JPS6041694A - Separation of sterol in deodorization distillate of oil and fat - Google Patents

Abstract

PURPOSE:To reduce the amount of fractionation solvent in the separation of sterols from a deodorizing distillate by the solvent fractionation crystallization process, and to enable the separation of sterols with a small-sized separator in high efficiency, by carrying out the separation using a centrifugal precipitation separation process in combination with a centrifugal filtration process. CONSTITUTION:Sterols are separated from the deodorizing distillate produced as a by-product of the deodorization of oils or fats by solvent fractionation crystallization process (the solvent is preferably a 1-4C aliphatic alcohol such as methanol, an aliphatic carboxylic acid ester such as ethyl acetate and/or an aliphatic ketone such as acetone). In the above process, the separation is carried out by using the centrifugal precipitation separation process (preferably using a basket-type centrifugal precipitator at a centrifugal effect of 1,000- 1,500) in combination with the centrifugal filtration (preferably using a basket- type centrifugal filter at a centrifugal effect of 700-900).

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for separating sterins from deodorized distillate produced as a by-product in the deodorizing process of fats and oils.

Soybean oil, rapeseed oil, cottonseed oil, safflower oil, sunflower oil,
Rice bran oil, corn oil, coconut oil, wheat bran oil, /
Deodorized scum, deodorized sludge, hotwell soapstock, etc. produced as by-products in the deodorizing process of f-muker oil, etc. (hereinafter referred to as deodorized distillate)
contains sterins, hydrocarbons, tocopherols, glycerides, free fatty acids, etc.

These deodorized distillates contain sterine compounds at positions 1 to 35, which are used as cosmetic bases due to their emulsion stabilizing effects and moisturizing properties on the skin, and are also used as a resource for the synthesis of various steroid hormones. It can be used for pharmaceutical synthesis, as well as as a feed additive for shrimp, eel, and silkworms.

Further, tocopherols, which are contained in the deodorized distillate in an amount of about 0.1 to 20%, are useful substances as medicines, foods, or antioxidants.

Conventional methods for obtaining deodorized distillates and cytocopherol concentrates often have difficulty in processing the deodorized distillates containing sterins. Therefore, it is necessary to first separate the sterins. There are four methods that can be applied to industrial processing to normally separate sterolins: 1) Solvent fractionation crystallization method 2) Dibasic organic acid adduct method 3) Urea adduct method 4) Metal chloride adduct method Conceivable.

Among these, the operation of separating all the crystals of sterine compounds precipitated by the solvent fractional crystallization method is usually carried out by ultracentrifugation (centrifugal effect 3000
(above) or by filtration, but the disadvantages are that the equipment used for these operations becomes large and that it is often difficult to handle the separated sterins.

Further, when performing these separation operations, it is necessary to use a solvent in an amount 15 to 30 times that of the deodorized distillate due to the separation characteristics of sterolins. However, in the presence of fatty acids, sterine compounds have a certain degree of solubility in solvents, so if sterine compounds remain in the deodorized distillate that has gone through the entire separation process, they will precipitate in the subsequent process and have no effect. It often affects people. For example, when methanol is used as a solvent, the solubility of sterine compounds in the presence of fatty acids is about 2%, and the greater the amount of bath medium used, the greater the amount of sterine residues remaining. Therefore, the precipitation of sterine compounds in the post-process can be prevented by adding a third component such as hexane, toluene, or xylene, but in this case, the solvent recovery equipment becomes complicated because multiple solvents need to be recovered. .

An object of the present invention is to provide a complete method for separating sterine compounds from deodorized fat and oil distillates, which can reduce the amount of solvent used for fractional crystallization and efficiently separate sterine compounds using a small-sized separation device. It's about doing.

That is, the method for separating sterins in a deodorized distillate of fats and oils according to the present invention involves a separation operation when sterins in a deodorized distillate, which is produced as a by-product in the deodorizing process of fats and oils, is separated by a solvent fractional crystallization method. This method is characterized in that it is carried out by a combination of centrifugal sedimentation and centrifugal E-filtration.

In the present invention, the separation operation for sterolins is performed by centrifugal sedimentation and centrifugal filtration, either alone or in combination. A sufficient effect can be obtained by combining all the operations of centrifugal filtration, and in order to take advantage of the features of these unit operations, centrifugal sedimentation and centrifugation Pi1M are combined in this one @ basic separation operation. Preferably, it constitutes a part. In this way, the separation operation performed by a combination of centrifugal sedimentation and centrifugal filtration makes it possible to separate sterenes with high efficiency using a small amount of solvent, and the equipment used for each unit separation operation can be made smaller. In addition, the work is simplified and the detached sterine compounds are extremely easy to handle. In addition, in order to further improve the recovery rate of sterins and other components in the deodorized distillate, other operations such as centrifugal sedimentation and centrifugal filtration 1-W number combination, and solid content washing may be added. You can also do it.

A preferred mode of carrying out the method of the present invention can be exemplified by the separation method shown in the flow sheet below. - φ To the subsequent process, 1/3 to 1 times the amount of solvent is first added to the deodorized distillate and dissolved by heating. This dissolution temperature should be particularly limited as long as the deodorized distillate is dissolved in the solvent.

After heating and dissolving, the mixture is slowly cooled to 10 to 20°C to primarily precipitate sterins. This stock solution is fed into a centrifugal sedimentation separator, centrifugal sedimentation is performed, and the supernatant liquid is skimmed.

Next, 1 to 3 times the amount of solvent is added to the remaining solution, the solution is heated to redissolve it, and then slowly cooled to 0 to 5°C to recrystallize the sterine.

At this time, if the cooling temperature is lowered to -5 to -10°C, even the fatty acids contained will solidify and become yeast-like, making separation difficult.

Next, this stock solution is supplied in a manner similar to centrifugal filtration, and centrifugal filtration is performed. 2/3 to 1 times the amount of the same solvent is added to the obtained separated solid content, and the inside of the machine is washed to improve the oil recovery rate. Furthermore, the supernatant liquid from the centrifugal sedimentation and the F solution from the centrifugal filtration are mixed, heated and dissolved, and then slowly cooled to θ ~ 5°C to recrystallize the remaining sterins. Separate sterins. In this method, the separation characteristics are further improved by filtering the undissolved matter during the recrystallization operation while hot.

The centrifugal sedimentation separator used in the present invention is preferably a basket type centrifugal sedimentation separator, and the centrifugal effect is 1
It is preferable that it is 000-1500. In addition, the centrifugal filter is preferably a basket-type centrifugal filter, and the centrifugal effect is preferably 700 to 900. By using such a highly versatile centrifugal separator with a low centrifugal effect, work becomes easier and labor savings are achieved.

As the solvent used in the present invention, any known solvent may be used, such as aliphatic alcohols having 1 to 4 carbon atoms such as methanol, ethanol, impronol, imbutanol, aliphatic alcohols such as ethyl acetate, etc. Caldic acid ester 1. (Tyl in butyl ketone, methyl ethyl ketone,
Preferably, it is an aliphatic ketone such as acetone.

These solvents may be used alone or in combination.
Two or more types of C may be appropriately mixed and used. Although the shape of the crystals of the sterine to be separated changes depending on the solvent used, it is possible to achieve almost uniform separation regardless of these shapes. In addition, the isolated sterins have good dehydration properties and are easy to handle.

The present invention will be described below with specific examples. Although it will be explained in more detail, the embodiments of the present invention are not limited thereto.

Example 1 The method of the present invention was carried out according to the flow sheet and using methanol as a solvent.

(a)-Next precipitation/centrifugal sedimentation deodorized distillate (rapeseed oil) 38.2 kg (inner sterine 10
．． 28 kg) methanol 9.93 kfl The deodorized distillate excluding sterins is collectively referred to as oil. same as below.

(b) Recrystallization (1), centrifugal filtration (1) Methanol during recrystallization 29.8kl? (c) Recrystallization (2) centrifugal filtration (2) (2) Centrifugal filtration (2) Recrystallization (2) Centrifugal filtration (2) When the above results are summarized, Sterine recovery rate: 95.2% Oil recovery rate: 99.0% Example 2 Example 1 The method of the invention was carried out in a similar manner as in Example 1, using isopropanol as the solvent.

(a)-Next precipitation centrifugal sedimentation deodorized distillate (soybean oil) 40.0 kg (inner sterins 8.8 ml) Impropanol 50.9 hours (b) Recrystallization (1) Centrifugal filtration (1) Inpropanol at the time of recrystallization: 50.9 klj (c) Washing: Inzorono and Nor at the time of washing: 12.7 kg) Recrystallization (2) Centrifugal filtration (2) Summarizing the above results, solid content recovery rate: 95.5% Oil recovery Rate: 99.5% Example 3 The method of the present invention was carried out in the same manner as in Example 1, using acetone as the solubilizer.

(a)-Next precipitation Centrifugal sedimentation deodorized distillate (cottonseed oil) 45.0 kg (inner sterine 7.
8 kg) Acetone 113.8ky (b) Recrystallization (1
) Centrifugal filtration (1) Acetone during recrystallization 26.0 kg (c) Acetone during washing 17. rkg) Recrystallization (2) Centrifugal filtration (2) When all the above results are totaled, solid content recovery rate is 97.6 (4) Oil content recovery rate 80.8 (%) Procedure amendment book Shoga 058 can December 9th Patent Office Commissioner Kazuo Wakasugi1, Indication of the case, Patent Application No. 1982-1492402, Name of the invention, Method for separating sterine compounds in deodorized oil and fat distillate 3, Relationship with the amended person case Patent Applicant address: 40 Mori Building, Toranomon 5-13-1, Minato-ku, Tokyo Column 6 of the detailed explanation of the invention in the specification, Contents of amendment (1) "Filtration" is written on page 3, line 12 of the specification. "filtration"
I am corrected.

(2) r 46.0 in the “total” line in the top table on page 10 of the same book
6Ky J, r 37.63Kg-1 and r8.43
~”, respectively r46.06J and r37.63
J and r8.43J.

Claims (3)

[Claims] (1) When separating sterine compounds in the deodorized distillate produced as a by-product in the deodorizing process of fats and oils by a solvent fractional crystallization method, the separation operation is performed by a combination of centrifugal sedimentation and centrifugal filtration. A method for separating sterolins in deodorized oil and fat distillates. (2) The sterine compound in the oil and fat deodorized distillate according to claim (1), wherein the solvent is an aliphatic alcohol having 1 to 4 carbon atoms, an aliphatic caldic acid ester, an aliphatic ketone, or a mixture thereof. separation method. (3) The centrifugal sedimentation is carried out using a basket-type centrifugal sedimenter at a centrifugal effect of 1000 to 1500, and the centrifugal filtration is carried out using a basket-type centrifugal filter at a centrifugal effect of 700 to 900. A method for separating sterolins in deodorized oil and fat distillates.