JP4586220B2 - Separation of unsaponifiable matter from shea butter - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for separating unsaponifiable matter in shea butter, and more particularly to a method for insolubilizing unsaponifiable matter by mixing shea butter with a polar organic solvent to separate and remove it.
[0002]
[Prior art]
Shea fat is used in large quantities in chocolate and the like because its fractionated fat has excellent properties as a tempering type hard butter. Tempering type hard butter is similar to cocoa butter in its composition and physical properties, and as a substitute for cocoa butter, or for the purpose of preventing so-called fat bloom where the surface of chocolate products is whitened or powdered inside It is blended in chocolate.
Usually, shea fat contains several percent of a high-melting point unsaponifiable product mainly composed of isoprene polymer. If this is not removed, the workability in the chocolate production process is deteriorated and the texture of the chocolate is lowered, which is not preferable. For this reason, various studies have been made in the past regarding the removal of unsaponifiable matter of shea fat. Japanese Patent Publication No. Sho 41-17465 proposes a method for removing high-melting point unsaponifiable matter from shea fat, and Japanese Patent Laid-Open Publication No. 61-42595 proposes a method for degumming shea fat. In these methods, polar organic solvents such as acetone and methyl ethyl ketone are mixed with shea butter, and the unsaponifiable matter contained in shea butter is insolubilized by holding the mixture for a certain period of time while stirring and mixing. This was separated and removed by a solid-liquid separation method such as filtration and centrifugation.
[0003]
In the conventional method of separating unsaponifiable matter from shea fat, in order to insolubilize the unsaponifiable matter, the mixture of shea fat and polar organic solvent is kept at a constant temperature (for example, 24 ° C.), and stirring is gentle and requires a long time. Was. Consideration has been made not to break the precipitated crystals, either because it is performed as a separate process. Thus, since it must be held for a long time of 10 minutes to 60 minutes, it was necessary to increase the equipment scale in order to increase the processing amount. Further, the insolubilized unsaponifiable matter is dispersed in the mixed solution and is very fine, so the filtration rate is slow and the efficiency is poor. In order to increase the efficiency, it is necessary to increase the filtration area, so that the capital investment is increased. In addition, in this method, part of the oil / fat portion is removed by being compatible with the unsaponified product, which is a factor that hinders the yield reduction of the shea fat and the effective use of the unsaponified product.
[0004]
[Problems to be solved by the invention]
It is an object of the present invention to provide a method for separating unsaponifiable matter from shea fat, which has a short time until insolubilization and coagulation sedimentation, suppresses equipment scale and capital investment, has high separation efficiency and good separation accuracy. .
[0005]
[Means for solving the problems]
The present invention is a method of separating and removing unsaponifiable matter after the step of insolubilizing unsaponifiable matter by mixing shea butter and a polar organic solvent in the method for separating unsaponifiable matter from shea fat. However, the insolubilizing step is a step of mixing a mixture of shea butter and a polar organic solvent in a temperature range of 20 ° C. to 40 ° C. so that the Reynolds number is 5,000 or more and 200,000 or less. When the mixture is allowed to stand separately for 1 minute, unsaponifiable matter in the supernatant liquid cannot be detected. Unsaponifiable matter is agglomerated and separated and removed. Saponification separation method.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
The shea butter referred to in the present invention is a fat collected from the fruit of a natural tree called Baia Parkii that is produced in the West Coast of Africa, Nigeria and the like, and is usually fractionally purified and used as a substitute fat for cacao. However, as is well known, shea fat naturally contains 1 to 10% unsaponifiable matter, and if shea fat is used in chocolate as a substitute for cacao without removing unsaponifiable matter, Viscosity increases, tempering becomes extremely difficult, and the mouthfeel of the chocolate product becomes worse. Conventionally, unsaponifiable materials are mainly isoprene polymers, terpenes and sterols.
[0007]
The polar organic solvent referred to in the present invention is an aliphatic organic monohydric alcohol having 1 to 4 carbon atoms such as methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol and its isomer as a strong polar organic solvent, Examples of acetone, methyl ethyl ketone, and low polarity organic solvent include hexane. Acetone is preferable from the viewpoint of the dissolving power of fats and oils. A mixed solvent of a strong polar organic solvent such as ethyl alcohol and a low polar organic solvent such as hexane may be used.
[0008]
In the present invention, it is preferable that the mixture of the shea fat and the polar organic solvent is vigorously mixed so that the Reynolds number is 5000 or more and 200000 or less, and the unsaponified product is aggregated to be separated and removed. Examples of the method of intensive mixing include a line mixer, a static mixer, a stirrer, a fluid circulation or a sparging method.
Separation may be any of natural sedimentation, filtration, and centrifugation, and the unsaponifiable product and solvent layer are separated at the end of powerful mixing. When the Reynolds number is less than 5000 with respect to the mixture of the shea fat and the polar organic solvent, the insolubilized unsaponifiable matter is finely dispersed, resulting in poor separation efficiency. When the Reynolds number exceeds 200,000, the effect corresponding to the increase in mixing energy cannot be obtained.
[0009]
The mixing conditions for achieving the Reynolds number differ depending on the mixing apparatus. For example, when mixing by rotating a stirring blade in a cylindrical tank, the peripheral speed is usually 0.9 m / min for a mixture of shea fat and a polar organic solvent. It is often in the range of stirring and mixing in the range of sec to 45 m / sec and stirring power of 0.5 W / kg to 10 KW / kg. When the stirring is less than 0.9 m / sec or the stirring power is less than 0.5 W / kg, the insolubilized unsaponifiable matter is finely dispersed, resulting in poor separation efficiency. If the stirring exceeds 45 m / sec or the stirring power exceeds 10 KW / kg, the effect corresponding to the increase in stirring energy cannot be obtained.
The unsaponifiable matter dispersed in the shea fat is aggregated in a much shorter time than before by vigorous mixing, and the separation efficiency is high and the separation accuracy is very good.
[0010]
In the present invention, when strongly mixing the mixture of shea butter and polar organic solvent so that the Reynolds number is 5000 or more and 200,000 or less, 1.5 to 20 parts of polar organic solvent is added to 1 part of shea butter. Is preferred. More preferably 3 to 6 parts are added. The temperature of the mixture at this time is preferably 20 ° C to 40 ° C. For example, if the temperature of the mixture is too high as 55 ° C., the organic solvent evaporates, and if the temperature of the mixture is too low as 15 ° C., for example, oily crystals will precipitate, so that these temperatures do not occur. Should be selected. When the polar organic solvent is less than 1.5 parts with respect to 1 part of the shea fat, oily fat crystals of the shea fat are precipitated, making it difficult to separate from the unsaponified product. Moreover, when the amount of the polar organic solvent exceeds 20 parts relative to 1 part of the shea fat, it is not economical and not preferable.
[0011]
【Example】
EXAMPLES The present invention will be described in more detail with reference to the following examples, but the spirit of the present invention is not limited to the following examples. In the examples, “%” and “part” mean weight basis.
[0012]
Example 1
The deoxidized shea fat that has been heated to 50 ° C to completely melt the fat crystals is cooled to 35 ° C, and 5 parts of acetone with a purity of 99.0% adjusted to 30 ° C in advance is added to 1 part of the deoxidized shea fat. It was. 1 kg of this mixture was stirred for 5 minutes at a Reynolds number of 10700, a peripheral speed of 2.9 m / sec, and a stirring power of 3.7 W / kg. After completion of the stirring, the mixture was placed in a Nutsche having a diameter of 150 mm and ADVANTECTOYO filter paper NO. 2 was vacuum filtered. The time required for filtration was 10 seconds and the filterability was good. The size of the precipitated unsaponifiable particles was confirmed in the state of the filter paper after filtration. Since the unsaponifiable matter was agglomerated, the particles were large and did not spread over the entire filter paper (FIG. 1).
Further, in order to investigate the sedimentation property of the unsaponifiable matter that had been precipitated, deoxidized shea butter and acetone were mixed and stirred in the same manner as described above, and after treatment under the same conditions, the mixture was transferred to a 200 ml graduated cylinder, immediately after 10 seconds, Visual confirmation was performed after 5 minutes. Immediately after the transfer to the graduated cylinder, sedimentation began, and after 10 seconds, the unsaponifiable matter was completely deposited on the bottom of the graduated cylinder, and there was no particle that could be visually confirmed in the supernatant (FIG. 3). After 1 minute, the supernatant was collected and the unsaponifiable matter contained in the solution was measured, but no unsaponifiable matter was detected.
[0013]
Example 2
Deoxidized shea butter that has been completely heated to 50 ° C and melted the fat crystals is cooled to 35 ° C, and 3 parts of 99.8% pure acetone adjusted to 30 ° C in advance is added to 1 part of deoxidized shea butter. It was. 1 kg of this mixture was stirred for 2 minutes at a Reynolds number of 16000, a peripheral speed of 4.4 m / sec, and a stirring power of 12.3 W / kg. After completion of the stirring, the mixture was placed in a Nutsche having a diameter of 150 mm and ADVANTECTOYO filter paper NO. 2 was vacuum filtered. The time required for filtration was 10 seconds and the filterability was good.
[0014]
Example 3
The deoxidized shea butter that has been completely melted with heating to 50 ° C is cooled to 35 ° C, and 19 parts of 99.0% pure acetone adjusted to 30 ° C in advance is added to 1 part of deoxidized shea butter. It was. 1 kg of this mixture was stirred for 5 minutes at a Reynolds number of 10700, a peripheral speed of 2.9 m / sec, and a stirring power of 3.7 W / kg. After completion of the stirring, the mixture was placed in a Nutsche having a diameter of 150 mm and ADVANTECTOYO filter paper NO. 2 was vacuum filtered. The time required for filtration was 10 seconds and the filterability was good.
[0015]
Example 4
Deoxidized shea butter, which has been heated to 50 ° C. and completely melted the fat and oil crystals, is cooled to 35 ° C., and 6 parts of 99.8% pure acetone adjusted to 25 ° C. in advance is added to 1 part of deoxidized shea butter It was. 1 kg of this mixture was stirred for 5 minutes at a Reynolds number of 5030, a peripheral speed of 0.9 m / sec, and a stirring power of 0.6 W / kg. After completion of the stirring, the mixture was placed in a Nutsche having a diameter of 150 mm and ADVANTECTOYO filter paper NO. 2 was vacuum filtered. The time required for filtration was 10 seconds and the filterability was good.
[0016]
Example 5
Deoxidized shea butter, which has been heated to 50 ° C and completely melted the fat crystals, is cooled to 35 ° C, and 3 parts of acetone with a purity of 99.0% adjusted to 25 ° C in advance is added to 1 part of deoxidized shea butter. It was. 1 kg of this mixture was stirred for 5 minutes at a Reynolds number of 6900, a peripheral speed of 1.2 m / sec, and a stirring power of 1.4 W / kg. After completion of stirring, the mixture was centrifuged at 3500 G for 2 minutes to separate the precipitated unsaponifiable matter. After separation, the unsaponifiable matter contained in the supernatant was measured, but no unsaponifiable matter was detected.
[0017]
Comparative Example 1
In the same manner as in Example 1, deoxidized shea butter and 99.0% purity acetone were mixed, and 1 kg of this mixture was mixed with ordinary stirring, a Reynolds number of 3300, a peripheral speed of 0.6 m / sec, and a stirring power of 0.2 W / kg. Performed for 45 minutes. After the stirring, when vacuum filtration was performed under the same conditions as in Example 1, the unsaponifiable matter spread over the entire filter paper, and the filter paper was clogged, and the vacuum filtration could not be continued unless the filter paper was replaced. Filterability was poor. The size of the precipitated unsaponifiable matter particles was confirmed in the state of the filter paper after clogging. The unsaponifiable matter was fine and spread throughout the filter paper (Fig. 2).
In addition, in order to examine the sedimentation property of the unsaponifiable matter, deoxidized shea butter and acetone were mixed and stirred in the same manner as described above, treated under the same conditions, and then the mixture was transferred to a 200 ml graduated cylinder. Later, visual confirmation was performed. Immediately after the transfer to the graduated cylinder, unsaponifiable matter deposited on the entire graduated cylinder drifted. After 10 seconds, a large portion of the unsaponifiable matter that began to deposit began to accumulate at the bottom of the graduated cylinder, but most remained floating. After 5 minutes, the particles were deposited up to 2 ml, but the fine particles drifted to the top, and could not be separated by natural sedimentation (Fig. 4). After 1 minute, the supernatant was collected and the unsaponifiable matter contained in the solution was measured. As a result, 0.8% unsaponifiable matter was detected in the supernatant.
[0018]
【The invention's effect】
According to the present invention, in the method for separating unsaponifiable matter from shea butter, the time to insolubilization and coagulation sedimentation is short, the scale of equipment and the equipment investment are suppressed, the separation efficiency is high, and the separation accuracy is high. Is now possible.
[Brief description of the drawings]
FIG. 1 is a schematic diagram showing the size of precipitated unsaponifiable matter particles in Example 1, and the state after filtration. FIG. 2 is a schematic diagram showing the size of particles in Comparative Example 1, precipitated unsaponifiable matter. Fig. 3 Example 1 visual confirmation of sedimentation in a 200 ml graduated cylinder. Fig. 4 Comparative example 1 visual confirmation of sedimentation in a 200 ml graduated cylinder.

Claims (4)

In the method for separating unsaponifiable matter from shea butter, a method for separating and removing unsaponifiable matter after the step of mixing the shea butter with a polar organic solvent to insolubilize the unsaponifiable matter. However, the insolubilizing step is a step of mixing a mixture of shea butter and a polar organic solvent in a temperature range of 20 ° C. to 40 ° C. so that the Reynolds number is 5,000 or more and 200,000 or less. When the mixture is allowed to stand for 1 minute in an agglomerated state, unsaponifiable matter in the supernatant cannot be detected. A mixture of shea butter and a polar organic solvent is stirred and mixed at a peripheral speed of 0.9 m / sec to 45 m / sec and a stirring power of 0.5 W / kg to 10 KW / kg to agglomerate and separate and remove the unsaponifiable matter. The method of claim 1. The method of Claim 1 or Claim 2 which polar organic solvent mixes 1.5-20 parts with 1 part of shea fats. The method according to any one of claims 1 to 3, wherein the polar organic solvent is acetone.

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