Method for Synthesizing Glyoxylic Acid by Ozonation of Maleic Anhydride Mixed Solvent

A maleic anhydride and mixed solvent technology, applied in the field of glyoxylic acid preparation, can solve the problems of low space-time yield of equipment, low yield of raw materials, easy corrosion of equipment, etc., and achieve good mass transfer effect, method and process Simple, short hydrolysis time effect

Active Publication Date: 2021-02-09
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oxalic acid electrolytic reduction method and the glyoxal oxidation method have both realized industrial production, however, the oxalic acid electrolytic reduction method mainly has the disadvantages that the yield of the equipment is low when the space is empty, and the product contains a large amount of oxalic acid that is difficult to separate.
The glyoxal oxidation method is the most widely used, but its disadvantages are large solvent loss, easy corrosion of equipment, low yield of raw materials, poor product quality, and serious environmental pollution
The disadvantage of selective oxidation of glycolic acid is that the cost of synthesis is relatively high, and the key is to obtain a highly selective catalyst
Dibromoacetic acid hydrolysis reaction conditions are mild, but the separation of reaction products is difficult, and the price of raw materials used is high, and the product yield and quality are not very satisfactory.
Adopting this method requires higher requirements for ozone generators, higher equipment investment, greater energy consumption, and the production rate is highly dependent on hydrogenation catalysts, requiring expensive hydrogenation catalysts, resulting in higher production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat it in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of ethyl acetate to carry out the hydrolysis reaction, the hydrolysis temperature is 65°C, and the hydrolysis time is 50min.

[0070] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 5mL methanol + 10mL ethyl acetate mixed solvent, and carry out ozonation. To be able to fully contact, control the reaction temperature at 5°C and the time for 3h.

[0071] c. At the end of the ozone oxidation stage, stop feeding ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.

[0072] d. Slowly add the reacted solution into the 8% sulfurous acid solution, and control the system temperature at 55-65°C.

[0073] e. After all the addition, slowly add about a certain amount of CaO, then add 5mL of water, and control the temperature below 10°C, after that, ...

Embodiment 2

[0078] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat it in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of n-hexane to carry out the hydrolysis reaction, the hydrolysis temperature is 60°C, and the hydrolysis time is 60min.

[0079] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 7.5mL methanol + 15mL n-hexane mixed solvent, and carry out ozonation. Ozone is blown in from the bottom of the maleic acid solution to make the ozone and solution To be able to fully contact, the reaction temperature is controlled at 0°C and the time is 2.5h.

[0080] c. At the end of the ozone oxidation stage, stop feeding the ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.

[0081] d. Slowly add the reacted solution into 8% sulfurous acid solution, and control the system temperature at 55-65°C.

[0082] e. After all the addition, slowly add about a certain ...

Embodiment 3

[0087] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of ethyl acetate to carry out the hydrolysis reaction, the hydrolysis temperature is 65°C, and the hydrolysis time is 30min.

[0088] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 5mL methanol + 10mL ethyl acetate mixed solvent, and carry out ozonation. To be able to fully contact, control the reaction temperature to 5°C and the time to 2.5h.

[0089] c. At the end of the ozone oxidation stage, stop feeding ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.

[0090] d. Slowly add the reacted solution into the 10% sulfurous acid solution, and control the system temperature at 55-65°C.

[0091] e. After all the addition, slowly add about a certain amount of CaO, then add 5mL of water, and control the temperature below 20°C, after that, l...

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PUM

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Abstract

The invention relates to a method for synthesizing glyoxylic acid by means of ozonizing maleic anhydride and mixed solvents, and belongs to the field of technologies for preparing glyoxylic acid. The method for synthesizing the glyoxylic acid by means of ozonizing the maleic anhydride and the mixed solvents is low in cost. The method includes steps of carrying out hydrolysis, ozone oxidation, reduction, reduced-pressure distillation, crystallization and the like on the inexpensive maleic anhydride in the mixed solvents to ultimately obtain glyoxylic acid solid. The method has the advantages that the glyoxylic acid solid with high purity can be directly obtained by the aid of the method, and products are high in quality and wide in application; the method is easy to implement and high in glyoxylic acid yield, the maleic anhydride can be converted into the glyoxylic acid at a low price, the method can be used for industrial large-scale production, and certain contribution can be made for solving the problem of situation of excessive maleic anhydride; optimization of the traditional processes for producing the glyoxylic acid and elimination of backward processes can be stimulated, environment-friendly oxidizing agents are adopted, and accordingly huge contribution can be made for environmental protection.

Description

technical field [0001] The invention relates to a method for synthesizing glyoxylic acid by ozonation of a mixed solvent of maleic anhydride, and belongs to the technical field of glyoxylic acid preparation. Background technique [0002] Glyoxylic acid is an important organic chemical intermediate raw material. In recent years, its downstream products have been continuously developed, and glyoxylic acid has a good market prospect. Glyoxylic acid can synthesize vanillin, 2-hydroxyquinoline, 2-hydroxyphosphoacetic acid, D-hydroxyphenylglycine, allantoin, etc. In recent years, with the rapid development and development of glyoxylic acid downstream products, the market Demand continues to expand. In particular, the demand for high-purity solid glyoxylic acid will increase, and the application range will be wider. [0003] At present, the production methods of glyoxylic acid mainly include oxalic acid electrolytic reduction method, glyoxal oxidation method, glycolic acid select...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/25C07C59/147
CPCC07C51/087C07C51/25C07C59/147C07C57/145
Inventor 朱学军邓俊张毅李玉峰唐酞峰
Owner PANZHIHUA UNIV
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