JPH0355520B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to an improved fat and oil fractionation method for economically and economically separating components that can be used as hard butter from various raw material fats and oils, that is, components with medium melting points. Known methods for separating fats and oils include the wintering method, surfactant method, and solvent fractionation method. It can be said that the solvent fractionation method is superior because it facilitates crystallization and has good fractionation accuracy. However, on the other hand, the operating cost of the solvent fractionation method is higher than that of other fractionation methods in terms of cooling and distillation recovery of the solvent, and effective improvement in this point is a major challenge. To solve this problem, various methods have been used to reduce thermal energy using mechanical devices, such as the effective use of heat exchangers in sorting equipment.
On the other hand, it is necessary to improve crystallization by taking advantage of the characteristics of the crystallization mechanism of oils and fats. In other words, the goal is to reduce the amount of solvent used during crystallization as much as possible, which makes it possible to reduce the thermal energy required for cooling and distillation recovery of the solvent, and also eliminates supercooling during crystallization. These include reaching crystallization equilibrium and reducing cooling energy loss as much as possible. Of course, another objective is to improve the throughput by producing crystals with good separability and short elapsed time per unit area in other industrial operations. Based on this point of view, the present inventors conducted a study on the Japanese Patent Publication No. 1983-1993 in order to fractionate a medium-melting point component of good quality.
While conducting various studies using the separation method shown in Publication No. 39005 as a reference, we encountered the following problem. The crystallization and separation of high melting point components such as trisaturated glycerides in the first fractionation were carried out without any problems using conventional methods, but in the second fractionation, the middle melting point components that can be used as hard butter were separated. When normal cooling and crystallization are carried out when the oil concentration in the micella is in the range of 14% to 40%, the crystals that grow and aggregate become large crystals that embrace the liquid oil micella, and the crystals are washed away with a large amount of solvent. Even if washed with water, the entrapped liquid micella could not be washed out, and the obtained medium melting point component had no problems in separation and separation.
The quality was poor. For this reason, various studies were conducted to increase the stirring intensity to suppress the growth and aggregation of the crystals, and to make the crystals finer. However, in all cases, the crystals were found to have a wide distribution, ranging from fine needle-like ones to moderately granular ones. No matter what cloth was used, the elapsed time was long and the separation was poor. Among these, this tendency is most pronounced when acetone is used as the solvent compared to when other methyl ethyl ketone, nitropropane, and hexane are used, and this tendency is especially strong when palm oil is used as a raw material. It was. As described above, when crystallizing intermediate melting point components using conventional solvent fractionation techniques, there is a contradictory relationship between the quality of the obtained intermediate melting point component and its over-separability, and conventional methods have not been able to find suitable solutions that satisfy both. No such measures were found. The object of the present invention is to be able to separate high-quality medium-melting point components to be used as hard butter from raw material fats and oils that do not substantially contain high-melting point components, and to easily prevent excessive separation of the medium-melting point components and to prevent crystallization from occurring at an early stage. The object of the present invention is to provide a solvent fractionation method that is economical to complete. In particular, whereas conventional seeding in fractional crystallization attempts to improve transient properties by coarsening the resulting crystals, the fractionation method of the present invention uniformly refines the resulting crystals and prevents entrapment of liquid components. The purpose is to prevent this from happening. That is, in the method for fractionating fats and oils of the present invention, 1 part by weight of raw material fats and oils that do not substantially contain high melting point components is mixed with acetone.
After dissolving in 1.5 to 6 parts by weight, the above raw material fat is cooled at a temperature between 3.5°C higher than the temperature at which crystals of the medium melting point component precipitate and the temperature at which the added fat and oil crystals do not dissolve. 0.02 to 3.0% by weight of the crystallized product obtained by dissolving the same oil or fat with glyceride composition or glyceride physical properties similar to the above raw material fat in acetone and crystallizing the medium melting point component based on the above raw material fat. It is characterized by adding, cooling, crystallizing and fractionating the intermediate melting point component. Hereinafter, the method of the present invention having the above features will be described in detail. Raw material oils and fats used in the present invention that do not substantially contain high melting point components (hereinafter simply referred to as raw material oils and fats)
For example, sal fat, shea butter, palm oil, cocum fat, Borneo tallow fat, mora fat, beef tallow, lard, various hydrogenated oils and fats, and various transesterified oils and fats that do not substantially contain or have high melting point components removed. It is an oil or fat containing a hard butter component such as, and preferably one that has been purified by degumming, deacidification, decolorization, deodorization, etc. Removal of high melting point components to obtain the above-mentioned raw material fats and oils can be carried out by conventional fractionation methods such as wintering method, surfactant method, solvent fractionation method, etc., which do not remove medium melting point components. The crystallized product of fats and oils used in the present invention includes solid crystals consisting only of medium-melting-point components of fats and oils, slurries containing some non-medium-melting-point components, crystalline micella, and the like. In carrying out the present invention, first, the raw material fat is dissolved in acetone, and then cooling of the raw material fat is started. The amount of solvent added to the above raw material oil is 1.5 parts to 6 parts per 1 part of the raw material fat, but from the economic point of view, the amount should be kept to the minimum depending on the content of the medium melting point component of the raw material fat. Also, the amount added should be adjusted depending on the type of solvent and the glyceride composition of the raw material oil. For example, if the content of medium melting point components is in the range of 20% to 30%.
When the amount is in the range of 1.5 parts to 2.5 parts, and 50% to 70%, it is preferably 3.5 parts to 5 parts. A small amount of the crystallized oil and fat is added just before the crystals of the medium melting point component of the micella of the cooled raw material fat and oil are precipitated, but this is at a temperature at which the crystals of the medium melting point component of the micella of the raw material fat and oil are precipitated. more than 3.5
The temperature range is from a high temperature to a temperature at which the added crystallized fat or oil does not dissolve. As the crystallized product of the oil and fat added to the raw material fat, the same oil or fat as the raw material oil used, or one having similar glyceride composition or glyceride physical properties to the raw material oil or fat is used. For example, when palm oil from which high melting point components have been removed is used as a raw material oil, the crystallized oil to be added is as follows:
Palm oil, palm oil from which high-melting point components have been removed, medium-melting point components of palm oil, monkey fat, shea butter, etc. that are cooled and crystallized are used. In addition, even if the crystallized product of the above-mentioned fats and oils contains some crystals of high-melting point components, the final medium-melting point component has characteristics as hard butter, such as SFI (solid fat index). The amount may be any amount as long as it does not affect melting in the mouth or tempering properties as shown in . however,
Preferably it is a crystal of only a medium melting point component, and more preferably a crystal of the same medium melting point component as the raw material oil or fat. Furthermore, the finer the crystallized oil or fat to be added, the more preferable it is, more preferably needle-like crystals, and the size is preferably 20 μm or less. In the present invention, the crystallized product of the fat and oil added to the raw material fat is produced by cooling the same fat and oil as the raw material fat under high-speed stirring to finely crystallize it, but preferably the same fat and oil as the raw material fat. It is produced by dissolving in a solvent and then crystallizing it in the same manner. Further, the granular crystalline miscella (slurry containing oil crystals) of the intermediate melting point component finally obtained by the fractionation method of the present invention is pulverized into fine particles, which can also be used as the crystallized oil or fat. The amount of the crystallized oil and fat to be added depends on the type of raw material oil, the content of intermediate melting point components, the mechanical properties of the crystallization device (stirring efficiency, shape, etc.), and the amount of the crystallized oil and fat to be added. Although it varies depending on the method, it ranges from 0.02% to 3.0% based on the raw material fat. In the method of the present invention, after adding the crystallized fats and oils to the raw material fats and oils as described above, cooling is further performed to sufficiently crystallize the medium melting point component, which is filtered and separated, and the crystals are washed with an appropriate amount of solvent. The solvent is recovered to obtain a medium melting point component and a liquid oil component. INDUSTRIAL APPLICABILITY The present invention enables high quality and economical separation of medium melting point components used as hard butter from various raw material fats and oils. That is, according to the solvent fractionation method of the present invention, fractionation can be performed in a system using an extremely small amount of acetone, and the treatment of the present invention can be carried out after removing high melting point components by the conventional fractionation method. By employing a two-step fractionation process in which intermediate melting point components are efficiently fractionated, a fractionation process with extremely low loss of thermal energy can be achieved compared to conventional fractionation methods. The most important point of the present invention is that, according to the present invention, a medium with excellent quality and separation performance, which has never been obtained with conventional fractionation techniques for separating medium-melting point components, is achieved. It is possible to obtain melting point components. In particular, a remarkable effect is brought about when the intermediate melting point component to be separated is a disaturated-unsaturated triglyceride. The crystals of the intermediate melting point component obtained in the present invention are hard crystals with a well-organized particle morphology that do not entrap liquid oil easily due to the addition of fine crystal particles with a uniform particle size distribution, and therefore are suitable for crystallization. The types of equipment and their separation and operability have been greatly relaxed and improved. EXAMPLES The present invention will be described in detail below with reference to Examples, but the present invention is not limited to these Examples. Example 1 0.3 parts by weight of acetone (containing 0.3% water) was added to 1 part by weight of deoxidized and decolorized palm oil (water content 0.1%, acid value 0.3, iodine value 52.8), and after heating and dissolving this, the solution was stirred for 4 hours. After cooling to 20℃ and holding at 20℃ for 1 hour, add 0.3 parts by weight of acetone (same as above) at 15℃, hold for 10 minutes, and filter to remove the crystalline part of the high melting point component and the liquid oil. After fractionation, the crystalline portion was washed with 0.3 parts by weight of acetone at 15°C and the solvent was removed to obtain fractionated oils shown in Table 1.

[Table] Next, add 2 parts by weight of acetone to 1 part by weight of a mixture of liquid oil and cleaning oil in a proportion of yield (hereinafter abbreviated as second raw material oil), and then add 750 g of the mixture to an inner diameter of 750 g.
Transfer to a 10.5 cm 1.5 cylindrical separable flask,
After heating and dissolving the miscella, use a stirring blade with an area of 33 cm ² to
While stirring at a rotation speed of 80 rpm, cool from 50°C to 12°C (crystals of medium melting point components precipitate at 8.5°C) in 3 hours. Add 0.5 g of crystallized crystallized crystals (20μ or less in size) by cooling to 7°C with high-speed stirring, and further cooling from 12°C to 6°C in 1 hour.
After being kept at 6°C for 1 hour, it was filtered at a reduced pressure of 560 mm/Hg using a cloth with an over area of 130 cm ² at an air permeability of 40 ml/sec/cm 2 to separate the crystals of the medium melting point component and the liquid (liquid oil component) ^. Obtained. The crystals formed were fine and contained less liquid components, and the elapsed time was 5 seconds/500 ml of liquid, indicating good over-separation. The crystals were washed with 500 g of acetone at 1°C and the solvent was removed to obtain the fractionated oil shown in Table 2. Example 2 As the raw material oil, the second raw material oil of Example 1 was used, and as the crystallized oil and fat to be added, 2 parts by weight of acetone was added to 1 part by weight of the second raw material oil of Example 1,
The mixture was heated and dissolved, and then cooled to 4° C. while stirring at high speed using a homogenizer. Fractionation was carried out under exactly the same conditions as in Example 1, except that 2.5 g of crystallized misella was used. The crystals formed are fine and contain less liquid oil, and the elapsed time at this time is 5 seconds/500ml of liquid, which shows good separation properties, and the quality of the medium melting point components is as follows.
As shown in Figure 2, the results were very good. Comparative Example 1 The second raw material oil of Example 1 was used, and fractionation was carried out under exactly the same conditions as Example 1, except that oil crystals were not added. The elapsed time at this time is 5 seconds/liquid.
Although the overseparability was good at 500 ml, the quality of the medium melting point component was very poor as a large amount of liquid oil was mixed in as shown in Table 2. Comparative Example 2 Fractionation was carried out under exactly the same conditions as Comparative Example 1, except that the second raw material oil of Example 1 was used and the rotation speed of the stirring blade was 155 rpm. The time that has passed at this time is
The overseparability was poor at 135 seconds/500 ml of liquid. Furthermore, as shown in Table 2, the quality of the medium melting point component is slightly inferior to that obtained by the method of the present invention, as it contains a large amount of liquid oil. Comparative Example 3 Fractionation was carried out under exactly the same conditions as in Comparative Example 1, except that the second raw material oil of Example 1 was used and the rotation speed of the stirring blade was 170 rpm. The elapsed time at this time is 95
The overseparability was very poor at 200ml/second/liquid, and it was not possible to obtain a medium melting point component. Example 3 150 g of raw monkey fat (moisture 0.1%, acid value 0.3, iodine value 40.8) obtained by cooling and crystallizing high melting point components using hexane and 600 g of acetone were added to the crystallization apparatus (stirring blade) used in Example 1. After heating and dissolving this, cool it from 50°C to 16°C (crystals of medium melting point components precipitate at 14°C) over 3 hours while stirring at 80 rpm with a stirring blade. Add 8 g of crystallized raw monkey fat miscella (4 parts by weight of acetone added to 1 part by weight of raw monkey fat, dissolved by heating, then cooled to 2°C and crystallized while stirring at high speed with a homogenizer). Then, the mixture was further cooled from 16°C to 5°C over 1 hour and 30 minutes, kept at 5°C for 1 hour, and then subjected to the same overseparation as in Example 1. The produced crystals were fine and contained little liquid oil, and the elapsed time was 5 seconds/500 ml of liquid, and the overseparability was good. The crystals were washed with 400 g of acetone at 1°C and the solvent was removed to obtain the fractionated oil shown in Table 2. Example 4 Example 4 except that 8 g of the crystallized slurry obtained in Example 3, which had just been over-separated, was crushed with a homogenizer to a size of 20μ or less, as the crystallized oil added to the raw material oil. The separation was carried out under exactly the same conditions as in 3. The crystals formed were fine and contained less liquid oil, and the elapsed time was 5 seconds/500ml of liquid, which showed good separation properties, and as shown in Table 2, a good medium melting point component was obtained. . Comparative Example 4 Fractionation was carried out under exactly the same conditions as in Example 3, except that micella of raw monkey fat from which crystals were precipitated was not added. The elapsed time at this time is 5 seconds/500ml of liquid.
Although the overseparability was good, as shown in Table 2, the quality of the medium melting point component was poor. The SFI (solid fat index) shown in Table 2 is as follows: Examples 1 and 2 and Comparative Examples 1 and 2 were left at 26°C for 6 days, and Example 3 and Comparative Example 4 were left at 20°C.
Leave it for 2 hours at
Measurements were made in accordance with conventional methods except for repeated tempering conditions.

[Table] Comparative Example 5 750 g of 1 part by weight of the second raw material oil of Example 1 added with 2 parts by weight of hexane was heated and dissolved in the same manner as in Example 1, and then dissolved at 50°C to 8°C (medium melting point components) with stirring. (crystals precipitate at 5°C), cooled for 3.3 hours, added 0.5g of oil crystals used in Example 1, and heated to 8°C.
The mixture was cooled to -7°C over 2 hours, kept at -7°C for 1 hour, and a filtrate was obtained in the same manner as in Example 1. The filtration time at this time was 16 seconds/500ml of filtrate, and the filtration separation was not so bad. The crystals were washed with 500 g of hexane at -12°C and the solvent was removed to obtain fractionated oils shown in Table 3. As shown in Table 3, the quality of the medium melting point component was that it contained a large amount of liquid oil component, had a high iodine value, and had a low SFI value. Comparative Example 6 The second raw material oil of Example 1 was used, the amount of acetone was adjusted to 0.5 parts by weight, the oil crystals were added at 14°C (crystals of intermediate melting point components precipitated at 11°C), and fractionated at 8°C. The fractionation was carried out in the same manner as in Example 1. The filtration time at this time was 7 seconds/500ml of filtrate, and the filtration separation was good, but as shown in Table 3, the quality of the medium melting point component was that it contained a large amount of liquid oil component and had a high iodine value. The SFI value was also low. Comparative Example 7 The second raw material oil of Example 1 was used, acetone was not used, oil crystals were added at 21°C (crystals of intermediate melting point components precipitated at 18°C), and the fractionated oil was fractionated at 15°C. The separation was carried out in the same manner as in Example 1, except that washing with a solvent was not performed. At this time, the filtration time was 14 seconds/500ml of filtrate, so the filtration separation was not so bad, but the quality of the medium melting point component was as shown in Table 3, as it contained a large amount of liquid oil component and had a high iodine value. It's something
The SFI value was also low. Comparative Example 8 Fractionation was carried out in the same manner as in Example 1, except that the second raw material of Example 1 was used and the crystallized oil and fat was added at 15°C. The filtration time at this time is 36 seconds/filtrate 500
ml, it had poor filtration separation, and as shown in Table 3, the quality of the medium melting point component was that it contained a large amount of liquid oil component, had a high iodine value, and had a low SFI value. . Comparative Example 9 Fractionation was carried out in the same manner as in Example 1, except that the second raw material oil of Example 1 was used and the crystallized fat or oil was added at 7°C. The quality of the medium melting point component is not that bad as shown in Table 3, but the filtration time is
The separation by filtration was very poor at 205 seconds/500 ml of filtrate. Comparative Example 10 Fractionation was carried out in the same manner as in Example 1, except that the second raw material oil of Example 1 was used and 0.02 g of crystallized oil and fat was added. Filtration time at this time is 5 seconds/500ml of filtrate
However, as shown in Table 3, the quality of the medium melting point component is that it contains a large amount of liquid oil component γ-(p-aminophenoxy)propyltriethoxysilane and has a high iodine value. SFI
The value was also low. Comparative Example 11 Fractionation was carried out in the same manner as in Example 1, except that the second raw material oil of Example 1 was used and 12 g of crystallized oil and fat were added. The quality of the medium melting point component is not that bad as shown in Table 3, but the filtration time is 156 seconds/500
ml, and had very poor filtration separation.

【table】

Claims (1)

[Scope of Claims] 1. Dissolve 1 part by weight of raw material fats and oils substantially free of high melting point components in 1.6 to 6 parts by weight of acetone, and then cool;
At a temperature between 3.5°C higher than the temperature at which crystals of the intermediate melting point component are precipitated and a temperature at which the added fat and oil crystals do not dissolve, the same oil or fat as the raw material oil or the triglyceride composition or A crystallized product obtained by dissolving an oil with similar physical properties to glyceride in acetone and then crystallizing the medium melting point component is added at a ratio of 0.02 to 0.02 to the above raw material oil.
A method for fractionating fats and oils, characterized by adding 3.0% by weight, cooling, crystallizing and fractionating medium melting point components. 2. The method for fractionating fats and oils according to claim 1, wherein the crystallized product of fats and oils to be added is obtained by dissolving the fats and oils in acetone and then pulverizing a medium melting point component obtained by crystallization.