Method of larch complex treatment

FIELD: agriculture.

SUBSTANCE: it is provided method of larch complex treatment, including treatment of disrupt larch in medium on the basis of deionised water and organic solvent, in rotor-type pulsating facility - cavitator at temperature of self-heating, with following separation of received pulp on liquid and solid phases, separate treatment of liquid and solid phases, release from solid phase of natural resins, by means of extraction by organic solvent, with following drying and modification of activated wood, release from liquid phase of dihydro-meletin by means of re-extraction by methylthreat butyl ether, with following vacuum evaporation of re-extract and drying of received product, herewith in the capacity of organic solvent there are used nonmiscible with water solvents, selected from the group: tetrachloromethane, chloroform, dichloroethane, or its mixtures at mass correlation deionised water: organic solvent from 9:1 to 8:2, and mass correlation of wood : water-organic medium are 1:8-1:10.

EFFECT: release from larch of dihydro-meletin with grade 93-97%, with yield 2,5-2,6% of mass of bone-dry wood and resinous mass with yield 4,5-5,0%.

4 ex, 1 tbl

 

The invention relates to the field of processing ligninsulfonate raw materials, namely larch wood, particularly wood waste processing - butt part of the Siberian and Dahurian larch obtaining biologically active flavonoid - dihydroquercetin (DHQ), which are used in medicine and food industry, as well as with the extraction of natural resinous materials for the production of rosin, surfactants, odorous substances, virucidal, as well as receiving technical products from wood.

Known methods of allocation of DHA from larch wood (RF patents №2114631 and No. 2180566).

However, these methods are characterized by low use of wood.

A known method of processing of larch wood, including extraction of destructional wood natural substances by treatment with an organic solvent containing water, separation of the extraction of the mass of the extract and the solid phase in the form of a carbon-containing polymer of wood, which is marked as the target product and/or subjected to carbonization in an inert gas atmosphere to obtain from the resulting organic and aqueous phases of the respective target products (patent RF №2165416, 2001).

The disadvantage of this method is the use of a large number of organic solvents, such as hexa is, or gasoline, acetone, ethyl alcohol, which is either expensive or toxic. Also, this way of ethnological, because it is necessary to conduct separate operations at high pressure. In the process of wood pulp remaining after extraction, receive only one product is activated carbon.

The known method for integrated processing of larch wood, including processing destructional larch wood in a fluidized state with deionized water at a mass ratio of wood:neionizirovanny water from 1:4 to 1:10, separating the resulting slurry into liquid and solid phases, separate treatment of liquid and solid phase organic solvent and the allocation of dihydroquercetin and natural resins, and processing destructional larch wood in a fluidized bed state is carried out in the cavitator at a temperature of 70-92°C for 5-15 minutes the Liquid phase is treated with an organic solvent, the solid phase obtained after separation of the pulp, before treatment with an organic solvent is subjected to drying to a moisture content of 9-11 wt.%, as the organic solvent used methyl tertiary butyl ether, solid phase methyl tertiary butyl ether is carried out at 50-55°C with the release of the resulting solution natural resins, and the rest of aktivirovannoi wood pulp is subjected to interaction with fosforiliruyusciye, similitude or chloranilide agent at 60-70°C (RF patent No. 2233858, 2004). This method is chosen as a prototype.

However, the known method has several disadvantages, namely cavityretina wood retains its mass is a large amount of resin, and the isolation and purification of DHA is difficult because of the presence of stable emulsions.

The present invention is the creation of a new, more technologically advanced method for integrated processing of larch, which increases the output of DHA due to prevent the formation of stable emulsions, and also reduces the amount of tar in kawailani wood.

This object is achieved in that the integrated processing of larch wood includes processing destructional larch wood in the environment on the basis of deionized water in a rotary pulsation device cavitator with temperature self-heating, with subsequent separation of the resulting slurry into liquid and solid phases, separate treatment of liquid and solid phase, separation of the solid phase natural resin by extraction with organic solvents, followed by drying and modification of activated wood, separation from the liquid phase of dihydroquercetin reextracting methyl tertiary butyl ether, followed by vacuum evaporation of reextract the drying of the resulting product, moreover, the processing destructional larch wood is carried out in the environment on the basis of deionized water and an organic solvent, where the organic solvent used water-immiscible solvents selected from the group of carbon tetrachloride, chloroform, dichloroethane, or a mixture thereof at a mass ratio of deionized water:organic solvent of 9:1 to 8:2, and the mass ratio of wood:an aqueous-organic medium is 1:8-1:10.

The essential difference between the proposed method for integrated processing of larch wood from well-known is that the decomposition of wood is carried out in an aqueous-organic medium consisting of deionized water and immiscible with it solvent selected from the group of carbon tetrachloride, chloroform, dichloroethane or mixtures thereof at a mass ratio of deionized water:organic solvent of 9:1 to 8:2, and the mass ratio of wood:an aqueous-organic medium is 1:8-1:10, what is new and meets the condition of inventive step.

The method is as follows. The wood of larch, such as waste wood processing industry (sawdust, shavings, chips), loaded into a container, then add the calculated amount of the mixture of deionized water and organic p is storytale, taken in a ratio of from 9:1 to 8:2, to mass ratio of the solid and liquid phases of 1:8-1:10.

The mixture from the tank into the reactor, which represents a rotary pulsation device, such as a cavitator, the temperature of the suspension in the cavitator due to self-heating is raised to 60-65°C. In the cavitator when the pressure differential extraction process is accompanied by the simultaneous destruction of biological structures of wood, with aqueous-organic medium with the dissolved substances becomes disintegrated fluidized condition characterized by a decrease in viscosity and increase in yield stress, all contribute to the most complete extraction of natural wood resins and dihydroquercetin (DHQ), and optimal activation of wood needed in preparation for further processing wood pulp. The hot extract was filtered from the cell residues, liquid phase spontaneously splits, and it is divided into aqueous and organic components. Organic part evaporated in vacuum and get the tree resin. Eviteranno wood pulp is washed with an organic solvent and dried. The water part extravert methyl tertiary butyl ether. After separation of the ether extract from the water, it is also evaporated in vacuum and get the target di is irakurtzean.

The proposed method is illustrated by the following examples and Table 1.

Example 1. 1000 g of sawdust butt part larch (relative humidity 10%) load in cavitator, pour a heterogeneous mixture of solvents consisting of 9 liters of deionized water and 1 liter of dichloromethane and subjected to kawailani for 2 minutes. The temperature of the suspension due to cavitation is increased to 60-65°C. the Hot extract is filtered (centrifuged) from the cell residues, liquid phase spontaneously splits, and it is divided into aqueous and organic components. Organic part evaporated in vacuum and get 50 grams of wood resin. Eviteranno wood pulp is washed with dichloroethane and dried, get 700 g (77%). The water part extravert 1.5 liters of methyl tertiary butyl ether. After separation of the ether extract from the water (with separator), it is also evaporated in vacuum and get 22.5, dihydroquercetin 93%purity (2.5% in terms of absolutely dry wood).

Received DHA has the following physicochemical characteristics: TPL238°C, [α]D20=+36°(CL, methanol). Individuality proven NMR spectra of1H and13C.

Example 2. The process is carried out analogously to example 1 at a ratio of water to ethylene dichloride 8:2 for 3 minutes. The temperature of the pulp povyshaetsya 65°C. The hot slurry is centrifuged, separating the cellular remnants from the liquid phase. After that, the liquid phase spontaneously splits into water and the organic part. Organic part evaporated in vacuum and obtain 48 g of wood resin. Eviteranno wood pulp is washed with dichloroethane and dried receive 710 g (78.1%). The water part extravert 1.5 l of methyl tertiary butyl ether. The ether extract is evaporated in vacuum and obtain 22.7 g of DHA, which is recrystallized from hot water and obtain 21.3 g of DHA 97% purity (yield 2.4% in terms of absolutely dry wood).

Example 3. The process is conducted as in example 2 at a ratio of water to carbon tetrachloride 8:2 for 3 minutes. The temperature of the pulp is increased to 65°C. the Hot slurry is centrifuged, separating the cellular remnants from the liquid phase. After that, the liquid phase spontaneously splits into water and the organic part. Organic part evaporated in vacuum and obtain 51 g of wood resin. Eviteranno wood pulp is washed with carbon tetrachloride and dried, get 700 g (77%). The water part extravert 1.5 l of methyl tertiary butyl ether. The ether extract is evaporated in vacuum and obtain 22.8 g of DHA, which is recrystallized from hot water and obtain 21.5 g of DHA 97% purity (yield 2.4% in terms of absolutely dry wood).

Example 4. The process is conducted analogion the example 3 when the ratio of water to the chloroform 8:2 for 3 minutes. The temperature of the pulp is increased to 60°C. the Hot slurry is centrifuged, separating the cellular remnants from the liquid phase. After that, the liquid phase spontaneously splits into water and the organic part. Organic part evaporated in vacuum and obtain 49 g of wood resin. Eviteranno wood pulp is washed with chloroform and dried receive 705 g (78%). The water part extravert 1.5 l of methyl tertiary butyl ether. The ether extract is evaporated in vacuum and obtain 22.8 g of DHA, which is recrystallized from hot water and obtain 21.1 g of DHA 97% purity (yield 2.4% in terms of absolutely dry wood).

The proposed method allows you to select from larch wood valuable substances, such as dihydroquercetin, large compared to the prototype output 2.5-2.6% of the mass of absolutely dry wood with purity of 93-97%and resinous mass with the release of 4.5-5%.

In addition, the inventive method for integrated processing of larch wood is more sophisticated, because the selection of target products easier, more cost-effective, because the temperature treatment of wood in the water-organicheskoi environment cavitator occurs when the self-heating at a temperature of 55-65°C.

Method for integrated processing of larch wood, including processing destructional trees is the Sina larch in the environment on the basis of deionized water in a rotary pulsation device the cavitator at a temperature of self-heating, with subsequent separation of the resulting slurry into liquid and solid phases, separate treatment of liquid and solid phase, separation of the solid phase natural resin by extraction with organic solvents, followed by drying and modification of activated wood, separation from the liquid phase of dihydroquercetin reextracting methyl tertiary butyl ether, followed by vacuum evaporation of reextract and drying the resulting product, wherein the processing destructional larch wood is carried out in the environment on the basis of deionized water and an organic solvent as the organic solvent used is not miscible with water, the solvents selected from the group of: carbon tetrachloride, chloroform, dichloroethane or their mixture at a mass ratio of deionized water : organic solvent of 9:1 to 8:2, and the mass ratio of wood : an aqueous-organic medium is 1:8-1:10.



 

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Modified gum arabic // 2347788

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SUBSTANCE: invention concerns organic chemistry, particularly method of dihydroquercetin extraction from larch wood, and can be applied in chemical and pharmaceutical industry, medicine, food industry. Invention claims method of dihydroquercetin extraction from milled larch wood by extraction with organic solvent. Wood is milled into chips, extraction is performed gradually in several stages in at least two extractors, maintaining continuous circulation of one minimal extraction solvent volume required for chip submersion in liquid medium at each stage, simultaneously generating low-frequency oscillating field at temperature close to boiling point of solvent, with further hot extract transport after completion of process at one stage in one extractor volume to the next extraction stage, each time adding new extraction solvent in amount equal to solvent outflow with extracted chips. Then each extracted chip portion is flushed with one minimal solvent volume required, extracts from the last n extraction and flushing stages are combined into one volume, solvent is separated from it, remains are concentrated, and dihydroquercetin is extracted. Invention also claims aggregate for dihydroquercetin extraction from larch wood, including feeding tank, heater, extraction solvent collector and at least one extraction solvent processing lines with further dihydroquercetin extraction from it, each line including inlet and outlet valves, extraction reactor and pulp pump and carrying solvent vapour condenser, heater for solvent heating and low-frequency oscillator in the form of diaphragm pump mounted on pipeline. Each extractor is active periodically and is connected to feeder tank outlet by one of inlets, to extract feed unit by the other inlet over first inlet valve, to condenser inlet by one of outlets. Condenser outlet is connected over second inlet valves to another inlet of each extractor, the other extractor outlet connected to third inlet of each extractor over a sequence of heater, pump, oscillator and third inlet valve. Third extractor inlets are connected to extraction solvent collector over third pump and fourth valve.

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5 cl, 2 dwg, 3 tbl, 2 ex

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