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Method for preparing vanilline

A technology of vanillin and methyl phenol, which is applied in the field of compound preparation, can solve the problems of phenol-containing wastewater, serious environmental pollution, high production cost, etc., achieve high product yield, reduce production cost, and save equipment investment

Active Publication Date: 2013-06-05
毕新民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Journal of Huaihai Institute of Technology" No. 3, 2000 reported a method for preparing vanillin, and evaluated the advantages and disadvantages of the above-mentioned technology: the nitrosation method produces a large amount of waste water, and the environment is seriously polluted; the glyoxylic acid process also exists With the problem of phenolic wastewater, its production cost is relatively high, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 2-bromo-4-methylphenol (hereinafter referred to as monobromophenol) 75g (0.4 mole) in the medium-pressure reactor (pressure-resistant 2.5MPa) of 1000ml, 28% industrial sodium methylate solution 155g (containing sodium methylate 0.8 mol), basic copper carbonate 2.3g (0.01 mol). After blowing in nitrogen to replace the air in the kettle, the reaction was carried out at 100° C. and a stirring speed of 500 rpm for 3 hours. Then vent the pressure after passing the cooling water to cool down, open the lid of the kettle and drop into the still 1g of cobalt acetate, 72g of solid caustic soda (1.8 moles), 340ml of anhydrous methanol, feed oxygen and at 100 ℃ and a stirring speed of 500 rpm The reaction was carried out for 8 hours. Cool down, lower the temperature, take out the solution, first filter out the solids, then distill off the methanol, then add hydrochloric acid to adjust the pH of the solution to 4-5. After the solution was cooled in water at 15°C for 2 hours, v...

Embodiment 2

[0023] Add 75g (0.4 moles) of monobromophenol, 125g (containing 0.65 moles of sodium methoxide) of 28% industrial sodium methoxide solution, and 2.3g (0.01 moles) of basic copper carbonate in a 1000ml medium-pressure reactor (2.5MPa pressure resistance). . After blowing in nitrogen to replace the air in the kettle, the reaction was carried out at 100° C. and a stirring speed of 500 rpm for 3 hours. Then the cooling water is cooled to 40°C, the pressure is released, the lid of the kettle is opened, and 1g of cobalt acetate is dropped into the kettle, 72g of solid caustic soda (1.8 moles), 300ml of anhydrous methanol, and oxygen is fed into the kettle at 100°C and 500 rpm. The reaction was carried out for 9 hours at a constant stirring speed. Cool down, lower the temperature, take out the solution, first filter out the solids, then distill off the methanol, then add hydrochloric acid to adjust the pH of the solution to 4-5. After the solution was cooled in water at 15°C for 2 ...

Embodiment 3

[0025] Add monobromophenol 75g (0.4 mole) in the medium-pressure reactor (2.5MPa of pressure resistance) of 1000ml, 18% industrial sodium ethylate solution 300g (containing sodium ethylate 0.8 mole), basic copper carbonate 2.3g (0.01 mole) . After blowing in nitrogen to replace the air in the kettle, the reaction was carried out at 100° C. and a stirring speed of 500 rpm for 3 hours. Then pass cooling water to cool down to 40°C, and then put 1g of cobalt acetate, 72g (1.8 moles) of solid caustic soda, 200ml of absolute ethanol into the kettle, and feed oxygen at 100°C for 8 hours. After cooling and cooling down, the solution was taken out. Ethanol was distilled off first, and then hydrochloric acid was added to adjust the pH of the solution to 4-5. The solution was cooled in cold water at 15°C for 2 hours, and then crystals were precipitated. After filtration, the crude ethyl vanillin is distilled under reduced pressure, recrystallized from ethanol aqueous solution, recryst...

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PUM

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Abstract

The invention discloses a method for preparing vanilline, which comprises the following steps: taking 2-bromine-4-methyl phenol as a raw material, carrying out a methoxylation reaction firstly, then carrying out an oxidation reaction for preparing mother liquid containing the vanilline, and finally, obtaining the vanilline by separation and refinement. The method is characterized by comprising the following steps: adding 1 mol of 2-bromine-4-methyl phenol, 1.0-3.0 mols of alkoxyl metal salt, 0.005-0.1 mol of copper salt catalyst and 0-0.05 mol of catalyst promoter into an intermediate-pressure reaction kettle and reacting at the temperature of 70-125 DEG C; after completing the reaction, cooling, carrying out pressure relief, then putting a cobalt salt catalyst, right amount of alcohol solvent and right amount of solid alkali into the kettle, afterwards introducing oxygen into the solution to carry out oxidation reaction and preparing the mother liquid containing the vanilline. The method used for producing the vanilline has the advantages of high yield and low production cost. The production wastewater can achieve zero discharge after comprehensive utilization, thus thoroughly solving the problem of wastewater pollution in the production of the vanilline.

Description

[0001] This application is a divisional application of the invention patent application with application number 200610043309.4. The invention title of the original patent application is "a method for preparing 2-bromo-4-methylphenol and a method for preparing vanillin", and the filing date is March 16, 2006. technical field [0002] The invention relates to a preparation method of a compound, in particular to a method for preparing vanillin. Background technique [0003] Vanillin is a broad-spectrum spice widely used in food industry, pharmaceutical industry and organic synthesis. The current production process is mainly glyoxylic acid method and nitrosation method using guaiacol as raw material. "Journal of Huaihai Institute of Technology" No. 3, 2000 reported a method for preparing vanillin, and evaluated the advantages and disadvantages of the above-mentioned process: the nitrosation process produces a large amount of waste water, and the environment is seriously pollute...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/58C07C45/32C11B9/00
Inventor 毕新民
Owner 毕新民