JPS624787A - Fractionation of oils and fats - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Technical Field) The present invention relates to a method for fractionating high-quality liquid fractions and solid fractions with good yield from natural and/or synthetic oils and fats containing triglyceride components having different melting points.

(Prior Art) Conventionally, as a method for fractionating triglyceride components having different melting points contained in fats and oils, a fractionation method using a solvent such as acetone or hexane has been exclusively carried out. Normally, when multiple fractions of fats and oils are fractionated in multiple stages, the type of solvent is not changed from beginning to end during the fractionation process because it is easy to perform continuously or can be performed at low manufacturing cost. The same type of solvent has been used throughout. For example, in Japanese Patent Application Laid-Open No. 53-84009,
In all of the examples, the same type of solvent is used to separate the desired liquid fraction and intermediate melting point fraction.

(Problem to be solved by the present invention; Objective) However, in recent years, the demand for quality improvement has been increasing, and in view of this demand, liquid fractions and solid fractions conventionally obtained by fractionation using the same type of solvent The quality of the solvent depends on the type of solvent, so if one is high quality, the other is low quality, and it has been found that the quality of both parts is not superior, and there is still room for improvement. Ta.

By the way, hexane, which is conventionally known as a low polar solvent,
Compared to acetone, which is known as a polar solvent, it has excellent fractionation ability for each triglyceride component due to the difference in melting points such as low melting point, medium melting point, and high melting point, and because it hardly dissolves water, it can easily remove water from contamination. Although it has advantages such as being able to be removed, it has disadvantages such as poor fractionation ability for impurities such as diglyceride components and the need for large-scale cooling equipment and costs due to the low separation temperature. On the other hand, acetone, which is a polar solvent, has superior ability to separate impurities such as diglyceride components compared to hexane and has a high separation temperature, so it is economical because it requires only small-scale cooling equipment. It has poor fractionation ability and impurities such as diglyceride components are concentrated in the low melting point fraction, resulting in poor stability when used as frying oil, etc. Furthermore, since it is soluble in water, it is susceptible to water contamination. It has disadvantages such as the fact that the sorting conditions are easily influenced.

As described above, the conventionally used fractionation methods using solvents such as hexane or acetone each have their own advantages and disadvantages.
The object of the present invention is to fractionate high-quality liquid fractions and solid fractions from fats and oils in good yield by taking advantage of the advantages of these two types of solvents.

(Means for solving the problem; configuration) As a result of intensive research in view of the above points, the present inventors have found that the quality of the liquid fraction and/or solid fraction separated by changing the solvent during the fractionation process is lower than that of the conventional method. The present invention was completed based on the findings that the quality of the two fractions was superior and the yield was unexpectedly higher.

That is, in the present invention, when fractionating fats and oils into triglyceride components based on the difference in melting point using a solvent, the low melting point fraction is first fractionated using a low polar solvent, and if necessary, the high melting point fraction is further separated from the crystal part. It is a fractionation method for fats and oils that consists of removing part or all of the solvent, then adding a polar solvent and re-fractionating it into a medium-melting point fraction and a low-melting point fraction. be.

The present invention will be explained in detail below.

First, in the present invention, it is necessary to first fractionate the low melting point fraction using a low polar solvent, and by performing this treatment first, a high quality liquid fraction with a high iodine value can be obtained in high yield. It can be obtained by

On the other hand, when polar solvents are used, large amounts of impurities such as diglyceride components and gum components are mixed in, which does not meet the strict quality requirements of recent years. If a process of separating a medium-melting point fraction and a low-melting point fraction is carried out, only a low-quality liquid fraction with a low iodine value is obtained.

Normally, such liquid fractions are more stable than liquid oils such as salad oils, so they are used for frying or mayonnaise. Stable fats and oils with a low content of impurities such as diglyceride components and gums are required, and the low melting point fraction obtained by the present invention fully satisfies these requirements.

Next, the high melting point fraction is fractionated and removed from the other crystal part from which the low melting point fraction was fractionated, using the same solvent if necessary. It is better to perform a treatment to remove the high melting point fraction at this point, and by performing such treatment, impurities such as diglyceride components or gum components are removed, even if the amount is small or trace, so that the high melting point fraction can be removed in subsequent steps. The quality of the solid fat fraction produced is excellent.

Thereafter, in the present invention, the initially used low polar solvent is distilled off, and a new polar solvent is added for refractionation. The low polar solvent to be distilled off does not necessarily have to be the entire amount, and may be a mixed solvent in which a portion of the low polar solvent remains in the newly added polar solvent, but preferably the entire amount is replaced. It is better to In this way, a medium melting point fraction and a low melting point fraction are fractionated using a polar solvent or a mixed solvent. The intermediate melting point fraction separated here has extremely low impurities such as diglyceride components and gum components, so that it can withstand use as a hard butter fraction. It can be obtained in high yield.

In the present invention, examples of low polar solvents include petroleum ether, hexane, heptane, octane, nonane, etc., and examples of polar solvents include acetone, methyl ethyl ketone, etc.

In addition, the oils and fats that can be applied in the present invention include shea butter,
Examples include natural oils such as palm oil, sal fat, mango kernel oil, ace-ino oil, mora oil, and kanya oil, as well as synthetic oils such as enzyme-transesterified oils. A part of the high melting point fraction may already be removed by acid treatment or as appropriate, and it is particularly preferable that the acid value is 5 or less.

(Effects of the Invention) As described above, the present invention first performs multi-stage fractionation of fats and oils by sequentially using a low polar solvent and then a polar solvent to separate liquid fractions and solid fractions of excellent quality in high yield. It became possible to take it. In particular, in the case of solvent fractionation, it is extremely economically advantageous to increase the yield of the intermediate melting point fraction, which has high utility value, by 1%, and efforts have been made to increase the yield even by a small amount. From this point of view, the method of the present invention makes it possible to separate a high-quality medium-melting point fraction suitable for use as a hard butter fraction at a high yield, several percent higher than that of the conventional method (see Comparative Example 2 below). ), which has a very remarkable effect.

(Examples) Below, Examples and Comparative Examples will be illustrated to further clarify the effects of the present invention, but it goes without saying that these are merely illustrative and the spirit of the present invention is not limited by such illustrative examples. stomach.

Example 1 Iodine (il) containing 7.7% by weight of diglyceride component
1 part by weight of palm olein of li 57.2 was added to 1 part by weight of hexane.
Micella mixed and dissolved in parts by weight was cooled while stirring to precipitate crystals, and kept at -15°C for 1 hour. After that, it is filtered and fractionated into a crystal part and a filtrate part, and the crystal part is further divided into 11 parts.
After washing with 1 part by weight of hexane at 5°C, the mixture was filtered again and the filtrate was combined with the previous filtrate. The yield of oil and fat recovered by removing the solvent from the crystalline part (relative to palm olein, the same applies hereinafter) is 39
．． At 0% by weight, the iodine fi was 39.9 and the diglyceride component content was 6.8% by weight. The liquid fraction recovered from the filtrate had a high yield of 61.0% by weight and an iodine value of 68.4.
The diglyceride component content was 8.4% by weight, and the cloud point was as low as 2°C, making it suitable as a frying oil. On the other hand, 1 part by weight of the fats and oils recovered by removing the solvent from the crystalline part was dissolved in 1 part by weight of acetone, cooled to 5°C with stirring and held for 20 minutes, and separated into a crystallized part and a filtrate part by filtration. The crystalline portion was washed and filtered with 1 part by weight of acetone at 5°C. Thereafter, the crystalline portion was removed from the solvent to obtain a medium melting point fraction with a yield of 25.7% by weight. Both of the components thus obtained had an iodine value of 33.4 and a diglyceride component content of 1.2% by weight. Jensen is a mixture of 50 parts by weight of this palm mid-melting point fraction and 50 parts by weight of shea stearin with an iodine value of 39.0.
) The maximum temperature reached (TMax) in the method cooling curve is 28
It had a fairly high c of 9'c, and the crystal transition was fast, making it suitable as a hard putter.

Example 2 In Example 1, the oil concentration of the hexane micella obtained by heating and melting the crystal part during the first stage fractionation with -xane was adjusted to 33ffi%, and then cooled to 5 ° C. The crystal part that precipitated after holding for a minute was fractionated by filtration. The high melting point fraction after solvent removal had a yield of 1.9% by weight, an iodine value of 30.0, and a diglyceride component content of 30.2% by weight. After removing the solvent from the filtrate, it was redissolved in 9 parts by weight of acetone, the micella was cooled with stirring and held at 4°C for 20 minutes, and then fractionated into a crystal part and a filtrate part by filtration. The crystalline portion was similarly washed with 1 part by weight of acetone, and then the solvent was removed to obtain a medium melting point fraction with a yield of 26.6% by weight, an iodine value of 35.0, and a diglyceride component content of 1.2% by weight. The maximum temperature reached (TMax) in the Jensen method cooling curve of this mixed oil of 50 parts by weight of palm mid-melting point fraction and 50 parts by weight of shea stearin with an iodine value of 39.0 is extremely high at 29.4°C. ,
When used in chocolate as 7X-Dochter, it exhibited excellent mold release and shrinkage properties.

Comparative Example 1 In Example 2, the filtrate obtained by filtering off the crystalline part (high melting point fraction) after the second stage fractionation with hexane was adjusted to an oil and fat concentration of 10% by weight without removing the solvent, and then stirred and cooled. -12℃
After holding for 20 minutes, the crystalline portion precipitated was fractionated by filtration. After washing the crystalline portion with 1 part by weight of hexane at -12° C., the crystalline portion was desolvented to obtain a medium melting point fraction with a yield of 26.6% by weight. This palm mid-melting point fraction has an iodine value of 34.4.
However, the diglyceride component content was 5.2% by weight, which was much higher than that of the intermediate melting point fraction obtained in Examples 1 and 2. The maximum temperature reached (TMax) in the Jensen method cooling curve of the mixed oil and fat was 27.8°C.
It was low. When used in chocolate as hard butter, mold warming and shrinkage properties were inferior to those of Examples 1 and 2 when tempered and cast under similar conditions.

Comparative Example 2 1 part by weight of palm olein, the same as that used in Example 1, was mixed and dissolved in 4 parts by weight of acetone, and the miscella was maintained at 3° C. for 1 hour while stirring and cooling. The crystalline portion was fractionated by filtration and further washed with 1 part by weight of acetone at 3°C. The yield of the liquid fraction obtained by removing the solvent from the filtrate combined with the washing solution was 46.5% by weight, which is lower than the yield in Example 1 using hexane, and the yield was lower than that of Example 1 when hexane was used.
．． 0 and the diglyceride component content is 12.3% by weight.
There were many.

This liquid fraction appeared cloudy when left at room temperature (approximately 20° C.) for a week. On the other hand, the crystal part is heated to melt and the fat concentration is 1.
After adjusting the acetone miscella to 0% by weight, the mixture was cooled to 7°C with stirring, kept for 1 hour, and then fractionated into a crystal part and a filtrate part by filtration. After washing the crystalline portion with acetone at 7°C, the solvent was removed to obtain a palm mid-melting point fraction with a yield of 22.3% by weight, an iodine value of 35.0, and a diglyceride component content of 0.8% by weight.

Add 50 parts by weight of both of these to 50 parts by weight of shea stearin as in the previous example.
Jensen, a mixed oil and fat blended with parts by weight.
) The maximum temperature reached (TMax) in the method cooling curve is 2
The temperature was as high as 9.2°C, but as mentioned above, the yield was 22.3% by weight, which was considerably lower than in Examples 1 and 2.

Claims (3)

[Claims] (1) When fractionating fats and oils into triglyceride components with different melting points using a solvent, the low melting point fraction is first fractionated using a low polar solvent, and if necessary, the high melting point fraction is further extracted from the crystalline part. A method for fractionating fats and oils, which comprises removing a fraction, distilling off part or all of the solvent, and then adding a polar solvent to refractionate into a medium melting point fraction and a low melting point fraction. (2) The method according to claim (1), wherein the low polar solvent is a single or mixed solvent of hydrocarbon compounds such as petroleum ether, hexane, heptane, octane, and nonane. (3) The method according to claim (1) or (2), wherein the polar solvent is acetone or methyl ethyl ketone.