Method of preparing extractive substances from birch bark

FIELD: natural substances technology.

SUBSTANCE: method of preparing extractive substances from ground birch bark comprises extraction and filtration of precipitated extract. Extraction is effected with extractant condensate sprinkling ground birch bark bed in presence of ascending vapors of the same extractant. Extractant is two-component mixture of water and low-boiling solvent having boiling point below 100°C. Product is isolated by bringing extractant condensate containing dissolved extract with contents of receiver. Once extraction is completed, solvent is removed with live steam.

EFFECT: reduced consumption of extractant, increased degree of extractant regeneration, simplified isolation of product, and reduced fire and explosion risk.

1 tbl, 2 ex

 

The present invention relates to a method of allocating valuable extractive substances from plant materials, namely the method of production of extractives from the bark of the birch, used in medical, food and perfume industry.

A method of obtaining extractives from the bark of the birch on the example of betulin (RU # 2172178 C1, 2000.11.29). Shredded birch bark is separated into bark and phloem. To shredded bark add ethyl alcohol with a temperature of 70-75°and activated carbon. The solution is kept at this temperature for 3 hours, then filtered and from the filtrate the solvent is distilled off and get dry extract with access to 39% by weight of bark.

The disadvantage of this method is the high consumption of solvent (up to 500 kg of solvent per 100 kg of birch bark), the use of large amounts of activated carbon (up to 45 kg of coal per 100 kg of birch bark), technological difficulties associated with the separation of the dry product from the extract and disposal of spent activated charcoal and bark.

The known method of extraction of plant raw materials (P.I. resurrection, the Technique of laboratory work. Edition 10th, stereotypical, M., "Chemistry", 1973). The extractor is an open at both ends criticise tube, the lower part of which, at some distance from the narrow end finds the I glass or quartz spiral or porcelain grid. On top of the extractor is connected with a reflux condenser, and the bottom - flask. The substrate subject to extraction, is placed in the extractor to approximately half the height. Into the flask to 2/3 of its volume pre-pour extractant. The extractant is heated to boiling. Vapours pass through a layer of the substrate, are condensed in the refrigerator and drain back into the flask, passing once again through the layer of the substrate. As the extraction is almost at a temperature vapor extractant, it usually ends in a very short period of time.

The disadvantages of this method include the need to include additional stages to separate the extract from the extracting liquid, and in the case of applying the organic solvent is removed from the substrate and regeneration.

The closest in technical essence of the present invention is a method of separation of Betulinol (RU # 2206572 C1, 2002.03.12). The crushed bark of the birch is subjected to extraction in hexane to conventional Soxhlet extractions within 3-5 hours, then the extract is treated with an equal volume of water. Then the aqueous layer was separated, filtered precipitated from the hexane residue, and then remove the hexane fully. The mass of the dried sludge is 5-8% by weight of bark taken.

The disadvantage of the above method is the long extraction time, having a separate breadboard the stage of regeneration of hexane from birch bark.

Objectives of the invention are to reduce consumption of extractant, a more complete regeneration of the extractant, facilitating the selection of the target product from the extractant, the simplification of the process and apparatus of the scheme, the reduction of fire and explosion process.

The proposed method includes the following hardware. The extraction process is carried out in the extractor. The extractor is an extraction column, the top of which is attached a reflux, and the lower receiver with choke input acute water vapor. The receiver is heated by the heater. Technological scheme is that the shredded bark of the birch is loaded into the extraction column. The receiver is loaded extractant (extractant is a two - component mixture consisting of boiling solvent with a boiling point below 100°and water). The receiver is heated supplied it with water vapor, or heater. A pair of extractant pass through a layer of shredded bark birch and are condensed in the reflux. Condensate irrigates a layer of shredded bark birch, passes through the layer, enriched extractive substances and flows into the receiver. When the solvent evaporates and is returned to the extraction column, and dissolved the extract falls in the pond in the form of granules.

After extraction, the reflux condenser is replaced by a direct and distilled acute water vapor or temperature rise of the receiver boiling solvent from the receiver and the crushed bark of the birch in the extraction column. The precipitate was separated by filtration and dried. Regenerated boiling solvent used again.

The main distinctive feature of the claimed invention is that the extraction was carried out by the extractant, which is a two-component mixture consisting of water and boiling solvent.

Importantly, it is the presence of water, as one of the components of the extractant, promotes granulation of the resulting residue in the receiver, which eventually leads to the simplification of the subsequent stages of processing such as filtering and drying the final product. And found the range of ratios of water and boiling solvent in the receiver, for which there is a stable granulation.

Boiling solvent should meet the following criteria.

1) Can represent both the mixing and not mixing with the water liquid.

2) boiling point boiling solvent should be below 100°S. This condition is necessary for distillate boiling solvent from sodering the receiver and extractable substances acute water vapor. Use boiling solvent, which tend to form azeotrope with water.

3) Boiling solvent is chosen in such a way that the target of the extracted substance was dissolved in it.

Another distinctive feature of the proposed method is that the extraction process takes place in a thin layer under irrigation layer of birch bark condensate extractant, thereby minimizing the flow boiling of the solvent and reduce the cost of the final product. In addition, the concentration gradient of extractives in the system extractant - bark birch unlike protopapa always higher, resulting in the intensification of the extraction process.

Regeneration boiling solvent residues from birch bark in the extraction column by filing an acute water vapor in the receiver, resulting in the displacement of boiling solvent from the receiver and extraction columns with subsequent condensation. The advantage of this method lies primarily in the fact that all stages of extraction, including regeneration boiling solvent are carried out in one apparatus, which significantly simplifies the process and instrumentation diagram process. Moreover, the spent bark does not contain boiling solvent, which reduces fire and explosion the security process.

The combination of all the innovative characteristics of the invention allows to solve videostephanie tasks.

Table 1
EthanolIsopropanolHexaneThe ethyl acetate
The content of Betulinol extract, %65,836,6to 92.134,5

Example 1

In the extraction column load of 100 g of the crushed bark of the birch. In the receiver fill in the extractant (250 ml of hexane and 100 ml of water). The receiver is heated to boiling. The solvent evaporates, vapours pass through a layer of shredded bark birch and are condensed in the reflux. The resulting condensate irrigates the crushed bark of the birch, passes through the layer, on the way enriched by extractive substances, and flows into the receiver. While the solvent is again evaporated and returned to the extraction column, and dissolved the extract precipitates and granulated. Extraction lasts 2.5 hours, about the end of the extraction judged by the absence of significant quantities of the extract in the condensate at the outlet of the extraction columns. After extraction, the reflux condenser is replaced by a direct and deletion of acute water vapor or p is a rise in temperature of the receiver is distilled hexane from the receiver and birch bark. Get a mixture of hexane with water, then in a separating funnel to separate hexane from the aqueous layer. The amount of regenerated 240 ml hexane, and the total losses amount to no more than 4%. After distillation of the hexane whole extract is the receiver in the water in the granular sludge, which is then filtered and dried. The dry weight of the extract is 6 grams or 6% by weight of bark taken. Mass fraction of Betulinol in the resulting dry extract is 92-97%. Regenerated hexane re-use.

Example 2

In the extractor download 100 g of crushed bark of the birch. In the receiver pour 250 ml of 96% ethanol and 100 ml of water. Then the receiver is heated to boiling and serve acute water vapor. The solvent evaporates, vapours pass through a layer of shredded bark birch and are condensed in the reflux. The resulting condensate irrigates the crushed bark of the birch, passes through the layer, on the way enriched by extractive substances, and flows into the receiver. While the solvent is again evaporated and returned to the extraction column, and dissolved the extract precipitates and granulated. Extraction lasts 3 hours, about the end of the extraction judged by the absence of significant quantities of the extract in the condensate out of the extraction column. After extraction with a reflux Zam is both direct and deletion of acute water vapor distilled ethanol from the receiver and bark. The volume of the regenerated aqueous solution of ethanol is 394 ml with ethanol content of 66%. The total loss of the extractant in terms of pure ethanol is 5%. After distillation of the ethanol whole extract is the receiver in the water in the granular sludge, which is then filtered and dried. The dry weight of the extract is 24.5 g or 24.5% of the mass of bark.

The method of obtaining the extractive substances from the crushed bark of the birch, including extraction, filtration of precipitated extract, characterized in that the extraction is carried out by condensation of the extractant, irrigating a layer of shredded bark birch, in the presence of the ascending vapors of the same extractant, the extractant is a two-component mixture consisting of water and boiling solvent with a boiling point below 100°C, the product released during the interaction of the condensate extractant containing dissolved extract the contents of the receiver, after the extraction with boiling the solvent is removed acute water vapor.



 

Same patents:

FIELD: resin industry.

SUBSTANCE: method is designed for use in fabrication of plastics and composites with mineral and organic fillers. Method of invention comprises treating initial material with acetic anhydride in presence of catalyst at a ratio of 0.5-3.0 mole anhydride per 1 mole hydroxyl groups of material at intensive mechanical division of reaction mixture for 0.5 to 3 h at 25°C, said catalyst being ammonium sulfate used in amount 5-30% of the mass of lignohydrocarbon material.

EFFECT: reduced consumption of reagents by a factor 3 to 10, reduced duration of process to 1-3 h at temperature lowered to 25°C, and reduced process expenses.

4 tbl, 19 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention concerns preparation of sodium salts of sulfate esters of lingo-carbohydrate materials, which can be used as chemical additives to control properties of washing fluids used in boring oil and gas wells. Method of preparing water-soluble sulfuric acid esters of cellulose-based lingo-carbohydrate materials consists in that material is activated with sodium hydroxide and then affected by sodium fluorosulfonate. Activation of mechanically divided lingo-carbohydrate material composed of non-preliminarily separated cellulose, lignin, and hemicelluloses is conducted for 1 h at 70°C and reaction is carried out in isopropyl alcohol fir 3-15 h at 50-90°C and molar ratio of lingo-carbohydrate material to sodium fluorosulfonate equal to 1:(1-1.75).

EFFECT: enabled utilization of total amount of lingo-carbohydrate material, reduced price cost of final product, improved environmental condition, and widened spectrum of properties of final product.

4 tbl, 15 ex

FIELD: method for production of carboxymethyl esters useful as adsorbents.

SUBSTANCE: claimed method includes preliminary removing from air-dry lignocarbohydrate material of extractive and water soluble substances by 3-steps subsequent extraction with alcohol/benzene mixture, hot water and cold water. Then macromolecules are cross-linked by polycondensation of extracted material with formaldehyde in ratio lignocarbohydrate material OH-groups/formaldehyde of 1:3-5 in presence of alkali catalyst. Cross-linked lignocarbohydrate material is washed and carboxymethylated with monochloroacetic acid and alkali in ratio lignocarbohydrate material OH-groups/ClCH2COOH/NaOH of 1:3:27 at 45-65°C for at least 3 h. Obtained product is separated, treated with mineral acid to convert carboxylic groups to H-form; washed with water up to neutral filtrate pH-value, and dried.

EFFECT: product with high content of carboxylic groups, increased change capacity, and stability in aqueous and non-aqueous media.

6 ex, 2 tbl

FIELD: chemical wood reprocessing, in particularly for production of nitrogen-containing fertilizers and sorbents based on lignocarbohydrate raw material.

SUBSTANCE: claimed method includes treatment of lignin-containing raw material with ammonium solution of peroxide compound (e.g., hydrogen peroxide) containing 0.03-0.9 of hydrogen peroxide and 0.25-1.5 g of ammonium (in respect to 1 g of raw material), while thorough mechanical grinding at 20°C, frequency of 2800 cm-1,for 0.25-2.0 h. Method of present invention makes it possible to reduce oxidizing agent consumption by 4-5 times and ammonium amount by 1,5 times.

EFFECT: method with decreased reagent consumption and reduced process durability.

22 ex, 4 tbl

The invention relates to methods of extraction of valuable chemicals from waste processing and can be used in industry, for example in medical, cosmetic

The invention relates to chemical processing of lignocellulosic materials and can be used to obtain a nitrogen-containing organic fertilizers prolonged action on the basis of lignouglevodnyh plant materials
The invention relates to wood processing

The invention relates to a method of acid hydrolysis of lignocellulosic material such as wood, straw, vegetables, etc. to obtain sugars and lignin, as well as to the hydrolysis reactor for the implementation of this method

The invention relates to chemical processing of wood and can be used to produce nitrogen fertilizers and sorbents on the basis of different materials lignouglevodnyh
The invention relates to methods of extraction of valuable chemicals from waste wood, namely the method of obtaining betulin from birch bark

FIELD: fine organic synthesis, in particular production of triterpene compounds, betulin, useful in pharmaceutical and cosmetic industry.

SUBSTANCE: betulin is isolated from birch bark by extraction with neutral organic solvents, namely dioxan aqueous solution containing 0-20 mass % of water.

EFFECT: accelerated extraction process, increased yield of target product, decreased concentration of ester contaminants, and simplified betulin purification.

1 cl, 7 ex, 1 tbl

FIELD: organic chemistry of steroids, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing chemical compounds of steroid order, namely, to a method for preparing epibrassinolide representing (22R,23R,24R)-2α,3α,22,23-tetrahydroxy-B-homo-7-oxa-5α-ergostane-6-one and relating to biologically active substance - a phytostimulator regulating growth of plants. Method involves the successive carrying out the following stages: a) synthesis of ergosterol mesylate by treatment of ergosterol with methanesulfochloride in pyridine; b) synthesis of isoergosterol by boiling ergosterol mesylate in aqueous acetone in the presence of potassium (sodium) hydrocarbonate; c) synthesis of isoergosterone by oxidation of isoergosterol with chrome anhydride in pyridine; d) synthesis of 7,8-dihydroergosterol by reduction of isoergosterone with sodium dithionite in the presence of a solubilizing medium containing cationic, anionic or nonionic surface-active substances of the following order: CnH2n+1X wherein n = 9-18; X means -NMe3, -NEt3, -COOH, -SO3H, -OSO2M, -OP(O)(OM)2 wherein M means alkaline metal, polyethylene glycol, (C2-C6)-aliphatic alcohols or monoesters of ethylene glycol or diethylene glycol as a co-solubilizing agent, electrolyte and water taken in the molar ratio = 1:(5-6):(100-250), respectively; e) steroid rearrangement of 7,8-dihydroisoergosterol; f) formation of 24-epicastasterone by treatment of (22E,24R)-5α-ergosta-2,22-diene-6-one with methanesulfoneamide and potassium carbonate with using catalytic amounts of potassium ferricyanide (III) and osmium tetraoxide; g) dissolving 24-epicastasterone formed in chloroform followed by treatment with trifluoroperacetic acid forming in mixing trifluoroacetic anhydride and hydrogen peroxide in chlorinated organic solvent, and isolation of the end product of the formula (I) with high yield.

EFFECT: improved preparing method.

2 cl, 7 ex

FIELD: chemistry of natural compounds, chemical technology, pharmaceutical industry.

SUBSTANCE: invention relates to the improved method for preparing betulinic acid from betulonic acid. Method is carried out by reduction of betulonic acid with sodium boron hydride in water. Method provides simplifying the process, declining cost of the process for preparing betulinic acid and enhancing ecological safety of the process. Invention can be used in producing antitumor and anti-HIV medicinal preparations.

EFFECT: improved preparing method.

1 cl, 2 ex

FIELD: natural compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing biologically active substances from products of chemical processing vegetable biomass, in particular, to a method for preparing betulinic acid from betuline. Method is carried out by oxidation of betuline with chrome anhydride in acetic acid to betulonic acid, and reduction of betulonic acid with sodium boron hydride is carried out in diethyl ether solution being without its preliminary isolation. Invention provides enhanced yield, simplifying technology, decrease of the process time and decreasing set of solvents used.

EFFECT: improved preparing method.

1 cl, 1 ex

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

FIELD: chemical technology.

SUBSTANCE: invention relates to methods for preparing oleanolic acid used as a standard sample (comparison samples) in carrying out standardization of medicinal vegetable raw and phytopreparations comprising triterpene saponins - derivatives of oleanolic acid. For preparing oleanolic acid method involves sum of saponins extracted by alkaline extraction from sugar or table beet root crops followed by reprecipitation in acid medium and extraction of precipitate with ethanol, chloroform. Method provides preparing oleanolic acid of high purity degree from inexpensive and available raw.

EFFECT: improved preparing method.

2 cl, 3 ex

FIELD: chemical technology, natural materials, medicine, pharmacy.

SUBSTANCE: invention relates to the improved method for preparing betulin from betulinic acid that can be used in preparing anti-tumor and anti-HIV medicinal preparations. Method for preparing betulinic acid involves oxidation of betulin with chrome (VI) oxide in acetic acid to betulonic acid and reduction with sodium boron hydride to betulinic acid. Betulonic acid sodium salt is reduced to betulinic acid and reduction reaction is carried out at room temperature at the concentration of sodium boron hydride 1.0-6.0 wt.-%. Invention provides simplifying method for preparing betulinic acid, reducing its cost and enhancing ecological safety of the process of it producing.

EFFECT: improved preparing method.

1 cl, 4 ex

The invention relates to new biologically active compounds, namely diglyceride glycyrrhizic acid methyl ester L-valine of formula (I), stimulating primary immune response

The invention relates to new chemical substance, specifically to biologically active compounds having immunostimulatory and antiviral activity (anti-HIV and anti-herpes), - N'-{N-[3-oxo-20(29)-lupen-28-oil] -9-aminopentanoic} -3-amino-3-phenylpropionic acid of the formula I

FIELD: fine organic synthesis, in particular production of triterpene compounds, betulin, useful in pharmaceutical and cosmetic industry.

SUBSTANCE: betulin is isolated from birch bark by extraction with neutral organic solvents, namely dioxan aqueous solution containing 0-20 mass % of water.

EFFECT: accelerated extraction process, increased yield of target product, decreased concentration of ester contaminants, and simplified betulin purification.

1 cl, 7 ex, 1 tbl

Up!