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Method for preparing glyoxylate

A technology of glyoxylic acid and glyoxal, applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low yield, easy environmental pollution, easy corrosion of equipment and cost, etc. The effect of stable quality, avoiding easy environmental pollution and improving productivity

Active Publication Date: 2007-07-25
SHANGHAI SHISI CHEM PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem solved by the present invention is to provide a preparation method of glyoxylic acid, so as to overcome the disadvantages of easy environment pollution, easy corrosion of equipment, high cost and low yield in the existing preparation method

Method used

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  • Method for preparing glyoxylate
  • Method for preparing glyoxylate

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 300ml (2.55mol) of 40% glyoxal solution into a 2500ml reactor equipped with a reflux condenser, stirrer, and thermometer, stir and cool, control the temperature at 5±2°C, and slowly drop 30% peroxide in 4 hours at the same time 290ml (2.55mol) of hydrogen solution, 260ml (0.255mol) of 14% ferrous sulfate solution and 100ml (0.65mol) of 10% ammonia solution, keep at 5±2°C for 4 hours, let stand overnight, filter the reaction solution to remove solid by-products 300ml of water-carrying agent toluene was added to the reaction mother liquor, heated to reflux, water removed, and water-carrying agent toluene was evaporated to obtain an oxidation product.

[0024] Add 100ml of concentrated sulfuric acid and 600ml of absolute ethanol to the oxidized product, perform esterification at 120°C for 2 hours, then distill under reduced pressure, collect at 0.01Mpa, 175°C to obtain the esterified product.

[0025] 100 ml of 16% sulfuric acid was added to the esterification product,...

Embodiment 2

[0027] Add 600ml (2.55mol) of 20% glyoxal solution into a 2500ml reactor equipped with a reflux condenser, stirrer, and thermometer, stir and cool, control the temperature at 6±2°C, and slowly drop 20% peroxide within 4 hours Hydrogen solution 435ml (2.55mol), 14% ferrous sulfate solution 260ml (0.255mol) and 20% ammonia solution 60ml (0.77mol), keep the controlled temperature reaction for 4 hours, stand overnight, the reaction solution is filtered to remove solid by-products, react Add 300ml of water-carrying agent toluene to the mother liquor, heat to reflux, remove water, distill out the water-carrying agent toluene, and obtain the oxidation product. Add 300ml of water-carrying agent toluene to the reaction solution, heat to reflux, remove water, and distill the water-carrying agent toluene to obtain the oxidation product.

[0028] Add 100ml of concentrated sulfuric acid and 600ml of absolute ethanol to the oxidation product, react at 120°C for 2 hours, then distill under r...

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Abstract

This invention discloses a method for preparing glyoxalic acid. The method comprises: oxidizing glyoxal solution by hydrogen peroxide in the presence of ferrous sulfate catalyst and cocatalyst, esterifying for separation, and hydrolyzing to obtain the target product. The purity, yield and melting point of glyoxalic acid are higher than 98%, 85%-90% and 96.2-97.9 deg.C, respectively. Compared with the present techniques, the method can increase glyoxalic acid yield by adding cocatalyst (ammonia solution). Besides, the method has improved operation condition, thus avoiding environmental pollution and apparatus corrosion. The product has stable quality.

Description

technical field [0001] The invention relates to a preparation method of glyoxylic acid. Background technique [0002] Glyoxylic acid is an important intermediate in organic synthesis, especially as an intermediate in the synthesis of vanillin, ethyl vanillin, allantoin, p-hydroxyphenylglycine, etc. Widely used, its structural formula is as follows: [0003] [0004] In the prior art, the commonly used preparation method of glyoxylic acid has nitric acid oxidation method, hydrogen peroxide, electrochemical method etc., Zhang Kefeng, modern chemical industry, reported in 1992 (4) 62-63 to prepare acetaldehyde with nitric acid oxidation glyoxal Acid method, the reaction process of this method is accompanied by the generation of a large amount of nitrogen oxides, serious environmental pollution, the reaction process is carried out under strong acidic conditions, and the equipment is extremely easy to corrode. [0005] Cui Zhimin, Chemical World, reported in 2004 (9) 478-480...

Claims

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Application Information

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IPC IPC(8): C07C51/235C07C59/147
Inventor 揭元萍宋振
Owner SHANGHAI SHISI CHEM PROD
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