RU2462448C2 - Method of processing of wood green of siberian fir - Google Patents

Abstract

FIELD: agriculture.

SUBSTANCE: method of processing of wood green of Siberian fir, which includes obtaining of ethyl acetate extract by dissolving the alcoholic extract of wood green of fir tree in ethyl acetate, followed by rinsing the solution with water with the separation of pine wax, treatment of purified ethyl acetate extract with aqueous alkaline agent solution with the separation the solution by retention for the organic layer, of which, after distillation the solvent, the extraction fir balsam is obtained, and the aqueous alkaline layer which is chilled down with obtaining at the same time of the deposit - the biologically active amount of triterpene acids salts, and of the water part - the maltol.

EFFECT: invention enables to increase the yield and to improve the consumer properties of the target product - the amount of biologically active triterpene acids salts, to expand the range of products obtained by processing fir raw, to increase environmental friendliness of the method.

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Description

The invention relates to methods for processing natural raw materials, in particular woody Siberian fir, to obtain the main product - the biologically active amount of salts of triterpenic acids - the basis of plant growth regulators widely used in crop production (SILK, Biosil, Novosil, etc.), as well as coniferous wax, extraction balm, maltol, used in various sectors of the economy.

A known method of obtaining a biologically active amount of triterpenic acids from chopped wood fir green by extraction with an organic extractant, which is used as an aliphatic alcohol selected from the group of alcohols with the number of carbon atoms 1, 2, 3 or acetone containing not more than 50 wt.% Water, s subsequent isolation of the target product by distillation of the alcohol / water or acetone / water mixture, and separation of water, followed by the use of the distilled mixture as an extractant (RU 2179393 C1, A01N 65/00, A61K 35/78, 02.20.2002).

When implementing this method, a biologically active amount of triterpenic acids is obtained in a mixture with other substances contained in green wood, i.e. the entire amount of water and alcohol soluble substances. Some of them, in particular coniferous wax, reduce the effect of the target product on the treated plants, others, for example, maltol, are ballast.

A known method of producing maltol from plant raw materials of fir, including treating it with carbon dioxide at a temperature of 20-60 ° C and a pressure of 40-60 atm for 2-6 hours, followed by treatment with hot water at a temperature of 90-95 ° C for two days , the concentration of the aqueous extract, treatment with diethyl ether and extraction with chloroform (RU 2171805 C1, C07D 309/40, 08/10/2001).

This method is associated with the use of toxic solvents (ether, chloroform), uneconomical due to the inefficient use of needles to produce one product.

There is also known a method of obtaining a biologically active amount of triterpenic acids from dried chopped wood green fir, which is sequentially extracted with gasoline or petroleum ether and ethyl acetate, or a mixture thereof, the extract is treated with an aqueous solution of an alkaline agent, acidified with an aqueous alkaline solution to pH 2, the target product is isolated by extraction ethyl acetate (SU 1809975 A3, C07C 57/26).

As a result of the implementation of this method, only one product is obtained - the biologically active amount of triterpenic acids, while the target product has the necessary purity, but its yield is not high enough. In addition, the sum of triterpene acids is insoluble in water, and its use is possible only in the form of an aqueous emulsion prepared according to a specially developed method, which complicates the technology and increases the complexity of the method. The disadvantages of the method should also include environmental pollution with effluents containing toxic substances.

The objective of the present invention is to increase the yield and improve the consumer properties of the target product is a biologically active amount of salts of triterpene acids, expanding the range of products obtained from the processing of fir raw materials, increasing the environmental friendliness of the method.

The problem is solved in that a method of processing woody Siberian fir greenery involves producing an ethyl acetate extract by dissolving the alcoholic extract of fir needles in ethyl acetate, then washing the solution with water to separate the coniferous wax, treating the purified ethyl acetate extract with an aqueous solution of an alkaline agent, separating the solution by settling into the organic layer, from which, after distillation of the solvent, an extraction fir balsam is obtained, and a water-alkaline layer, which is cooled with radiation from the sediment - the biologically active amount of salts of triterpenic acids, and from the water part - maltol.

The method is as follows.

Fir needles are poured with alcohol, infused, poured miscella (infusion), needles are again poured with alcohol, insisted and poured infusion. Both solutions are mixed and the solvent is distilled off by heating under vacuum. The resulting alcoholic extract was dissolved in ethyl acetate, stirred, water was added, stirred and asserted. In the process of settling in water in the form of a suspension, coniferous wax is released, which is drained with water. The extract purified from wax is treated with 2% NaOH solution and sedimented. After delamination and separation of the solution from the upper organic layer, the solvent is removed to obtain an extraction fir balsam; the lower, water-alkaline layer is drained, clean it of residual solvent by distillation, and chill. In this case, the solution is divided into two layers, the resulting precipitate is obtained — the salts of triterpenic acids, after dilution, are used as the active substance of the plant growth regulator, and maltol crystals are isolated from the aqueous part after evaporation under vacuum.

Example. For the extraction of woody green Siberian fir, an extractor is used with a working space volume of 0.5 m ³ , into which 132-136 kg of raw material is loaded. The extractor is filled with isopropyl alcohol to completely cover the woody greens - 380 l. After 4-hour infusion, 260 liters of alcohol are poured from the extractor with extractives dissolved in it, and the raw material is poured with a fresh batch of alcohol in a volume of 260 liters, it is infused for 4 hours and the second batch is drained. The resulting two batches are mixed, the alcohol is distilled off by heating to 80 ° C under vacuum. The alcohol extract obtained in an amount of 23 kg was dissolved in 69 liters of ethyl acetate, stirred, 1 part of water was added, mixed and defended. Water with precipitated flakes of coniferous wax is drained, the wax is filtered off and dried to obtain 2.3 kg of wax. 90 l are poured into a purified ethyl acetate solution (90 L). 2% NaOH solution and mix thoroughly. The mixture is defended in a separatory funnel-settler until its separation within 1.5-2 hours. The lower water-alkaline layer is purified from residual ethyl acetate by distillation, the remaining mixture is chilled to a temperature of 2-4 ° C, as a result of which the mixture is divided into two layers - the precipitate and the aqueous part. The water part is drained and crystals of maltol are planted from it, which are sent, for example, to the food industry. The precipitate containing salts of triterpenic acids, in the dried state having the form of a powder, is diluted with water to the desired concentration and is used as a plant growth regulator SILK. The yield of salts of triterpenic acids is 11-12% by weight of dry raw materials, the yield of maltol is 1-2%. Ethyl acetate is distilled off from the organic part resulting from the separation of the alkaline agent-treated ethyl acetate extract and an extract fir balsam is used, which is used to prepare the Fosprenil preparation used in veterinary medicine.

When implementing this method of processing woody greens of Siberian fir, in addition to the target product, the biologically active amount of salts of triterpene acids with a yield more than 2 times the product yield of the prototype, a number of products are also obtained, such as maltol, pine wax, extraction fir balm - widely used in various fields of activity.

Claims (1)

A method of processing Siberian fir wood greens, including obtaining an ethyl acetate extract by dissolving an alcohol extract of fir green greens in ethyl acetate, then washing the solution with water to separate coniferous wax, treating the purified ethyl acetate extract with an aqueous solution of an alkaline agent, separating the solution by settling into an organic layer, from which after distillation solvent get extraction fir balsam, and a water-alkaline layer, which is cooled with getting from the wasp dca - the biologically active amount of salts of triterpenic acids, and from the water part - maltol.