CA1141774A - Method of separating mixtures of fatty substances - Google Patents
Method of separating mixtures of fatty substancesInfo
- Publication number
- CA1141774A CA1141774A CA000344071A CA344071A CA1141774A CA 1141774 A CA1141774 A CA 1141774A CA 000344071 A CA000344071 A CA 000344071A CA 344071 A CA344071 A CA 344071A CA 1141774 A CA1141774 A CA 1141774A
- Authority
- CA
- Canada
- Prior art keywords
- fatty
- aqueous phase
- separation
- continuously
- melting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0091—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils non-solvents, e.g. water wherein the fat or oil is dispersed account a more washing out of fractions is not taken into
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0022—Evaporation of components of the mixture to be separated by reducing pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
This invention is directed to a method for separating fatty substance mixtures into components of different melting points by the "Rewetting or Hydrophilizatlon Process," wherein aqueous solution of higher melting fatty substance is recycled to cool molten fatty substance mixture.
This invention is directed to a method for separating fatty substance mixtures into components of different melting points by the "Rewetting or Hydrophilizatlon Process," wherein aqueous solution of higher melting fatty substance is recycled to cool molten fatty substance mixture.
Description
11417'74 This invention is directed to a method of separating fatty substances. More particularly, this invention is directed to an improved method of separating fatty substances into com-ponents of different melting points.
The separation of fatty acid mixtures or of fatty acid ester mixtures into components of different melting points by a wetting agent process is described in Stein et al., U.S.
Patent No. 2,80p,A93. This process has beaome kno~n as the "Rewetting or Hydrophilization Process." According to the Stein et al. patent, a mixture of solid and oily fatty sub-stance particles is transformed by means of a wetting agent solution, optionally containing non-surface-active electrolyte, into a dispersion of separate solid and oily fatty substance particles. This dispersion is separated by means of solid jacket centrifuges into an oily phase and an aqueous phase containing the solid fatty substance particles in dispersion.
The heat removal necessary for the crystallization by cooling devices, in particular, scraping condensers. After termina-tion of the separating process, the recovered wetting agent solution is recycled. German Patent No. 1,010,062 or Stein et al., U.S. Patent No. 2,972,636 describes a corresponding process for the separation of fatty alcohols.
nam/ -1-i ~
11~177g From U.S. Patent No. 3,541,122, a method is further known for the separation of mixtures of fat-like materials in-to fractions of different melting points, which method is also carried out by the rewetting process. Here, however, the cool-ing of the molten fatty substance mixture required for crystal-lization is obtained by vacuum evaporation of water. After complete dispersion of the fatty substance mixture consisting of liquid and solid particles in a wetting agent solution, the crystallized solid phase is separated by filtration, and the oily dispersion passes through the filter. In this procedure the separation of the oily fraction and the solid particles is not complete, so that the latter have a relatively high iodine number and hence a comparatively poor quality.
Published German Patent Application (DOS) No.
1,915,298, discloses a method of separating fatty acid, fatty alcohol, or fatty acid ester mixtures into components of dif-ferent mel~ing points by mixing the molten mixture with an aqueous wetting agent solution. The crystallization of the solid fractions to be separated is obtained by evaporating a part of the aqueous wetting agent solution under reduced pres-sure. Because the fatty substances used can be degased only with difficulty and incompletely on being fed into the crystal-lizer vessel, intense foaming takes place upon addition of the wetting agent solution, whereby the progress of the process is greatly disturbed. Moreover, the wetting agent nam/ -2-~141774 hinders crystal growth, which in turn leads to difficulties in the further separation of oily and solid phases.
An improved Rewetting or Hydrophilization Process is described in Jeromin et al., U.S. Patent No. 3,950,371. Ac-cording to this patent, mixtures of fatty substances are sep-atated into components of different melting points by the re-wetting process, where the heat removal required for the cool-ing and crystallization of higher melting fatty substance fractions is obtained by vacuum evaporation of an aqueous phase in direct contact with the fatty substance mixture.
More specifically, the Jeromin et al. process is character-ized by the following steps:
(a) partial or complete melting of the fatty substance mixture;
(b) addition of an aqueous non-surface-active electrolyte solution to the molten fatty substance mix-ture and evaporation of a part of the water of the elec-trolyte solution by means of a vacuum simultaneously with intensive mixing to produce partial or complete crystalli-zation of the higher melting fraction;
(c) addition of wetting agent solution with dis-persing of the liquid and solid fatty substance therein, preferably whil~ maintaining the vacuum and continuing the water evaporation until the separation temperature is reached;
(d) separation of the dispersion by means of centrifuge into an oily phase containing the lower melt-ing fatty substance fractions and an aqueous phase con-nam/ _3_ 11~177~
taining the crystallized fatty substance fractions in dispersed form; and J
(,e) separation of the higher meltin~ fatty substance fractions from the aqueous phase ~y filtration or by melting and subsequent separation of oily phase from aqueous phase by centri-fuging or allowing to settle.
This process can be carried out in'several separation steps by again su~jecting the oily phase obtained in step (d) oi the process, w~ich contains lower melting fatty components, to a similar separation process on a lower temperature level.
~urther separation steps can be added as necessary. The aqueous dispersion o~ the crystallized higher melting fatty components obtained in -addition to the oily phase in step ~d) of the pro-cess, is worked up separately according to step (e) of the pro-cess. The final separation temperature is reached only in the - last separation step in the multi~step procedure~ The step-by-step crystallization and separation of'the higher melting fatty components resulting from this can lead particularly to a purer oily phase with a low melting point.
However, this process still has certain defects, --especially when fatty substances that are more difficult to crystallize are to be separated. The result may then be delay-ed crystal formation in the vacuum evaporation phase, which leads to reduced throughput, i.e., to poorer quality of the final products. This delayed crystal formation is the reason that the process of the Jeromin et al. patent can either not be carried out in many actual cases or carried out only with inadequate success.
- , ,- - _4- , -119~17'~4 Another disadvantage of this process is that the aqueous dispersions of the crystallized, higher melting fatty components obtained in step (e) of the process carried out as a multi-step operation, must be worked up separately. This requires separate equipment and procedural s~eps, particularly .
an increased expenditure of energy for the melting of the solid fats present in the dispersion. A simultaneous processing of .:.
the obtained dispersions generally is impossible because of the varying quality of the obtained higher melting atty fractions.
It is an object of this invention to provide a method of separatingr-fatty substances.
It is also an object of this inventi.on to provide an improved Rewetting or Hydrophiliza~ion Process, It is further an object of this invention to provide an impxoved process comprised of the steps of:
~ a) partially or completely melting a fatty substance mixture;
(b) adding to the melted fatty substanc~ mix-ture aqueous, crystallized fatty components in di.spersed form and evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion has partly or completely crystallized;
(c) adding further aqueous wetting agent solution to form a dispersion of liquids and solid fats, prefera~ly with continued maintenance of vacuum and evaporation of water until the separation temperature is reached;
--5-- . -~41774 (dl separating the dispersion by centrifuging to obLain an oily phase containing the lower melting fatty compon-ents and an agueous phase containing crystallizea fatty components in dispersed form; and te) separating the higher melting fatty components fro~ the aqueous phase by filtration or by melting and subsequent cen,rifuging or settling out, whereby the separation process is carried out in several succes-sive separation stages.
These and other objects of the invention will become more apparent in the discussion below.
This invention is directed to an improvement of the known xe~letting process which results in improved products.
According to the invention, the separation of mixtures of fatty substances is carried out according to the separation steps de-scribed above, with the addition that the aqueous dispersion of the higher melting fatty components obtained in step ~d) of a subsequent separation stage is returned to the vacuum evapora-tion step (b) of a preceding separation stage, where it is com- -bined with the warmer starting mixture that has not yet cooled to the desired separation temperature of this step. The return-ed dispersion serves directly to cool and disperse the original fat~y mixture.
This approach ~ the productivity of existing equipment and eliminates the need for aaditional, expensive or involved procedures for the improvement of the crystallization of the fatty mixtures to be separated, for example, the removal of contaminants, or special equipment and procedures for the 11~1'774 working up of the aqueous dispersion containing higher melting components.
More particularly, the process according to the in~ 1, vention consequently can ~e carried out in the following man-ner:
Separation Stage I: , -~ a) partially or completely melting a fatty sub- ' stance mixture;
(,b) adding to the melted fatty su~stance mixture aqueous, crystallized fatty components in dispersed form as well as the aqueous phase from step (d) of Stage II, which contains wetting agent and eiectrolyte, and evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion has partly or completely crystallized, - tc2 adding further aqueous wetting agent and elec-trolyte solution ~Pld dilution) from step ~e) of Stage I plus,.
if desired, fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, preferably with continued maintenance of vacuum and evaporation of water until the separation temperature is reached;
(d) separating the disperslon by centrifuging,to obtain an oily phase containing the lower melting fatty components and an aqueous phase containing crystallized fatty components in dispersed form; and ~ .e~ separating the higher melting fatty components from the aqueous phase told dilution)'by filtration or by melting - ~ . . ..
17'74 and subsequent centrifuging or settling out.
Separation Stage II: -The oily phase obtained in step ~d) of the procedure of Separation Stage ~, which phase contains the lower melting fatty components, is subjected to one or more repetitions of a basically similar separation process, including step ~d) of ~he processr on a lower temperature leYel. The crystallization and dispexsing process [steps (b) and (c) of the process] is per-formed with the aid of old dilution from step (e~ cf the process of Separation Stage I, with the addition of fresh aqueous wet-ting agent and electrolyte solution, if desired.
_ . ~
The aqueous phase obtained in step ~d) of the proce-dure of Separation Stage II, which phase contains the crystal-lized fatty components in dispersed form, is not, however, pro-cessed further according to step (e) of Stage II, but is return-ed to step (b~ of Separation Stage I.
The temperature level of Separation Stage II may already correspond to the given separation temperature, or be above that temperature, in which case the final separation tem-perature is reached only after further, basically similar separa-tion stages. In this case, i.e., when further separation stages are used, the fatty suspension obtained in the respective step (d) of each stage is returned to step (b) of the respectively preceding separation stage as described.
The process according to the invention can be per-formed discontinuously or, preferably, continuously. In an especially preferred embodiment of the invention, fatty mixtures are separated in the following manner:
...... . .. . . . . . . . . .
1~1774 ~ a) continuously, partially or completely melting a fatty substance mixture;
(b) continuously adding to the melted fatty sub-stance mixture fro~ step ta) an aqueous dispersion comprising cry-stallized fatty components as well as wetting agent and electro-lyte solution from step ~i~ and continuously evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion of the fatty substance mixture has partly or completely crystallized;
~ c) continuously adding aqueous wetting agent and electrolyte solution ~the major part of the old dilution) from step ~e~ plus a portion of fresh aqueous wetting agent and electro-lyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and-evaporation of water until the . . .
separation temperature of the fatty substances is reachea;
(.d) continuously centrifuging the dispersion from step (c) to obtain an oily phase containing lower melting fatty components and an aqueous phase containing higher melting, crystal-lized fatty components in dispersed form;
~ e2 continuously separating higher melting compon-ents from the aqueous phase by filtration or by melting and subse--quent centrifuging or settling out, and recycling treated aqueous phase (old dilution) partially to each of steps (c), ~f~, and (g);
~ f) continuously adding to the oily phase from step ~d) an aqueous phase containing electrolyte and optionally treated aqueous phase (old dilution) from step (e) and evaporating part of the water under vacuum with the simultaneous intensive mixing, ~ ~ 74~
until higher melting fatty substance has partly or completely crystallized;
(g) continuously adding further aqueous phase (old dilution) from step (e) and fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until a second separation temperature is reached;
(h) continuously separating the dispersion by cen-trifuging to obtain an oily phase and an aqueous phase contain-ing crystallized fatty components in dispersed form;
(i) continuously recycling the aqueous phase fxomstep (h) to step (b); and (j) continuously recovering fatty substances of lower melting point from the oily phase from step (h).
The aqueous phase is treated as in step (e) to remove the higher melting fatty components, and the resulting treated aqueous phase (old dilution is reused. From about 40 to 70 percent of the old dilution is recycled to step (c), from about 0 to 10 percent of the old dilution is added to step (f), and from about 10 to 30 percent of the old dilution is added to step (g). From about 10 to 30 percent of the old dilution is removed from the system.
Other details concerning the steps of the separation process, including useful wetting agents, electrolytes, and the like, are described in U.S. Patent No. 3,950,371.
nam/ -10-11~1774 In the process of the invention, the wetting agent obtained as the so-called old dilution in step ~e) of Separation Stage I is returned into the separation process. Howe~er, the continuous removal of part of this solution from the circulation is necessary to pre~ent the accumulation of slimy contaminants contained in the starting fats, which can impair the crystalli2a-tion as well as the quality of the higher melting fat components.
The loss of wetting agent and electrolyte occurring here must be compensated by the addition of fresh wetting agent and electrolyte.
The preferred wetting agent is Na-dodecyl sulfate; the preferred -electrolyte is magnesium sulfate. Furthermore, the process must be monitored so that the loss of water occurring during th~ eva-poration cooling and due to the removal of wetting solution is compensated by the added electrolyte solution or the fresh wet-ting solution.
The process is suitable for the separation of the most diverse fatty mixtures. In particular, mixtures of fatty acids, esters of fatty acids, or fatty alcohols can be separated when the melting points of the components to be separated are suffi-ciently far apart.
~ he separation of fatty acid mixtures or technical olein and technical stearin toleic acid and stearic acid) or of fatty alcohol mixtures of oleyl alcohol and stearyl alcohol, is -of special technological significance. Similarly solid mixtures of trialycerides of fatty acids can be separated at room tempera-ture into fractions with lower and higher melting points. Such - .. - ' ,' .... ,,. .
1141'7791t fractions of triglycerides of fatty acids are used for the pre-paration of cooking fats. It is not necessary that one of the co~ponents to be separated is present as a liquid oil at room temperature. The process can also ~e used successfully when both components are solid and only differ to a sufficient degree in their melting points.
The described process can also be varied in such a manner that the vacuum evaporation step Cb) of Separation Stage I is preceded by conventional, indirectly acting cooling equip-ment, particularly a cooling step with rotating pressure coolers.
This constitutes a further improvement of the process, especial~
ly with respect to the productivity of available equipment, since the sta~ting fatty mixture now enters the vacuum evapora-tion step (b~ of Separation Stage I in a partially crystallized sta.e. The proportion of fat components precrystallized in the rotating pressure coolers is preferably from about 10 to 40 per-cen. by weight of the total higher melting components to be cry-stallized.
The special advantages of the process according to the invention are found in that the returned a~ueous dispersion -~distinctly improves the tendency of the fatty mixture to crystal-lize. This results in a considerable acceleration of the separa-tion process or a corresponding increase in the productivity ;of available equipment and a better separation effect per separation stage. In addition, there is a significant energy advantage since the cold, aqueous suspensions of higher melting fatty com-ponents from the subsequently added separation stages are used directly to cool the respective preceding steps. The separate working up of this dispersion by melting the fatty particles and .. . ~ . . . .. ~ . ~.. . . ..
11~1774 separation would require a considerable amount of energy, in addition to additional necessary equipment.
The return of aqueous dispersion of higher melting fatty components from a subsequently added separation stage into a preceding separation stage in a multiple-step separa-tion process already is the subject of German Published Ap-plication (DE-OS) No. 21 00 022. There, however, the cool-ing of the used fatty mixtures is performed exclusively with rotating pressure coolers, and the returned dispersion serves only for the dispersing of the partially crystallized fat mixtures with simultaneous cooling to the separation temper-ature. An improvem~nt of the tendency of the fatty mixtures to crystallize during the vacuum evaporation cooling could not be construed from this.
The following example is intended to illustrate the invention and is not to be construed as limiting the invention thereto.
Example Work was performed according to Example 1 of U.S.
Patent No. 3,950,371 with the difference that a two-stage separa-tor was employed. Crude stearic acid hydrolyzed from tallow at 46C (iodin~ number 58, turbidity point 39C) was used in the vacuum evaporation crystallizer of Separation Stage 1. This stearic acid was mixed with vigorous agitation with the total amount of stearin suspension of 26C obtained in the Separation Stage II. A mixing temperature of 36C was established, which nam/ -13-114177~
induced the crystallization of the higher melting stearic acid components. The further cooling to 20 C was achieved by the eva-cuation of the crystallization vessel with the aid of steam jets.
The addition of the old dilution from step (e) of Separation Stage I, with a content of 0.2% dodecyl sulfate by weight as wet-ting agent as well as additional amounts of wetting agent, elec-trolyte and water to compensate for losses, especially hy the re-moval of part of the old dilution! resulted in a separable disper-sion that was separated in a solid jacket centrifuge. The stearic acid suspension obtained in this step was heated to 90 - 95 C, and the stearic acid was separated from the old dilution in a separator. The old dilution was returned to tbe cycle - as de-scribed - after the removal of an amount of approximately 20%.
The oily phase obtained in Separation Stage I (mainly oleic acid, iodine number 82.6, turbidity point 21 C) was sub-jected to another separation in Separation Stage II, using also old dilution of Separation Stage I as wetting solution. The cool-ing to 3 - 5 C was again achieved by evaporation under vacuum.
An oleic acid fraction with an iodine number of 86 - 93 and a tur-bidity point of 1 - 5 C was obtained~ The stearin suspension containing wetting agents and electrolytes was returned to the vacuum evaporation crystallizer of Separation Stage I, after warming to 26 C.
The preceding use of a rotating pressure cooler was ad-vantageous for the improvement of the productivity of the equip-ment. The melted fatty acid entered the rotating pressure cool-er with a temperature of 46 C. After cooling to 30 C and partial 11~17~
crystallization of the higher melting portion, the fatty acid mixture was fed into the vacuum evaporation crystallizex and processed further, as described.
The preceding specific embodiments are illustrative of the practice of the invention. It is to be understood, how-ever, that other expedients known to those skilled in the art or disclosed hereinr may be employed withou~ departing from the spirit of the invention or the scope of the appended claims.
The separation of fatty acid mixtures or of fatty acid ester mixtures into components of different melting points by a wetting agent process is described in Stein et al., U.S.
Patent No. 2,80p,A93. This process has beaome kno~n as the "Rewetting or Hydrophilization Process." According to the Stein et al. patent, a mixture of solid and oily fatty sub-stance particles is transformed by means of a wetting agent solution, optionally containing non-surface-active electrolyte, into a dispersion of separate solid and oily fatty substance particles. This dispersion is separated by means of solid jacket centrifuges into an oily phase and an aqueous phase containing the solid fatty substance particles in dispersion.
The heat removal necessary for the crystallization by cooling devices, in particular, scraping condensers. After termina-tion of the separating process, the recovered wetting agent solution is recycled. German Patent No. 1,010,062 or Stein et al., U.S. Patent No. 2,972,636 describes a corresponding process for the separation of fatty alcohols.
nam/ -1-i ~
11~177g From U.S. Patent No. 3,541,122, a method is further known for the separation of mixtures of fat-like materials in-to fractions of different melting points, which method is also carried out by the rewetting process. Here, however, the cool-ing of the molten fatty substance mixture required for crystal-lization is obtained by vacuum evaporation of water. After complete dispersion of the fatty substance mixture consisting of liquid and solid particles in a wetting agent solution, the crystallized solid phase is separated by filtration, and the oily dispersion passes through the filter. In this procedure the separation of the oily fraction and the solid particles is not complete, so that the latter have a relatively high iodine number and hence a comparatively poor quality.
Published German Patent Application (DOS) No.
1,915,298, discloses a method of separating fatty acid, fatty alcohol, or fatty acid ester mixtures into components of dif-ferent mel~ing points by mixing the molten mixture with an aqueous wetting agent solution. The crystallization of the solid fractions to be separated is obtained by evaporating a part of the aqueous wetting agent solution under reduced pres-sure. Because the fatty substances used can be degased only with difficulty and incompletely on being fed into the crystal-lizer vessel, intense foaming takes place upon addition of the wetting agent solution, whereby the progress of the process is greatly disturbed. Moreover, the wetting agent nam/ -2-~141774 hinders crystal growth, which in turn leads to difficulties in the further separation of oily and solid phases.
An improved Rewetting or Hydrophilization Process is described in Jeromin et al., U.S. Patent No. 3,950,371. Ac-cording to this patent, mixtures of fatty substances are sep-atated into components of different melting points by the re-wetting process, where the heat removal required for the cool-ing and crystallization of higher melting fatty substance fractions is obtained by vacuum evaporation of an aqueous phase in direct contact with the fatty substance mixture.
More specifically, the Jeromin et al. process is character-ized by the following steps:
(a) partial or complete melting of the fatty substance mixture;
(b) addition of an aqueous non-surface-active electrolyte solution to the molten fatty substance mix-ture and evaporation of a part of the water of the elec-trolyte solution by means of a vacuum simultaneously with intensive mixing to produce partial or complete crystalli-zation of the higher melting fraction;
(c) addition of wetting agent solution with dis-persing of the liquid and solid fatty substance therein, preferably whil~ maintaining the vacuum and continuing the water evaporation until the separation temperature is reached;
(d) separation of the dispersion by means of centrifuge into an oily phase containing the lower melt-ing fatty substance fractions and an aqueous phase con-nam/ _3_ 11~177~
taining the crystallized fatty substance fractions in dispersed form; and J
(,e) separation of the higher meltin~ fatty substance fractions from the aqueous phase ~y filtration or by melting and subsequent separation of oily phase from aqueous phase by centri-fuging or allowing to settle.
This process can be carried out in'several separation steps by again su~jecting the oily phase obtained in step (d) oi the process, w~ich contains lower melting fatty components, to a similar separation process on a lower temperature level.
~urther separation steps can be added as necessary. The aqueous dispersion o~ the crystallized higher melting fatty components obtained in -addition to the oily phase in step ~d) of the pro-cess, is worked up separately according to step (e) of the pro-cess. The final separation temperature is reached only in the - last separation step in the multi~step procedure~ The step-by-step crystallization and separation of'the higher melting fatty components resulting from this can lead particularly to a purer oily phase with a low melting point.
However, this process still has certain defects, --especially when fatty substances that are more difficult to crystallize are to be separated. The result may then be delay-ed crystal formation in the vacuum evaporation phase, which leads to reduced throughput, i.e., to poorer quality of the final products. This delayed crystal formation is the reason that the process of the Jeromin et al. patent can either not be carried out in many actual cases or carried out only with inadequate success.
- , ,- - _4- , -119~17'~4 Another disadvantage of this process is that the aqueous dispersions of the crystallized, higher melting fatty components obtained in step (e) of the process carried out as a multi-step operation, must be worked up separately. This requires separate equipment and procedural s~eps, particularly .
an increased expenditure of energy for the melting of the solid fats present in the dispersion. A simultaneous processing of .:.
the obtained dispersions generally is impossible because of the varying quality of the obtained higher melting atty fractions.
It is an object of this invention to provide a method of separatingr-fatty substances.
It is also an object of this inventi.on to provide an improved Rewetting or Hydrophiliza~ion Process, It is further an object of this invention to provide an impxoved process comprised of the steps of:
~ a) partially or completely melting a fatty substance mixture;
(b) adding to the melted fatty substanc~ mix-ture aqueous, crystallized fatty components in di.spersed form and evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion has partly or completely crystallized;
(c) adding further aqueous wetting agent solution to form a dispersion of liquids and solid fats, prefera~ly with continued maintenance of vacuum and evaporation of water until the separation temperature is reached;
--5-- . -~41774 (dl separating the dispersion by centrifuging to obLain an oily phase containing the lower melting fatty compon-ents and an agueous phase containing crystallizea fatty components in dispersed form; and te) separating the higher melting fatty components fro~ the aqueous phase by filtration or by melting and subsequent cen,rifuging or settling out, whereby the separation process is carried out in several succes-sive separation stages.
These and other objects of the invention will become more apparent in the discussion below.
This invention is directed to an improvement of the known xe~letting process which results in improved products.
According to the invention, the separation of mixtures of fatty substances is carried out according to the separation steps de-scribed above, with the addition that the aqueous dispersion of the higher melting fatty components obtained in step ~d) of a subsequent separation stage is returned to the vacuum evapora-tion step (b) of a preceding separation stage, where it is com- -bined with the warmer starting mixture that has not yet cooled to the desired separation temperature of this step. The return-ed dispersion serves directly to cool and disperse the original fat~y mixture.
This approach ~ the productivity of existing equipment and eliminates the need for aaditional, expensive or involved procedures for the improvement of the crystallization of the fatty mixtures to be separated, for example, the removal of contaminants, or special equipment and procedures for the 11~1'774 working up of the aqueous dispersion containing higher melting components.
More particularly, the process according to the in~ 1, vention consequently can ~e carried out in the following man-ner:
Separation Stage I: , -~ a) partially or completely melting a fatty sub- ' stance mixture;
(,b) adding to the melted fatty su~stance mixture aqueous, crystallized fatty components in dispersed form as well as the aqueous phase from step (d) of Stage II, which contains wetting agent and eiectrolyte, and evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion has partly or completely crystallized, - tc2 adding further aqueous wetting agent and elec-trolyte solution ~Pld dilution) from step ~e) of Stage I plus,.
if desired, fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, preferably with continued maintenance of vacuum and evaporation of water until the separation temperature is reached;
(d) separating the disperslon by centrifuging,to obtain an oily phase containing the lower melting fatty components and an aqueous phase containing crystallized fatty components in dispersed form; and ~ .e~ separating the higher melting fatty components from the aqueous phase told dilution)'by filtration or by melting - ~ . . ..
17'74 and subsequent centrifuging or settling out.
Separation Stage II: -The oily phase obtained in step ~d) of the procedure of Separation Stage ~, which phase contains the lower melting fatty components, is subjected to one or more repetitions of a basically similar separation process, including step ~d) of ~he processr on a lower temperature leYel. The crystallization and dispexsing process [steps (b) and (c) of the process] is per-formed with the aid of old dilution from step (e~ cf the process of Separation Stage I, with the addition of fresh aqueous wet-ting agent and electrolyte solution, if desired.
_ . ~
The aqueous phase obtained in step ~d) of the proce-dure of Separation Stage II, which phase contains the crystal-lized fatty components in dispersed form, is not, however, pro-cessed further according to step (e) of Stage II, but is return-ed to step (b~ of Separation Stage I.
The temperature level of Separation Stage II may already correspond to the given separation temperature, or be above that temperature, in which case the final separation tem-perature is reached only after further, basically similar separa-tion stages. In this case, i.e., when further separation stages are used, the fatty suspension obtained in the respective step (d) of each stage is returned to step (b) of the respectively preceding separation stage as described.
The process according to the invention can be per-formed discontinuously or, preferably, continuously. In an especially preferred embodiment of the invention, fatty mixtures are separated in the following manner:
...... . .. . . . . . . . . .
1~1774 ~ a) continuously, partially or completely melting a fatty substance mixture;
(b) continuously adding to the melted fatty sub-stance mixture fro~ step ta) an aqueous dispersion comprising cry-stallized fatty components as well as wetting agent and electro-lyte solution from step ~i~ and continuously evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion of the fatty substance mixture has partly or completely crystallized;
~ c) continuously adding aqueous wetting agent and electrolyte solution ~the major part of the old dilution) from step ~e~ plus a portion of fresh aqueous wetting agent and electro-lyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and-evaporation of water until the . . .
separation temperature of the fatty substances is reachea;
(.d) continuously centrifuging the dispersion from step (c) to obtain an oily phase containing lower melting fatty components and an aqueous phase containing higher melting, crystal-lized fatty components in dispersed form;
~ e2 continuously separating higher melting compon-ents from the aqueous phase by filtration or by melting and subse--quent centrifuging or settling out, and recycling treated aqueous phase (old dilution) partially to each of steps (c), ~f~, and (g);
~ f) continuously adding to the oily phase from step ~d) an aqueous phase containing electrolyte and optionally treated aqueous phase (old dilution) from step (e) and evaporating part of the water under vacuum with the simultaneous intensive mixing, ~ ~ 74~
until higher melting fatty substance has partly or completely crystallized;
(g) continuously adding further aqueous phase (old dilution) from step (e) and fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until a second separation temperature is reached;
(h) continuously separating the dispersion by cen-trifuging to obtain an oily phase and an aqueous phase contain-ing crystallized fatty components in dispersed form;
(i) continuously recycling the aqueous phase fxomstep (h) to step (b); and (j) continuously recovering fatty substances of lower melting point from the oily phase from step (h).
The aqueous phase is treated as in step (e) to remove the higher melting fatty components, and the resulting treated aqueous phase (old dilution is reused. From about 40 to 70 percent of the old dilution is recycled to step (c), from about 0 to 10 percent of the old dilution is added to step (f), and from about 10 to 30 percent of the old dilution is added to step (g). From about 10 to 30 percent of the old dilution is removed from the system.
Other details concerning the steps of the separation process, including useful wetting agents, electrolytes, and the like, are described in U.S. Patent No. 3,950,371.
nam/ -10-11~1774 In the process of the invention, the wetting agent obtained as the so-called old dilution in step ~e) of Separation Stage I is returned into the separation process. Howe~er, the continuous removal of part of this solution from the circulation is necessary to pre~ent the accumulation of slimy contaminants contained in the starting fats, which can impair the crystalli2a-tion as well as the quality of the higher melting fat components.
The loss of wetting agent and electrolyte occurring here must be compensated by the addition of fresh wetting agent and electrolyte.
The preferred wetting agent is Na-dodecyl sulfate; the preferred -electrolyte is magnesium sulfate. Furthermore, the process must be monitored so that the loss of water occurring during th~ eva-poration cooling and due to the removal of wetting solution is compensated by the added electrolyte solution or the fresh wet-ting solution.
The process is suitable for the separation of the most diverse fatty mixtures. In particular, mixtures of fatty acids, esters of fatty acids, or fatty alcohols can be separated when the melting points of the components to be separated are suffi-ciently far apart.
~ he separation of fatty acid mixtures or technical olein and technical stearin toleic acid and stearic acid) or of fatty alcohol mixtures of oleyl alcohol and stearyl alcohol, is -of special technological significance. Similarly solid mixtures of trialycerides of fatty acids can be separated at room tempera-ture into fractions with lower and higher melting points. Such - .. - ' ,' .... ,,. .
1141'7791t fractions of triglycerides of fatty acids are used for the pre-paration of cooking fats. It is not necessary that one of the co~ponents to be separated is present as a liquid oil at room temperature. The process can also ~e used successfully when both components are solid and only differ to a sufficient degree in their melting points.
The described process can also be varied in such a manner that the vacuum evaporation step Cb) of Separation Stage I is preceded by conventional, indirectly acting cooling equip-ment, particularly a cooling step with rotating pressure coolers.
This constitutes a further improvement of the process, especial~
ly with respect to the productivity of available equipment, since the sta~ting fatty mixture now enters the vacuum evapora-tion step (b~ of Separation Stage I in a partially crystallized sta.e. The proportion of fat components precrystallized in the rotating pressure coolers is preferably from about 10 to 40 per-cen. by weight of the total higher melting components to be cry-stallized.
The special advantages of the process according to the invention are found in that the returned a~ueous dispersion -~distinctly improves the tendency of the fatty mixture to crystal-lize. This results in a considerable acceleration of the separa-tion process or a corresponding increase in the productivity ;of available equipment and a better separation effect per separation stage. In addition, there is a significant energy advantage since the cold, aqueous suspensions of higher melting fatty com-ponents from the subsequently added separation stages are used directly to cool the respective preceding steps. The separate working up of this dispersion by melting the fatty particles and .. . ~ . . . .. ~ . ~.. . . ..
11~1774 separation would require a considerable amount of energy, in addition to additional necessary equipment.
The return of aqueous dispersion of higher melting fatty components from a subsequently added separation stage into a preceding separation stage in a multiple-step separa-tion process already is the subject of German Published Ap-plication (DE-OS) No. 21 00 022. There, however, the cool-ing of the used fatty mixtures is performed exclusively with rotating pressure coolers, and the returned dispersion serves only for the dispersing of the partially crystallized fat mixtures with simultaneous cooling to the separation temper-ature. An improvem~nt of the tendency of the fatty mixtures to crystallize during the vacuum evaporation cooling could not be construed from this.
The following example is intended to illustrate the invention and is not to be construed as limiting the invention thereto.
Example Work was performed according to Example 1 of U.S.
Patent No. 3,950,371 with the difference that a two-stage separa-tor was employed. Crude stearic acid hydrolyzed from tallow at 46C (iodin~ number 58, turbidity point 39C) was used in the vacuum evaporation crystallizer of Separation Stage 1. This stearic acid was mixed with vigorous agitation with the total amount of stearin suspension of 26C obtained in the Separation Stage II. A mixing temperature of 36C was established, which nam/ -13-114177~
induced the crystallization of the higher melting stearic acid components. The further cooling to 20 C was achieved by the eva-cuation of the crystallization vessel with the aid of steam jets.
The addition of the old dilution from step (e) of Separation Stage I, with a content of 0.2% dodecyl sulfate by weight as wet-ting agent as well as additional amounts of wetting agent, elec-trolyte and water to compensate for losses, especially hy the re-moval of part of the old dilution! resulted in a separable disper-sion that was separated in a solid jacket centrifuge. The stearic acid suspension obtained in this step was heated to 90 - 95 C, and the stearic acid was separated from the old dilution in a separator. The old dilution was returned to tbe cycle - as de-scribed - after the removal of an amount of approximately 20%.
The oily phase obtained in Separation Stage I (mainly oleic acid, iodine number 82.6, turbidity point 21 C) was sub-jected to another separation in Separation Stage II, using also old dilution of Separation Stage I as wetting solution. The cool-ing to 3 - 5 C was again achieved by evaporation under vacuum.
An oleic acid fraction with an iodine number of 86 - 93 and a tur-bidity point of 1 - 5 C was obtained~ The stearin suspension containing wetting agents and electrolytes was returned to the vacuum evaporation crystallizer of Separation Stage I, after warming to 26 C.
The preceding use of a rotating pressure cooler was ad-vantageous for the improvement of the productivity of the equip-ment. The melted fatty acid entered the rotating pressure cool-er with a temperature of 46 C. After cooling to 30 C and partial 11~17~
crystallization of the higher melting portion, the fatty acid mixture was fed into the vacuum evaporation crystallizex and processed further, as described.
The preceding specific embodiments are illustrative of the practice of the invention. It is to be understood, how-ever, that other expedients known to those skilled in the art or disclosed hereinr may be employed withou~ departing from the spirit of the invention or the scope of the appended claims.
Claims (9)
1. In the process for the separation of fatty mix-tures into components with different melting points according to the rewetting process by (a) partial or complete melting of the fatty mixture; (b) cooling until the crystallization of the higher melting fatty components is achieved, with the removal of heat necessary for the cooling and crystallization of these components by the evaporation under vacuum of an aqueous phase that is in intimate contact with the mixture of fats; (c) preparing a dis-persion of liquid and solid fatty particles that are separated from one another; (d) separating this dispersion by centrifuging to obtain an oily phase containing the lower melting fatty compon-ents and an aqueous phase containing the crystallized fatty com-ponents in dispersed form; and (e) separating the higher melting fatty components from the aqueous phase by filtration or by melt-ing and subsequent centrifuging or allowing to settle out, the improvement wherein the separation process is carried out in several successive separation stages, whereby the aqueous dispersion of crystallized higher melting fatty components obtained during step (d) of a subsequent separation stage is re-cycled into the vacuum evaporation step (b) of a preceding separa-tion stage and is there combined with warmer starting mixture that has not yet been cooled to the desired separation temperature in step (b).
2. The process of Claim 1 wherein the separation is carried out in two successive separation stages.
3. The process of Claim 1 wherein mixtures of fatty acids, fatty alcohols, or glycerides of fatty acids are separa-ted.
4. The process of Claim 1 wherein the vacuum evapora-tion step (b) is preceded by a cooling step with rotating pre-sure coolers, in which from about 10 to 40% of the total higher melting fatty components to be crystallized are crystallized.
5. The process of Claim 1 which comprises the steps of:
(a) continuously, partially or completely melting a fatty substance mixture;
(b) continuously adding to the melted fatty sub-stance mixture from step (a) an aqueous dispersion comprising cry-stallized fatty components as well as wetting agent and electro-lyte solution from step (.alpha.) and continuously evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion of the fatty substance mixture has partly or completely crystallized;
(c) continuously adding aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until the separation temperature of the fatty substances is reached;
(d) continuously centrifuging the dispersion from step (c) to obtain an oily phase containing lower melting fatty components and an aqueous phase containing higher melting, cry-stallized fatty components in dispersed form;
(e) continuously separating higher melting compon-ents from the aqueous phase by filtration or by melting and subse-quent centrifuging or settling out, and recycling treated aqueous phase partially to each of steps (c), (f), and (g);
(f) continuously adding to the oily phase from step (d) an aqueous phase containing electrolyte and optionally treated aqueous phase from step (e). and evaporating part of the water under vacuum, with simultaneous intensive-mixing, until higher melt-ing fatty substance has partly or completely crystallized;
(g) continuously adding further aqueous phase from step (e) and fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until a second separation temperature is reached;
(h) continuously separating the dispersion by cen-trifuging to obtain an oily phase and an aqueous phase containing crystallized fatty components in dispersed form;
(i) continuously recycling the aqueous phase from step (h) to step (b); and (j) continuously recovering fatty substances of lower melting point from the oily phase from step (h).
(a) continuously, partially or completely melting a fatty substance mixture;
(b) continuously adding to the melted fatty sub-stance mixture from step (a) an aqueous dispersion comprising cry-stallized fatty components as well as wetting agent and electro-lyte solution from step (.alpha.) and continuously evaporating part of the water under vacuum, with simultaneous intensive mixing, until the higher melting portion of the fatty substance mixture has partly or completely crystallized;
(c) continuously adding aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until the separation temperature of the fatty substances is reached;
(d) continuously centrifuging the dispersion from step (c) to obtain an oily phase containing lower melting fatty components and an aqueous phase containing higher melting, cry-stallized fatty components in dispersed form;
(e) continuously separating higher melting compon-ents from the aqueous phase by filtration or by melting and subse-quent centrifuging or settling out, and recycling treated aqueous phase partially to each of steps (c), (f), and (g);
(f) continuously adding to the oily phase from step (d) an aqueous phase containing electrolyte and optionally treated aqueous phase from step (e). and evaporating part of the water under vacuum, with simultaneous intensive-mixing, until higher melt-ing fatty substance has partly or completely crystallized;
(g) continuously adding further aqueous phase from step (e) and fresh aqueous wetting agent and electrolyte solution, to form a dispersion of liquids and solid fats, with continued maintenance of vacuum and evaporation of water until a second separation temperature is reached;
(h) continuously separating the dispersion by cen-trifuging to obtain an oily phase and an aqueous phase containing crystallized fatty components in dispersed form;
(i) continuously recycling the aqueous phase from step (h) to step (b); and (j) continuously recovering fatty substances of lower melting point from the oily phase from step (h).
6. The process of Claim 5 wherein from 10 to 30% of the treated aqueous phase of step (e) is continuously removed from the system.
7. The process of Claim 5 wherein steps (f) to (i) are repeated prior to step (j).
8. The process of Claim l which is continuous.
9, The process of Claim 1 which is discontinuous.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP2904195.0 | 1979-02-05 | ||
| DE19792904195 DE2904195A1 (en) | 1979-02-05 | 1979-02-05 | METHOD FOR SEPARATING FATTY MIXTURES MIXED IN COMPONENTS FROM MELTING POINTS |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1141774A true CA1141774A (en) | 1983-02-22 |
Family
ID=6062142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000344071A Expired CA1141774A (en) | 1979-02-05 | 1980-01-21 | Method of separating mixtures of fatty substances |
Country Status (16)
| Country | Link |
|---|---|
| EP (1) | EP0014439A3 (en) |
| JP (1) | JPS55104398A (en) |
| AR (1) | AR220963A1 (en) |
| AU (1) | AU530343B2 (en) |
| BR (1) | BR8000662A (en) |
| CA (1) | CA1141774A (en) |
| CS (1) | CS216818B2 (en) |
| DD (1) | DD148959A6 (en) |
| DE (1) | DE2904195A1 (en) |
| DK (1) | DK14680A (en) |
| ES (1) | ES488918A0 (en) |
| HU (1) | HU183052B (en) |
| NO (1) | NO800074L (en) |
| PL (1) | PL127683B3 (en) |
| RO (1) | RO79359A (en) |
| SU (1) | SU1042622A3 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3807409A1 (en) * | 1988-03-07 | 1989-09-21 | Henkel Kgaa | METHOD FOR INSULATION OR CLEANING OF METHYL-BRANCHED, SATURATED C (ARROW DOWN) 1 (ARROW DOWN) (ARROW DOWN) 4 (ARROW DOWN) -C (ARROW DOWN) 2 (ARROW DOWN) (ARROW DOWN). 4 (ARROW DOWN) |
| CA2077914C (en) * | 1990-03-12 | 2000-05-30 | Einar Sola | Process for enrichment of fat with regard to polyunsaturated fatty acids and phospholipids, and application of such enriched fat |
| DE19602941A1 (en) * | 1996-01-27 | 1997-02-13 | Roehm Gmbh | Purificn. of (meth)acrylic ester(s) and amide(s) esp. macro-monomers from catalytic ester exchange - by centrifuging reaction mixture to remove impurities, e.g. pptd. catalyst materials, that are difficult to remove |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1915298A1 (en) * | 1969-03-26 | 1970-11-26 | Metallgesellschaft Ag | Process for the separation of fatty acid, fatty alcohol and / or fatty acid ester mixtures |
| DE2100022C3 (en) * | 1971-01-02 | 1980-04-24 | Henkel Kgaa, 4000 Duesseldorf | Process for separating mixtures of fatty substances into components with different melting points |
| BE791124A (en) * | 1971-11-11 | 1973-05-09 | Henkel & Cie Gmbh | PROCESS FOR SEPARATING FAT MIXTURES INTO DIFFERENT MELTING-FUSION CONSTITUENTS |
| DE2317563C3 (en) * | 1973-04-07 | 1979-10-04 | Henkel Kgaa, 4000 Duesseldorf | Process for separating mixtures of fatty substances into components with different melting points |
-
1979
- 1979-02-05 DE DE19792904195 patent/DE2904195A1/en not_active Ceased
-
1980
- 1980-01-10 HU HU8044A patent/HU183052B/en not_active IP Right Cessation
- 1980-01-14 NO NO800074A patent/NO800074L/en unknown
- 1980-01-14 DK DK14680A patent/DK14680A/en not_active Application Discontinuation
- 1980-01-21 CA CA000344071A patent/CA1141774A/en not_active Expired
- 1980-01-31 EP EP80100488A patent/EP0014439A3/en not_active Ceased
- 1980-02-01 DD DD80218812A patent/DD148959A6/en not_active IP Right Cessation
- 1980-02-01 PL PL1980221740A patent/PL127683B3/en unknown
- 1980-02-02 RO RO80100070A patent/RO79359A/en unknown
- 1980-02-04 AU AU55211/80A patent/AU530343B2/en not_active Expired
- 1980-02-04 JP JP1157980A patent/JPS55104398A/en active Granted
- 1980-02-04 SU SU802880650A patent/SU1042622A3/en active
- 1980-02-04 ES ES1980488918A patent/ES488918A0/en active Granted
- 1980-02-04 CS CS80756A patent/CS216818B2/en unknown
- 1980-02-04 BR BR8000662A patent/BR8000662A/en unknown
- 1980-02-05 AR AR279863A patent/AR220963A1/en active
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6337157B2 (en) | 1988-07-22 |
| NO800074L (en) | 1980-08-06 |
| RO79359A (en) | 1983-02-01 |
| DD148959A6 (en) | 1981-06-17 |
| ES8202355A2 (en) | 1981-08-16 |
| RO79359B (en) | 1983-01-30 |
| DE2904195A1 (en) | 1980-10-30 |
| SU1042622A3 (en) | 1983-09-15 |
| AU5521180A (en) | 1980-08-14 |
| EP0014439A3 (en) | 1980-09-03 |
| AU530343B2 (en) | 1983-07-14 |
| BR8000662A (en) | 1980-10-21 |
| JPS55104398A (en) | 1980-08-09 |
| ES488918A0 (en) | 1981-08-16 |
| CS216818B2 (en) | 1982-11-26 |
| PL127683B3 (en) | 1983-11-30 |
| DK14680A (en) | 1980-08-06 |
| AR220963A1 (en) | 1980-12-15 |
| HU183052B (en) | 1984-04-28 |
| EP0014439A2 (en) | 1980-08-20 |
| PL221740A3 (en) | 1980-12-15 |
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