A method of processing a neutral substances

 

(57) Abstract:

The invention relates to methods for processing of neutral substances secreted from low-grade hardwood sulfate soap, and can be used in the pulp and paper and timber industry for cleaning of sulfate soap from cooking a mixture of different species of wood including birch. In the processing of low-quality sulfate soap the traditional way to improve the quality obtained from tall oil, pre-extracted neutral compounds containing biologically active compounds: betulin, sterols, polyprenols, squalene. Known methods of processing the extracted neutral substances highlight only one or two of the listed biological active compounds. The proposed method for the processing of neutral substances sulfate soap allows one process stream to obtain concentrates all of these biologically active compounds: betulin ("sitemeta"), sterols ("cristial"), polyprenols, squalene. The proposed method is based on the use of differences in physico-chemical constants and chemical properties of individual groups and individual H filtering and extraction using selective between immiscible solvents. table 2.

The invention relates to chemical and pulp and paper industry, namely the processing of neutral substances secreted from low-grade hardwood sulfate soap.

There is a method of processing a neutral substances with the separation of sterols through the formation of complexes with the chloride of the metal [1]

There is a method of processing a neutral substances, with the separation of sterols from one stripped off an ethyl acetate extract of neutral substances by addition of water [2]

There is a method of processing a neutral substances with the release of phytosterol extraction with a mixture of hexane, acetone, methanol and water [3]

There is a method of processing a neutral substances with the release of phytosterol, processing aromatic hydrocarbon, a polar solvent with the addition of water [4]

The method for extracting sterols from neutral substances from the mixture of solvents: hexane, xylene, ethyl acetate and water [5]

Known methods of processing of neutral substances emitting sitosterol and the form of the hydrate of a mixture of sterols by treatment with an organic solvent [6, 7]

There is a method of processing a neutral substances emitting sitosterol treatment m the low-quality hardwood sulfate soap, with the release of betulin [9] beaupreau (polyprenols) [10] "cytometry" [11]

However, all these methods are aimed at the separation of neutral substances with floor doctrine as the end product of one or two compounds. Other compounds included in the composition of the neutral substances are not used.

The closest in technical essence and the achieved result for the proposed method is a method of processing a neutral substances sulfate soap from cooking a mixture of different species of wood including birch, which consists in extracting neutral substances with ethyl acetate, evaporation of the extract neutral substances to the dry matter content of 10 to 33.3% cooling one stripped off of the extract to a temperature of 18 of the 22oC and crystallized from the cooled solution "cytometry" within 2 9 h [12]

The disadvantage of this method is its low efficiency, which is caused by the product of cytometry", containing two main biologically active compounds sitosterol and betulin.

The objective of the invention increase the efficiency of the method of processing of neutral substances produced from low-grade hardwood sulfate soap, by allocating additional the processing of low-sulfate soap from cooking a mixture of different species of wood, including birch, soap extracted with ethyl acetate in the presence of water, separating the extract from the raffinate is distilled off from the extract of the extractant and produce a neutral substance that is transferred to the hydrocarbon solvent extraction gasoline, petroleum ether, nefras and others), when the content of dry substances in a solution of 1,4 9,0% washed with water or 2 5%-s ' solution of the hydroxide or carbonate of an alkali metal at a ratio of water: the solution is neutral substances equal to 0.5 to 5.0:1.0 for exemption from traces of salts of organic acids and solids, defend 0.25 to 2 h at a temperature of -30 +20oC. the Precipitated crystals betulin or "cytometry" separated by filtration and dried. The product yield is 3 to 15% of the amount of neutral substances passing into a hydrocarbon solvent.

The solids content in the solvent should not be less than 1.4 percent as in this case sharply reduced yield of betulin. With the increasing content of dry substances in the solvent than 2% cannot obtain pure betulin, as it begins simultaneously with betulin crystallization of sterols, while receiving the drug cytolethal". When the content of dry substances in solution more than 9% difficult operation full the I water: the solution is neutral substances is not determinative for the separation, but keeping it in the range of 0.5 to 5.0:1.0 to allows you to achieve a complete mixing system and, consequently, better removal of impurities. Increasing the volume of water greater than 5.0: 1.0 is rational due to the increase in equipment and energy consumption for mixing. The introduction of small amounts of alkali or soda to pH 8 9 shifts the equilibrium for organic acids towards the formation of soluble salts in water and therefore increases the efficiency of their Department. Increasing the concentration of alkali (soda) is impractical because at pH 8 9 already almost complete transition of organic acids from the molecular ion in the form.

Crystallization of less than 0.25 h decreases the yield of betulin ("cytometry") that with increasing time of crystallization of more than 2 h does not increase.

Increasing the crystallization temperature above 20oWith leads to reduction of yield of betulin, lowering the crystallization temperature to -18oC and crystallization time over 0.5 h leads to an increase in deposition simultaneously with betulin sterols, and at temperatures below -18oC also begin to precipitate aliphatic alcohols. Further lowering of the temperature below -30oC economically netsales the dry substances 10 33,3% then cooled to a temperature below 0oC and kept at this temperature for 1 to 3 hours this stands a crystalline product, which could be called the drug "cristial". The output of this product is 5 to 10% of neutral substances.

"Cristial" the white crystalline product containing 30 to 40% of betulin, 30 to 40% of a sitosterol /carotovora/, 8 12% b-sitosterol and 10 to 20% of aliphatic alcohols from 24 to 28 carbon atoms. The melting interval "Kristiana" 170 220oC.

The solids content in the solution during the precipitation of "Kristiana" should not exceed 33.3% of as otherwise impeded the operation of the filter due to the high solution viscosity. When the solids content in the solution is below 10% reduced yield a crystalline precipitate.

Increasing the crystallization temperature above 0oC leads to a decrease in the content of higher aliphatic alcohols in "cristyle", which in turn leads to contamination of the concentrate polyprenols and squalene remaining neutral substances aliphatic alcohols, for the removal of which requires an additional operation of crystallization. Division of polyprenols and higher aliphatic alcohols is one of the most difficult tasks. When the crystallization temperature below -18o

The filtrate 11 after selecting "Kristiana" evaporated to trace amounts of solvent. Selected neutral substances extracted aprotic polar solvent.

The raffinate after separation of the residue of the extractant is a concentrate containing Sterol, triterpene and aliphatic alcohols with a residual content of hydrocarbons and polyprenols.

The selected extract is washed (extracted) hydrocarbon dissolution and after distillation of the solvents get two products. First - viscous dark-colored product, a mixture of polyfunctional oxidized compounds. The second concentrate polyprenols and squalene. Further, if necessary, polyprenols separated from squalene adsorption liquid chromatography and get concentrate polyprenols and concentrate squalene. The output of concentrate polyprenols 22 24% yield of concentrate squalene 3 6% from neutral substances. The data are given in table. 1 and 2.

Example 1. 170 g hardwood sulfate soap, with a humidity of 50% is dissolved in 170 ml of water, then add 110 ml of ethylacetate. The whole mixture is stirred until the formation homogenates neutral substances, fending off the ethyl acetate. Get was 12.75 g of neutral substances which dissolve in 637,5 g of gasoline, you get a solution neutral substances solids content in the solution is 2% of the resulting solution was washed with 350 ml of 2% aqueous solution OH defend at a temperature of 20oC for 2 hours fall At the same time the crystals betulin 0,38 g, which is separated from the solution by filtration. From the filtrate distilled 550 g of gasoline, get a solution of neutral substances with a solids content in the solution is 14% which is cooled to -3oC and kept at this temperature for 1 h From the solution falls crystals of sterols, which are separated from the solution by filtration. Obtain 1.3 g of sterols. Then from the filtrate evaporated gasoline, and the remaining neutral substances extracted aprotic polar dissolution, then washed extract (extracted) hydrocarbon solvent is distilled off the solvent and receive (3.77 g) concentrate of polyphenols and squalene. The concentrate of polyphenols and squalene share of liquid adsorption chromatography to concentrate pranolol (3.12 g) and concentrate squalene (0,65). In addition to these products as waste get the raffinate (7.0 g) and concentrate polyfunctional oxidized compound (1.3 g).about alcohol at a temperature of 60oC, then for 15 minutes the resulting solution was extracted with petrol (800 g) at a temperature of 40othen extract the neutral substances are separated from sulfate soap. The extract obtained (700 g) is a solution of neutral substances in gasoline (hydrocarbon solvent) content of dry substances in a solution of 1.4% Solution of neutral substances washed with water (700 g), then prepare the chin at a temperature of +4oC for 0.5 hours, fall at the same time the crystals betulin, which is separated by filtration from the solution of neutral substances. Get the concentrate betulin (0.45 g). The filtrate is evaporated to a solids content in the solution is 20% distilled 656,8 g gasoline), cooled to -5oC and kept at this temperature 0,25 hours From the solution drop crystals sterols, which are separated from the solution by filtration. Obtain 1.35 g of the concentrate of sterols. From the filtrate evaporated gasoline, and the remaining neutral substances extracted aprotic polar solvent, and then hydrocarbon solvent is distilled off the solvent and obtain a concentrate of polyprenols and squalene (2.3 g). Concentrate polyprenol and squalene share in a known manner to concentrate pranolol (2,03 g) and conc).

A method of processing a neutral substances containing betulin, sterols, polyprenols and squalene, by extraction with an organic solvent, namely, that of a neutral substance is transferred into the solution of the hydrocarbon solvent, which is washed with 2 5% aqueous-alkaline solution, followed by crystallization and filtration of the solution neutral substances emit concentrate betulin content of dry substances in a solution of 1,4 2,0% then concentrate Sterol content of dry substances in a solution of 3.0 33.3% and a crystallization temperature below 0oAnd from the filtrate after removal of the solvent allocate remaining neutral substance, which is extracted aprotic polar solvent, and then hydrocarbon solvent is distilled off the solvent and produce a concentrate of polyprenols and squalene, which is then separated in a known manner adsorption, liquid chromatography to concentrate polyprenols and concentrate squalene.

 

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