Synthesis process for preparing glyoxalic acid solution by oxygen catalytic oxidation of glyoxal with nitrogen oxide

A technology of oxygen oxidation and synthesis methods, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylates, etc.

Inactive Publication Date: 2005-07-06
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problems existing in the existing glyoxylic acid production methods, the inventor invented a synthetic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Add 70ml of glyoxal aqueous solution with a mass fraction of 25% and 4.5ml of concentrated hydrochloric acid with a mass fraction of 36% in a 250ml reactor, start magnetic stirring, seal the reactor, open the nitrogen oxide gas valve, and 3 The flow rate of nitrogen oxide gas per hour is passed into the nitrogen oxide gas for 80s. After the nitrogen oxide gas is passed through, the valve is quickly closed, and then the oxygen valve is gradually opened until the pressure in the bottle reaches 0.5Mpa. At the same time, the water bath heats the reactor to 73°C. The absorption of the reaction drops by 0.05Mpa, and the oxygen valve is controlled to make up to the kettle. After 13 hours of reaction, stop stirring and heating, open the reaction kettle, pour out the reaction solution, cool to room temperature, put it in the freezer at about -15°C overnight, filter out the precipitated oxalic acid crystals in the solution, and obtain the product glyoxylic acid aqueous solution. ...

Embodiment 2

[0012] The conditions were the same as those in Example 1, except that the time for passing nitrogen oxide was changed to 70 s. The reaction results were as follows: the conversion rate of glyoxal was 97.1%, and the yield of glyoxylic acid was 84%.

Embodiment 3

[0014] The conditions are the same as those in Example 1, the time for changing nitrogen oxide to 90 s, and the reaction time to 10 h. The reaction results are: the conversion rate of glyoxal is 99%, and the yield of glyoxylic acid is 80.3%.

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Abstract

The invention relates to a synthesis method for catalytic oxygen oxidation of glyoxal aqueous solution to glyoxalic acid aqueous solution with nitrogen oxide, which belongs to the field of the chemical synthesis technology. The catalyst used in the method is exhausted nitrogen oxide gas in industrial production, the oxidizer is cheap industrial oxygen, and the product need only be cooled and crystallized for removing oxalic acid.

Description

Technical field [0001] The invention relates to a synthesis method for preparing an aqueous solution of glyoxylic acid by using oxygen to oxidize an aqueous solution of glyoxal under the catalysis of nitrogen oxide in a closed reactor, belonging to the field of chemical synthesis. Background technique [0002] Glyoxylic acid is the raw material of various fine chemical products, and is an intermediate of spices, medicines, pesticides, paints, amino acids and other products. Cross-linking agent during storage and polymer synthesis. With the development of downstream products, the market demand for high-quality glyoxylic acid has increased rapidly. In 2000, the demand for glyoxylic acid in my country was about 6,000 tons, and the current domestic production is less than 1,000 tons. [0003] At present, the synthesis methods of glyoxylic acid at home and abroad are: glyoxal oxidation method; maleic anhydride ozone oxidation-reduction method; electrochemical method; glycolic ac...

Claims

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Application Information

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IPC IPC(8): C07C51/235C07C59/147
Inventor 周智明徐巧余从煊
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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