Method of vanillin manufacturing

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

 

The invention relates to methods of producing vanillin from lignin-containing raw material and is designed to improve processes for the catalytic oxidation of lignins. Vanillin (4-hydroxy-3-methoxybenzaldehyde) is widely used in food, cosmetic and pharmaceutical industries.

A method of obtaining vanillin by oxidation of an aqueous solution of lignosulfonate in an alkaline medium under pressure at a temperature of 160-170C (433-443) [Kamardine OD, Mass AA Obtaining vanillin from lignosulfonate. // M: CBTI ZINES. 1959. 38]. According to a known method, the reaction mixture contains 300 g per liter of solids liquor and 100 g/l of caustic soda. Oxidation at 160C for 3 h gives a solution with a content of vanillin 7-8 g/l (2.3 to 2.7 wt.% in the calculation of the substrate or 6-7 wt.% in the calculation of the lignin lignosulfonate).

The disadvantages of this method are the high consumption of reagents, alkali (12-14 kg per kg of vanilla) and lignosulfonate (35-40 kg per kg of vanillin). These disadvantages are due to the nature of lignosulfonates, condensed structure, due to the harsh conditions of delignification of wood.

A method of obtaining vanillin from sawdust softwood timber by catalytic oxidation in alkaline medium with oxygen [Epstein RB the Floor is giving vanilla from the wood. // Sat. Tr. RBM. Institute of food industry. 1959. Vol.2. S-213].

The disadvantage of this method is the low yield of the target product in the calculation of raw materials, 1-3 wt.%. Low yield of vanillin by a known method due to the low lignin content in wood is about 20-28%.

The closest creature to the claimed method is a method of producing vanillin (EN 2059599, publ. 10.05.1996) by non-catalytic oxidation with oxygen at elevated temperatures and pressures in an aqueous-alkaline solution of lignin, obtained by enzymatic hydrolysis of softwood or wood affected brown or mottled rot, with the lignin content of 40-90 wt.%. According to a known method all the alkali is introduced into the reactor before the start of the experiment.

The disadvantages of this method are the high consumption of reagents, alkali (23-24 kg per kg of vanilla) and enzymatic lignin (11-15 kg per kg of vanillin). These disadvantages due to the fact that the process takes place largely in the diffusion region, and therefore the yield of vanillin is small compared to the maximum possible in the kinetic region, and consequently, the costs of alkali and lignin are relatively large compared to the minimum possible. Another reason contributing to these shortcomings is the absence of oxidation catalysts, which p is swalat a half to two times to increase the yield of vanillin per lignin and therefore, to reduce the consumption of alkali in the calculation to obtain vanillin [tarabanko V.E., Koropachinsky NV Catalytic methods for the preparation of aromatic aldehydes from lignin-containing raw material. // The chemistry of plant raw materials. 2003. No. 1. Pp.5-25.].

The task of the claimed invention is to cheapen the product by reducing the consumption of alkali and improving the environmental friendliness of the process through the use of enzymatic lignin by oxidation of the latter in vanilla.

This object is achieved in that in the method of producing vanillin catalytic oxidation enzymatic softwood lignins in aqueous-alkaline medium at elevated temperatures and pressures according to the invention the process is carried out at a continuous feeding of alkali in the reactor during 5-150 min in the presence of catalysts based on copper hydroxide.

Common features of the claimed invention and prototype - receiving vanilla oxidation by air oxygen lignin, obtained by enzymatic hydrolysis of softwood or wood affected brown or mottled rot, with the lignin content of 40-90 wt.%, in aqueous-alkaline medium at elevated temperatures and pressure.

Distinguishing features of the claimed invention consists in carrying out the oxidation process when the continuous supply of alkali in the reactor during 5-150 min presets the following catalysts based on copper hydroxide. In the prototype, the same alkali served in the initial moment of time, and the process is carried out without a catalyst.

The main technical result of the invention is to reduce the consumption of alkali per kilogram received vanillin 12-23 kg in the known methods to 7-9 kg in the claimed method. This technical result is fundamentally improves the economy of the process of obtaining vanillin from lignin.

The second technical result of the invention is to reduce the consumption of enzymatic lignin per kilogram received vanillin 11-15 kg up to 6-10 kg This technical result reduces the amount of organic substances formed as by-products in wastewater and improve the environmental friendliness of the process.

Called distinctive features lead to the achievement of the technical result of the claimed invention for the following reasons. With a full load of alkali in the reactor before the beginning of the oxidation process of the alkali in the reaction mass is in large excess compared to necessary for oxidation. The concentration of alkali in the solution factor, greatly accelerating the oxidation of lignins, as dissociatively under the action of alkaline phenolic group (phenolate anions) are oxidized much faster medicationabana phenols. As a result, when a high concentration is AI alkali in solution, the oxidation proceeds in the diffusion mode, i.e. the rate of oxidation is determined by the intensity of mixing. It is known that in the diffusion mode, the output of vanillin is lower in comparison with the process occurring in the kinetic regime [tarabanko V.E., Koropachinsky NV Catalytic methods for the preparation of aromatic aldehydes from lignin-containing raw material. // The chemistry of plant raw materials. 2003. No. 1. C.5-25]. When the continuous supply of alkali in the solution, the reaction rate of oxidation is determined by the feed rate of alkali, thus reducing the feed rate of alkali, it is possible to translate the process of diffusion in the kinetic mode.

Thus, the transition from loading all alkali in the reactor to the mode of its continuous supply translates the process of diffusion in the kinetic regime and, consequently, increases the yield of vanillin per loaded lignin and alkali, i.e. reduces the cost of these reagents in the process.

The second distinctive feature of the claimed invention is the use of catalysts based on copper hydroxide is also linked to the technical result, the growth yield of vanillin in the calculation of the lignin. It is known that such catalysts increase the yield of vanillin and a half to two times in total alkali loading in the reactor before the beginning of the oxidation, therefore, the observed growth of output in the conditions of continuous supply of alkali partly due to additive and catalyst.

Hence, the technical results and the distinctive features of the proposed method are in causal contact with each other. The method is confirmed by specific examples.

Example 1. For the experiment used a rotten pine wood dark brown color, easy kneading fingers, kept visible wood structure. The content of lignin in the substrate 65 wt.%.

In the reactor of 1 liter with a rotating magnetic stirrer was loaded with 23.3 g of substrate, 100 ml of water, 3.13 g pativedha of copper sulfate and 20 ml of 20%NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa for 20 min metering pump filed 80 ml of 20% solution of alkali. The reactor continued to heat with stirring for another 10 min, maintaining the operating temperature of 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The concentration in the reaction mass was 12.7 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass of rotten pine wood and 10.8 wt.%, the consumption of alkali per kilogram formed vanilla - 12,2 kg

Example 2 (prototype). For the experiment used a rotten pine tree is inu dark brown color, easy kneading fingers, kept visible wood structure. The content of lignin in the substrate 65 wt.%.

In the reactor with a rotating magnetic stirrer was loaded with 23.3 g of substrate, 100 ml of water and 100 ml of 40%NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa for 30 min supported operating temperature in the reactor to 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The concentration in the reaction mass was 8.2 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass of rotten pine wood - 7.0 wt.%, the consumption of alkali per kilogram formed vanilla - 24,4 kg

Example 3. For the experiment used a rotten motley decay of pine wood with lignin in the substrate 40 wt.%.

In the reactor with a rotating magnetic stirrer was loaded with 23.3 g of substrate, 100 ml of water, 3.13 g pativedha of copper sulfate and 20 ml of 20%NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa for 150 min metering pump filed 80 ml of 20% solution of alkali. The reactor continued to heat with stirring for another 20 min, maintaining the operating temperature of 160C. Then reacto is cooled, the content of the neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The concentration in the reaction mass was 6.8 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass of rotten pine wood - 5.8 wt.%, the consumption of alkali per kilogram formed vanilla - 14,7 kg

Example 4. For the experiment used a rotten spruce wood dark brown color, easy kneading fingers, kept visible wood structure. The content of lignin in the substrate 85 wt.%.

In the reactor with a rotating magnetic stirrer was loaded 15.0 g of substrate, 100 ml of water, 3.13 g pativedha of copper sulfate and 20 ml of 14%aqueous NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa and within 30 min of dosing pump filed 80 ml of a 14% solution of alkali. The reactor continued to heat with stirring for another 10 min, maintaining the operating temperature of 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The concentration in the reaction mass was 10.9 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass cgnews the th pine wood - of 14.5 wt.%, the consumption of alkali per kilogram formed vanilla - 6,4 kg

Example 5. For the experiment used a rotten pine wood dark brown color, easy kneading fingers, preserving the visible structure of the wood, the lignin content of 90 wt.%.

In the reactor with a rotating magnetic stirrer was loaded with 23.3 g of substrate, 100 ml of water, 0,63 g pativedha of copper sulfate and 20 ml of 20%NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa for 5 min metering pump filed 80 ml of 20% solution of alkali. The reactor continued to heat with stirring for another 25 min, maintaining the operating temperature of 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

The B concentration in the reaction mass was 7.7 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass of rotten pine wood and 6.6 wt.%, the consumption of alkali per kilogram formed vanilla - 13,0 kg

Example 6. For the experiment used a fir wood, gidralizovanny enzymatic product Cellolux-F (sibbiofarm, Berdsk) with lignin in the substrate 70 wt.%.

In the reactor with a rotating magnetic stirrer was loaded 15.0 g of substrate, 100 ml of water, of 6.26 g pativedha of copper sulfate and 20 ml of 14%is of astora NaOH. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa and within 30 min of dosing pump filed 80 ml of a 14% solution of alkali. The reactor continued to heat with stirring for another 10 min, maintaining the operating temperature of 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The B concentration in the reaction mass was 8.7 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass lignindegrading substrate - 11.6 wt.%, the consumption of alkali per kilogram formed vanilla - 8,1 kg

Example 7. For the experiment used pine wood, gidralizovanny multienzyme composition of drugs "Cellolux-A (sibbiofarm, Berdsk), "BrewZyme BGX" ("Polfa Tarchomin Pharmaceutical Works S.A., Poland) and Rapidase CR" ("DSM Food Specialties Beverage Ingredients, Netherlands) in a weight ratio of 5.4%, 47,3% 47,3%. The content of lignin in the substrate 70 wt.%.

In the reactor with a rotating magnetic stirrer was loaded 15.0 g of substrate, 100 ml of water, of 6.26 g pativedha of copper sulfate and 20 ml of 14%aqueous NaOH solution. The reactor was heated to 160C, gave air to the working pressure of 2.0 MPa and within 30 min of dosing pump filed 80 ml of a 14% solution of alkali. The reactor continued to heat up with re what asianam another 10 min, maintaining the working temperature of 160C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The B concentration in the reaction mass was 8.7 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass lignindegrading substrate - 11.6 wt.%, the consumption of alkali per kilogram formed vanilla - 7,9 kg

Example 8. For the experiment used a rotten pine wood dark brown color, easy kneading fingers, preserving the visible structure of the wood, the lignin content of 90 wt.%.

In the reactor with a rotating magnetic stirrer was loaded with 8.0 g of substrate, 100 ml of water, to 12.52 g pativedha of copper sulfate and 20 ml of an 8%aqueous NaOH solution. The reactor was heated to 110C, gave air to the working pressure of 0.2 MPa for 120 min metering pump filed 80 ml of 8% solution of alkali. The reactor continued to heat with stirring for 60 min, maintaining the operating temperature of 110C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The B concentration in the reaction mass was 4.7 g/l in terms of the final volume of the reaction is the ion mass. The yield of vanillin per mass of rotten pine wood - to 11.7 wt.%, the consumption of alkali per kilogram formed vanilla - 8,5 kg

Example 9. For the experiment used pine wood, gidralizovanny multienzyme composition of drugs "Cellolux-A (sibbiofarm, Berdsk) and Rapidase CR" ("DSM Food Specialties Beverage Ingredients, Netherlands) in a weight ratio of 10.3% and 89.7%of it. The content of lignin in the substrate 90 wt.%.

In the reactor with a rotating magnetic stirrer was loaded 15.0 g of substrate, 100 ml of water, of 6.26 g pativedha of copper sulfate and 20 ml of an 8%aqueous NaOH solution. The reactor was heated to 180C, gave air to the working pressure of 3.0 MPa for 10 min metering pump filed 80 ml of 8% solution of alkali. The reactor continued to heat with stirring for another 5 min, maintaining the operating temperature of 180C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The B concentration in the reaction mass amounted to 6.78 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass lignindegrading substrate, and 9.0 wt.%, the consumption of alkali per kilogram formed vanilla - 5,9 kg

Example 10. For the experiment used a pine wood, the guide is risovannoy multienzyme composition of drugs "BrewZyme BGX" ("Polfa Tarchomin Pharmaceutical Works S.A.", Poland) and Rapidase CR" ("DSM Food Specialties Beverage Ingredients, Netherlands) in a weight ratio of 50% and 50%. The content of lignin in the substrate 67 wt.%.

In the reactor with a rotating magnetic stirrer was loaded 40,0 g substrate, 100 ml of water, of 6.26 g pativedha of copper sulfate and 20 ml of 30%NaOH solution. The reactor was heated up to 130C, gave air to the working pressure of 2.0 MPa for 90 min metering pump filed 80 ml of 30% solution of alkali. The reactor continued to heat with stirring for further 30 minutes, maintaining the operating temperature of 130C. Then the reactor was cooled, the contents were neutralized 30%sulfuric acid to pH 3-4.

Vanilla was determined by exhaustive extraction with chloroform, followed by analysis by GLC. The concentration in the reaction mass was 10.9 g/l in terms of the final volume of the reaction mass. The yield of vanillin per mass lignindegrading a substrate of 5.45 wt.%, the consumption of alkali per kilogram formed vanilla - 13,7 kg

A method of producing vanillin oxidation by air oxygen lignin, obtained by enzymatic hydrolysis of softwood or wood affected brown or mottled rot, with the lignin content of 40-90 wt.% in aqueous-alkaline medium at elevated temperature and pressure, wherein the process is carried out in the presence of catalysts based on copper hydroxide if not the reading of the filing of the alkali solution in the reactor during 5-150 minutes.



 

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3 ex

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