SU794018A1 - Method of preparing phytosterol - Google Patents

Description

(54) METHOD FOR PRODUCING PHYTOSTEROL

one

This invention relates to an improved process for the preparation of a phytosterian which finds use in the pharmaceutical and cosmetic industry as a bioactive emulsifier and base for ointments and creams.

A known method for producing phytosterol is by dissolving phytosterol nitrile in ethanol and clarifying the alcohol solution with hydrogen peroxide in order to obtain a clarified phytosterol suitable for use as a bioemulsifier. This method allows the complex use of valuable components that are part of raw phytosterol (solid soaps — salts of fatty and resin acids, lignocerol alcohol, and sterol alcohols). After clarification, the solution is cooled, the precipitate of phytosterol is separated from the mother liquor and dried at 30-60 ° DJ.

However, this method is multi-stage, long-lasting, requires a large amount of solvents, which complicates and increases the cost of further cooling, crystallization and filtration, and also reduces the yield of the finished product.

A method of producing phytosterol is used, in which, along with raw phytosterol, solid soaps and bottoms production of phytosterol produced during the purification of raw phytosterol are used as sterol-containing raw materials. In this method, the sterol-containing raw material is dissolved in a 10-fold amount of 70% propyl alcohol at 60-70 s and stirred for 1.0-1.5 hours. The solution is clarified with 33% hydrogen peroxide, which is added to the amount of I / IO part of the solution. The clarified solution is cooled to 10-13 ° C and crystallized at this temperature for 10-12 hours. The crystals of the clarified phytosterol are separated from the mother liquor by filtration and dried.

0 at 30-B C, after which the phytosterol is ground to a powder. The output of phytosterol 60-70% of the loads of 9n dry matter C2,

 The disadvantages of the method are the duration and laboriousness of the filtration process due to the smearing of the pores of the filter materials with solid soaps, the large loss of solvent in the filtration process, the duration

0 drying of phytosterol and the appearance of solid soaps on the surface of phytosterol lumps from yellow to brown. This impairs the quality and appearance of the finished product.

The disadvantage of this method is also the melting of phytosterol crystals during grinding due to the heating of the rubbing parts of the grinding device, which leads to a reduced yield of the finished product.

The purpose of the invention is to eliminate these drawbacks inherent in the known method for producing phytosterol, and to increase the yield of the target product.

The goal is achieved by the fact that in the method of obtaining phytosterol by treating sterol-containing raw material - raw phytosterol, solid soaps and bottoms - with isopropyl alcohol when heated and with hydrogen peroxide followed by drying the clarified phytosterol, the clarified phytosterol is dried directly from the solution by spraying it onto the fluoroplastic fluoroplastic nozzle in the current of the gaseous coolant — air or carbon dioxide; and during the drying process, the temperature of the dried target product is maintained to the limit x 20-40 s.

A distinctive feature of the described method is that the bleached phytosterol is dried directly from the solution by spraying it on the flowing inert packing in a stream of gas coolant and during drying the temperature of the dried target product is maintained within 20-40 0.

The advantage of this method is to simplify the drying process of the target product and increase its yield up to 80%.

The flowing fountain is used with an inert fluoroplastic to eliminate the interaction of the hot solution with the packing material and not to degrade the quality of the finished product.

The technology of the method is as follows.

Sterol-containing raw materials (raw phytosterol, solid soaps and bottom residues obtained from the purification of raw phytosterol) are dissolved in a 10-fold amount of 70% isopropyl alcohol at 50-bO S. and stirred for 0.5-1.0 The solution was then clarified with 33% hydrogen peroxide, which was added in an amount of 1/10 of the solution. The clarified solution at 50-60 ° C is sprayed onto the flowing inert nozzle in a current of heat carrier — air or carbon dioxide. For this purpose, blowers are used. Depending on the drying capacity of the evaporated moisture, the feed rate of the hot solution is set.

In the course of drying, the temperature of the finished powder is kept in the range of 20-40 ° C. In this case, the flow rate of the heat transfer medium is adjusted in accordance with the feed rate of the solution in order to maintain the drying intensity.

The inert nozzle is manufactured from fluoroplastic in the form of cylinders or balls. Air or carbon dioxide is used as a heat transfer medium from other industries at room temperature 18-20 C.

Example 1. 1 kg of phytosterol and arsenic are dissolved in 10-fold amount of 70% isopropyl alcohol with and stirred for 30 minutes. The resulting solution was clarified with 33% hydrogen peroxide, taken in an amount of 1/10 part of the solution with stirring for 0.5 h. The clarified solution from the reactor was fed into a dryer with a flowing nozzle at 50 s at a rate of 3 l / h is a fluoroplastic cylinders with a size of bhb mm. Towards the solution serves coolant - carbon dioxide at a speed of 30 m / s at. Drying time 1 h 20 min. At the outlet of the dryer, the finished phytosterol powder is obtained in white color with a temperature of 20 s and is poured into plastic bags. The yield of clarified phytosterol is 90% of the phytosterol and arsenic. The content of volatile substances in the clarified product is 0.8%. The content of solid soaps in the finished product is 25 „0%.

Example 2. 1 kg of a mixture of solid soaps and bottoms obtained during the purification of raw phytosterol, which are mixed in a ratio of .1: 1, is dissolved in a 10-fold amount of 70% isopropyl alcohol with stirring for 1 h. Then the solution clarified with 33% hydrogen peroxide, taken in an amount of 1/10 part of the solution. The clarified solution from the reactor is fed to a dryer with a fluoroplastic nozzle at a BOS at a rate of 2 l / h. The temperature of the coolant is air, the speed is 25 m / s. Drying time 1 h 30 min.

The finished powder at the outlet of the drying has a white color at a temperature. The yield of clarified phytosterol is 80%. The content of flying substances in the clarified product is 0.5%. The content of solid soaps in the finished product is 30.0%.

Claims (1)

1. USSR author's certificate number 361172, cl. C 07 C 167/00, published 1971. 2, USSR Author's Certificate 556149, cl. C 07 J9 / OO, publ. 1975 (prototype).