetting agent solution contained 0.785 kg. of a paste of
61.6 kg.=77 weight-percent of the original charge in
lower-melting fat components (iodine num
ber 71.7)
18.4 kg.=23 weight-percent of the charge in higher-melt—
ing fat components (iodine number 36.0).
the alkylbenzolsulfonate described in Example 1 having
32 weight-percent active substance and 1.05 kg. sodium
sulfate. Then the emulsion was pumped through the cool
ing system within 4 hours, being cooled to 12° C. The
emulsion was maintained another 15 hours at this tempera
ture. After separation of the dispersion in the centrifugal
separator and separation of the aqueous phase from the
higher-melting components of the starting material, the
following fractions were obtained:
26.25 kg. solid components (iodine number 66.0; trans
content 67.5%)
8.75 kg. liquid components (iodine number 85.2; trans
content 58.5%).
When the same starting material was continually cooled
in the conventional manner over the same time interval
and processed under otherwise similar conditions, the
roundings, the temperature of the material fell within the
next two hours from 35° C. to 34° C.
The amount of
solid glyceride crystals separated during this time was
about 10-20% of the amount of solid glycerides present
at the ?nish of the entire cooling. After this condition
was reached, the jacket of the scraper cooler was charged
with water which was colder than the fat material being
passed through the cooler. In this manner the tempera
ture difference between the fat being passed through the
cooler and the cooling agent was regulated so that after
20 hours a fat temperature of 20° C. was attained.
The fat in the storage vessel, which was being con
tinually stirred, was then emulsi?ed by the addition of a
separation of the oil from the dispersion, in which the
1.5-fold by weight quantity of an aqueous wetting agent
quantity of solid components is far greater than the 15 solution containing 0.7% of a sodiumalkylbenzolsulfonate
quantity of liquid components, took place essentially more
(alkyl residue from tetrapropylene) and 3% sodium sul
fate. The emulsion was brought by further pumping
Example 5
through the cooling system within 4 hours to 12° C. and
kept for a further 16 hours at this temperature. Then
As starting material there was employed a mixture of
the dispersion was separated in a centrifugal separator
technical fat alcohols having an iodine number=72.5, 20 of the imperforate type into a lighter liquid glyceride
which mixture consisted predominantly of oleyl and
phase (12 weight-percent, iodine number 83.4) and into
stearyl alcohol. 30 kg. of this mixture were pumped
a heavier aqueous phase having therein dispersed solid
through the apparatus described in Example 1, being
glyceride particles (88 weight-percent; iodine number
cooled within two hours from 40 to +6° C., whereby there 25 69.5; cloud melting point 35.8° C.; clear melting point
was obtained a pasty mass permeated with crystals of solid
fat alcohols. This mass was emulsi?ed in 40 liters of an
36.8° C.).
The solid constitutents were usable as a
cocoa-butter substitute.
aqueous wetting agent solution, which contained 1 weight
In general, the invention may be used in the separa
percent of the sodium salt of a sulfation product of the
tion of different fatty materials, as fatty acids, fatty a1
technical fat alcohol serving as starting material and 3
weight-percent sodium sulfate. The dispersion was sepa 30 cohols and esters of fatty acids or fatty alcohols. The
term “fatty materials” designates compounds containing
rated at '+6° C. in a centrifugal separator of the imper
a higher fatty radical, this is to say an aliphatic straight
forate type into two phases. The lighter phase amounted
or branched chain, saturated or unsaturated radical, pref
to 73 weight-percent and consisted of the liquid com
ponents of the starting mixture. The aforesaid fraction 35 erably a hydrocarbon radical with 6-36, especially 10-28
carbon atoms.
had an iodine number of 92.5. From the aqueous phase
We claim:
there were isolated the solid components in an amount
1. In the method for the separation of organic mixtures
representing 27 weight-percent of the starting material.
from the group consisting of mixtures of fatty
The iodine number of the solid constituents was 19.3.
acids, mixtures of fatty alcohols, mixtures of fatty acid
Example 6
35 kg. tallow fatty acid (iodine number=52.5) in
molten condition were pumped from a vessel equipped
40 esters and mixtures of fatty alcohol esters into compo~
nents of different melting points by forming a dispersion
of such a mixture in an aqueous solution of a surface
active material at a temperature at which the mixture
contains both solid and liquid constituents and there
with a stirrer through a scraper cooler connected via an 45 after separating the aqueous dispersion into a speci?cally
expansion line, as was described in Example 1. ‘In the
course of 24 hours the tallow fatty acid was cooled from
40 to 10° C. There was then added 1.5 times the amount
of the fatty material of an aqueous solution having the
same temperature and containing 0.2% Cm-alkylsulfate
and 1% MgSO4, while continuously stirring. The disper
sion formed was then separated in a centrifugal separator.
The following products were obtained:
58.7% olein '(iodine number 82.2; cloud point 5° C.)
41.3% stearin (iodine number 10.1).
When the same tallow fatty acid mixture was continually
lighter phase of substantially liquid components of the
mixture and a speci?cally heavier phase of aqueous me
dium with substantially solid components of the mixture
suspended therein, the improvement which comprises
cooling the said mixture in its entirety in successive steps
from a temperature higher than the separation tempera
ture down to the separation temperature and interrupting
said cooling steps at least once with an intermediate stage
in which substantially no cooling takes place, the ratio of
55 the time of stay of said mixture in the cooling steps to the
time of stay in the‘ intermediate stage lies within the
range of 200:1 to 1:200.
2. Method according to claim 1 wherein said mixture
cooled in a vessel with stirrer, employing wall cooling,
is in the form of an aqueous dispersion.
but otherwise processed under the same conditions, the 60
3. Method according to claim 1 wherein said mixture
stearin obtained had an iodine number of 17.2.
Example 7
is in the form of a dispersion in an aqueous solution of
a surface active material.
4. Method according to claim 1 which comprises ef
fecting the cooling by the steps of cooling said mixture,
35 kg. of a slightly solid?ed olive oil (acid number: 65 maintaining said mixture in the following intermediate
0.9; saponi?cation number :19‘1; iodine number=70.8;
transcontent=65%) were completely molten by heating
stage so that the time of stay of said mixture in said cool
ing step is from 4 to 200 times as great as in said inter
mediate stage and when a part of the mixture as higher
to 80° C. and then so rapidly cooled by pumping through
the apparatus described in Example 1 that the tempera
melting component has solidi?ed thereafter effecting the
ture of the glyceride in the storage vessel fell within 30 70 cooling so that the time of stay of said mixture in the
minutes to 35° C. At this temperature the crystalliza
subsequent intermediate stage is from 4 to 200 times as
tion began. Then the jacket of the scraper cooler was
great as in the cooling step immediately preceding it.
charged with water having a temperature of 38° C. and
5. Method according to claim 1, wherein the time of
the fat further pumped therethrough. By the transfer
stay of said mixture in the intermediate stage is from 4
of heat from the material in the storage vessel to the sur 75 to 200 times as great as in the preceding cooling step.
6. Method according to claim 5, wherein the time of
1 2;
References Cited in the ?le of this patent
stay of_said mixture in the intermediate stage is from 10
to 50 tlmes as great as in the preceding cooling step.
7. Method according to claim 1, which comprises heat-
P091 et al~ ——————————— —— Feb- 27, 1951
ing said mixture in at least one of said intermediate stages. 5
Stem ———————————————— -- July 23, 1957
8. Method according to claim 7, which comprises heating said mixture in said intermediate stage to substantially the temperature of said mixture prior to the preced-
Devault ————————————— —— APT- 5, 1960
Great Britain _________ __ Dec. 21, 1955
ing cooling step.
7 42,3 5 4
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