Method of production of betulin

FIELD: medicine; pharmaceutical industry; perfumery-cosmetic industry; methods production of betulin.

SUBSTANCE: the invention is pertaining to the method of extraction of betulin from the wastes products of wood-processing, in particular, a birch bark processing and may be used in medicine, pharmaceutical and perfumery-cosmetic industries. The method provides for activation of a birch bark by the shock-acoustic impulses, an alkaline hydrolysis and an extraction of betulin by an alcohol. The operations are conducted simultaneously. The technical result of the invention is simplification of the method of the process, reduction of its duration and power input.

EFFECT: the invention ensures simplification of the method of the process, reduction of its duration and power input.

1 cl, 2 ex

 

The invention relates to extraction of valuable chemicals from waste timber, namely the allocation method betulin formula (1) of the outer layer of birch bark (bark).

Betulin is a white crystalline powder with Tpl.261-262°used in medicine, pharmaceutical and cosmetic industries.

It is known that the low solubility of betulin in water and available in many organic solvents makes its selection by extraction and complicates the technology of the processes of obtaining betulin from birch bark (Chemistry of wood, 1984, No. 3, p.3-28).

A method of obtaining betulin, namely, that the bark is first subjected to activation conditions pisabarro of paratrechina at a temperature of 180-260°C, a pressure of 2-5 MPa for 1-6 minutes, then alkaline hydrolysis in aqueous-alcohol-alkaline medium followed by extraction of betulin alcohols. The output of betulin is 25-37% of the weight of the absolutely dry bark (EN 2074867, 10.03.97).

The disadvantage of this method is its technological complexity, since the method involves 3 stages: activation conditions pisabarro of paratrechina at high temperature and high pressure alkaline hydrolysis in aqueous-alcohol-alkaline medium and extraction of betulin Speer is om.

The closest technological essence and the achieved result is a method of obtaining betulin, including activation of birch bark in conditions pisabarro of paratrechina at a temperature of 180-260°C, a pressure of 2-5 MPa, the duration of the activation 1-5 min in the presence of alkali (alkaline hydrolysis), taken in an amount of 5-20% by weight of the absolutely dry bark with subsequent extraction of betulin alcohol (EN 2131882, 20.06.99). In this way the combined stage activation bark and alkaline hydrolysis, but the extraction of betulin alcohol is a separate stage.

The disadvantage of this method is a complex process activation bark neishaburi paratrechina requiring the use of high pressure and high temperature to obtain a superheated water vapor, which complicates the technology and increases the energy intensity of the process of obtaining betulin. The disadvantage of this method is the necessity of using a separate phase extraction of betulin.

Object of the invention is the simplification of the process by combining the stages of activation, alkaline hydrolysis and extraction, as well as reducing the duration of the process and its intensity.

This object is achieved in that the crushed bark is treated with a mixture of water-alcohol-alkali when using the shock-acoustic impacts is generally within 5 minutes at a temperature of 70° C. Shock-acoustic activation intensifies the hydrolysis of birch bark, which in a few minutes turns into a homogeneous mass of brown, accelerates the transition of betulin in the solution and increases its output. Next betulin precipitated from one stripped off solution when diluted with water and separated by filtration.

The essential distinctive features of the prototype feature is the activation of birch bark and its alkaline hydrolysis simultaneously with the extraction of betulin, that is, in the proposed method there is no separate stage of betulin extraction with alcohol.

As a result, significantly simplifies the process of obtaining betulin, because the reduced number of process steps, reduced the duration and intensity: the activation process is carried out at a lower temperature and pressure and does not require the use of superheated steam.

Shock-acoustic setup used in this way as described in patent RU 2176158, 25.06.99.

The method is confirmed by specific examples.

Example 1. Shredded bark in the amount of 3.7 g, with humidity 2,41%, particle size of from 2 to 5 mm with the content of betulin 35% load reactor percussion-acoustic installation of 250 cm3add heated to 70°With a solution consisting of 30 ml of water, 4 g of sodium hydroxide and 150 ml Adilov the alcohol and subjected to shock-acoustic effect within 5 minutes

The reaction mixture discharged from the reactor, separating the solid residue by filtration on a Buchner funnel, the filtrate is completely evaporated alcohol, then diluted with 50-60 ml of distilled water. Fallen betulin is filtered off, washed on the filter with hot water until neutral and dried in air at room temperature. The output of betulin is 43% by weight of the absolutely dry bark.

Example 2. Perform analogously to example 1, but without the use of shock-acoustic activation. Obtaining betulin with the release of 41% is achieved by boiling the bark in water-alcohol-alkaline solution within 300 minutes.

Thus, the inventive method of obtaining betulin from the outer layer of birch bark (bark) allows to simplify the process: to reduce the number of stages and the duration of the process, and to reduce the energy intensity of the process.

The method of obtaining betulin from birch bark, including activation of birch bark in the presence of alkali and extraction of betulin alcohol, characterized in that the bark activated shock-acoustic pulses simultaneously with alkaline hydrolysis and extraction with alcohol.



 

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