Method of producing vanillin by oxidizing lignin-containing wood raw materials

FIELD: chemistry.

SUBSTANCE: method consists in oxidizing lignin-containing wood raw materials with oxygen in an alkaline medium at elevated temperature and pressure in the presence of an organic additive. Herewith sodium salt of copper tetrasulfophthalocyanine is used as an additive in the amount of 0.1-0.4 g/l of the reaction mass.

EFFECT: increasing the yield of the target product, shortening the duration of the process.

4 ex

 



 

Same patents:

FIELD: chemistry.

SUBSTANCE: method consists in air oxygen oxidation of lignin, obtained by fermentative hydrolysis of wood of coniferous species or wood, affected by brown or mottled rot, with content of lignin 40-90 wt % in water-alkali medium at higher temperatures and pressure. The process is carried out in presence of catalysts on the basis of copper hydroxide with continuous supply of alkali solution into reactor for 1-150 minutes.

EFFECT: method makes it possible to reduce alkali consumption counted per a kilo of obtained vanillin, and consumption of fermentative lignin, which reduces amount of organic substance, formed as byproducts, in sewage water and improves ecological compatibility of the process.

10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of purifying vanillin obtained from lignin oxidation products, by reacting vinillin-containing extracts with aqueous solutions sodium bisulphite, followed by decomposition of the vanillin-bisulphite derivative. The method is characterised by that the vanillin-bisulphite derivative is heated in an autoclave to 120-170C, the vapour-gas phase is released and vanillin is extracted from the obtained mixture or solution, followed by recycling the obtained aqueous solution of sulphurous anhydride and sodium sulphate into a solution of sodium bisulphite.

EFFECT: method enables to avoid the use of sulphuric acid and alkali when purifying vanillin, widely used in food, perfume, cosmetic and pharmaceutical industry.

5 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of separating vanillin, which is widely used in food, perfume-cosmetic and pharmaceutical industries, from lignin oxidation products by reacting vanillin-containing extracts with aqueous sodium hydrosulphite NaHSO3 solutions. The solutions used have sodium hydrosulphite concentration of 320-400 g/l and the vanillin-hydrosulphite derivative formed is separated from excess sodium hydrosulphite solution in form of a precipitate by filtration, centrifuging or decantation.

EFFECT: method enables to cut consumption of sodium hydrosulphite and increases the distribution ratio of vanillin into the precipitate and aqueous phase from the organic phase, which reduces the volume of extracts and re-extracts when separating vanillin.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of extracting ortho-vanilin and iso-vanilin from aqueous solutions. The method involves addition of a salting-out agent - sodium chloride to aqueous solutions of ortho-vanilin and iso-vanilin and a solution of polyvinyl caprolactam prepared beforehand, having concentration of 5-15 wt % until achieving 34-35 wt % content of salt in the solution, with volume ratio of the aqueous phase to organic phase equal to 10:1. The organic phase is extracted and separated, analysed spectrophotometrically and the recovery ratio (R, %) of ortho-vanilin and iso-vanilin is calculated using the formula: R=D100/(D+r), where D is coefficient of distribution of ortho-vanilin and iso-vanilin between the solution of polyvinyl caprolactam and the aqueous solution, r is the ratio of equilibrium volumes of the aqueous and organic phases.

EFFECT: method increases recovery ratio of ortho-vanilin and iso-vanilin from aqueous solutions.

1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: method of extracting vanillin, ethylvanillin, iso-vanillin and ortho-vanillin from water solutions is characterised by the following: preliminarily to water solutions of vanillin, ethylvanillin, iso-vanillin and ortho-vanillin added are; ammonium sulphate, until its content in solution is 42-43% to solution weight, and preliminary prepared mixture of solvents, consisting of 22-23 wt % acetone and 78-77 wt % diacetone alcohol, then extraction is carried out with molar ratio of water and organic phases 10:1, and degree of vanillins extraction (R,%) is calculated by formula: R=D-100/(D+r), where D is coefficient of vanillins distribution between solvent mixture and water-salt solution, r is ratio of equiweight volumes of water and organic phases.

EFFECT: increase of degree of vanillin, ethylvanillin, iso-vanillin and ortho-vanillin extraction from water solutions.

1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: vanillin is applied in confectionery, pharmaceutics and manufacturing of perfume and cosmetics, and lilac aldehyde is applied in manufacturing of trimetoprim, biseptol and other pharmaceutical drugs. Method involves extraction by oxygen-containing extraction agents at pH 6.0-8.0 and re-extraction by water alkaline solution at pH 10-14. Extraction stage involves use of tributhylphosphate, or kerosene solutions of tributylphosphate with 40-99 wt % of tributylphosphate, as extraction agents.

EFFECT: reduced volume of extraction agent required at extraction stage in comparison to existing technique.

7 ex

The invention relates to a method for products of fine organic synthesis of vanilla, lilac aldehyde, levulinate acid

The invention relates to a new method of obtaining 4-hydroxybenzaldehyde and its derivatives, in particular for the preparation of 3-methoxy-4-hydroxybenzaldehyde (vanilla) and 3-ethoxy-4-hydroxybenzaldehyde (ethylvanillin)

The invention relates to the chemical processing of wood components, specifically to an improved process for the preparation of vanillin and lilac aldehyde, which find wide application in the production of a large number of medicines, in the synthesis of polymers

The invention relates to a method for producing vanillin and lilac aldehyde products of fine organic synthesis

FIELD: chemistry.

SUBSTANCE: method consists in air oxygen oxidation of lignin, obtained by fermentative hydrolysis of wood of coniferous species or wood, affected by brown or mottled rot, with content of lignin 40-90 wt % in water-alkali medium at higher temperatures and pressure. The process is carried out in presence of catalysts on the basis of copper hydroxide with continuous supply of alkali solution into reactor for 1-150 minutes.

EFFECT: method makes it possible to reduce alkali consumption counted per a kilo of obtained vanillin, and consumption of fermentative lignin, which reduces amount of organic substance, formed as byproducts, in sewage water and improves ecological compatibility of the process.

10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of purifying vanillin obtained from lignin oxidation products, by reacting vinillin-containing extracts with aqueous solutions sodium bisulphite, followed by decomposition of the vanillin-bisulphite derivative. The method is characterised by that the vanillin-bisulphite derivative is heated in an autoclave to 120-170C, the vapour-gas phase is released and vanillin is extracted from the obtained mixture or solution, followed by recycling the obtained aqueous solution of sulphurous anhydride and sodium sulphate into a solution of sodium bisulphite.

EFFECT: method enables to avoid the use of sulphuric acid and alkali when purifying vanillin, widely used in food, perfume, cosmetic and pharmaceutical industry.

5 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of separating vanillin, which is widely used in food, perfume-cosmetic and pharmaceutical industries, from lignin oxidation products by reacting vanillin-containing extracts with aqueous sodium hydrosulphite NaHSO3 solutions. The solutions used have sodium hydrosulphite concentration of 320-400 g/l and the vanillin-hydrosulphite derivative formed is separated from excess sodium hydrosulphite solution in form of a precipitate by filtration, centrifuging or decantation.

EFFECT: method enables to cut consumption of sodium hydrosulphite and increases the distribution ratio of vanillin into the precipitate and aqueous phase from the organic phase, which reduces the volume of extracts and re-extracts when separating vanillin.

3 ex

FIELD: agents for controlling of mouse-like rodents.

SUBSTANCE: invention relates to purification of 1,3-indandione 2-acyl-derivatives which are blood anticoagulants of nondirect action useful in controlling of mouse-like rodents. Claimed method includes precipitation of 1,3-indandione 2-acyl-derivatives followed by decomposition thereof with strong acid, wherein 1,3-indandione 2-acyl-derivatives are precipitated with copper(II) salts in copper salt/1,3-indandione 2-acyl-derivative of (1.1-1.9):1, ant temperature of 40-60°C in medium of solvating organic solvent. Precipitate of copper-containing salt of 1,3-indandione 2-acyl-derivative is treated with potassium hydroxide, then with sulfur acid followed by extraction with chloroform.

EFFECT: simplified process; increased purification level.

1 tbl, 16 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to the improved method for extraction of carbonyl and (or) acid compounds from the complex multicomponent organic liquid mixtures. Method involves treatment of organic liquid mixtures with sodium sulfite an aqueous solution at intensity of mechanical stirring providing formation of uniform emulsion. The content of carbonyl compounds and acids in the parent mixture to be treated is determined and treatment is carried out with 4.16-26% aqueous solution of sodium sulfite as measured 1.05-1.1 mole of sodium sulfite per 1 g-equiv. of carbonyl compound, and in exceeding of the content of acids (g-equiv.) in the parent mixture over the content of carbonyl compounds - with 1 mole sodium sulfite per 1 g-equiv. of acids and in the mass ratio of sodium sulfite aqueous solution to organic mixture = (1-2.5):(2-1) at temperature 15-30°C; if the content of acids in the parent mixture (g-equiv.) is less the content of carbonyl compounds (g-equiv.) then under control of pH value change in an aqueous phase method involves additional addition of mineral or organic acid in the amount as a difference in the content of carbonyl compounds (g-equiv.) and the content of acids (g-equiv.) in the parent charge of organic mixture per treatment at such rate that pH value of aqueous would decrease constantly but not less 6.5. This simple method provides removing both carbonyl compounds and acids being without significant limitations for the content of carbonyl compounds and acids in the parent mixture. Invention can be used in different branches of industry for treatment of compositions or for utilization of carbonyl compounds and (or) acids.

EFFECT: improved method for extraction.

5 cl, 3 tbl, 26 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to the improved method for treatment of organic mixtures from carbonyl compounds and acids by their treatment with sodium sulfite. Method involves using organic mixtures comprising carbonyl compounds and carboxylic acids in the ratio = 1 g-equiv. : 1 g-equiv. or with excess of acids, or with excess of carbonyl compounds. In this case before treatment with sodium sulfite carboxylic acid is added to the parent mixture in the amount to obtain the ratio of carbonyl compounds to acids as 1 g-equiv. per 1 g-equiv. and treatment is carried out with solid sodium sulfite in beaded mill with the mass ratio of the composition charge to glass beads as a grinding agent = 1:(1-2) at the rate of mechanical mixer rotation 1440 rev/min, not less, and in dosing sodium sulfite 1.2-1.5 mole per 1 g-equiv. of carbonyl compounds or excess of acid in the presence of stimulating additive up to practically complete consumption of carbonyl compounds, or carbonyl compounds and acids. Process is carried out in the presence of sodium and potassium hydroxide and acetate and sodium nitrate also as a stimulating additive taken in the amount 1-4% of mass sodium sulfite to be added up to practically complete consumption of carbonyl compounds and acids in composition to be treated. This simple method provides high degree of purification being even in small parent content of carbonyl compounds and acids.

EFFECT: improved method for treatment.

4 cl, 3 tbl, 19 ex

The invention relates to an improved method of separation of functionalized alpha olefins from functionalized nikocevic olefins which involves the processing of raw materials containing functionalized alpha olefins and non-end functionalized olefins, which comprises: a) contacting the feedstock with a linear polyaromatic compound under conditions effective to form a reaction mixture containing adduct of a linear polyaromatic compound - functionalized alpha olefin; (b) isolation of the adduct of linear polyaromatic compound - functionalized alpha-olefin, and optionally also unreacted linear polyaromatic compounds, from the reaction mixture with receiving stream adduct functionalized alpha olefin and flow non-end functionalized olefins; (c) dissociation of the adduct of linear polyaromatic compound - functionalized alpha olefin in the above-mentioned flow of the adduct functionalized alpha-olefin obtaining linear polyaromatic compounds and compositions of functionalized alpha-olefin, and optionally, (d) the selection of the linear polyaromatic soedinitionotkannah alpha-olefins in the above-mentioned compositions alpha olefins increased compared with the concentration of functionalized alpha olefins in the feedstock, and where functionalized olefins or non-end, or alpha are compounds with at least one double bond located in the aliphatic or cycloaliphatic part of the connection, and where the olefin contains a functional group other than the C-C-unsaturation, with this functional group selected from a ketone or hydroxyl group

The invention relates to a method for producing vanillin and lilac aldehyde products of fine organic synthesis
The invention relates to the field of fine organic synthesis, namely the method of selection of vanilla and lilac aldehyde from a solution obtained by oxidation lignindegrading raw materials by extraction of the high-boiling alcohols or esters having a boiling point of more than 130oSince at pH 6-8 with further reextracting aqueous-alkaline solution at pH 10 to 14 and the release of vanillin by acidification with sulfuric acid to pH 5

The invention relates to oxygen-containing compounds, in particular to the processing of still residue of butyl alcohols production method oxosynthesis, more specifically to an improved method of processing waste products of alcohols and aldehydes by the method of propylene hydroformylation

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing 1-hydroxy-4-adamantanone - the active ingredient of immunomodulating drug Kemantan. The method includes oxidising adamantane with 98% sulphuric acid at 70-82C for 9-15 hours and further reaction with fuming nitric acid, followed by heating the reaction mixture for 6 hours at 25-45C.

EFFECT: method enables to obtain the end product using simple and safe technology.

10 ex

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