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Method for synthesizing glyoxalic acid by oxidation of glyoxal with maleuric ozonide

A technology of ozonide and maleic acid, applied in the direction of ozone oxidation to prepare carboxylic acid, organic chemistry, etc., can solve the problems of poor product quality and low conversion rate

Inactive Publication Date: 2005-12-21
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it has successfully solved the problems of low conversion rate and poor product quality in other glyoxal oxidation methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 29.4g maleic anhydride (0.30mol) and 5ml water, dissolve in 500ml acetic acid, then add 50ml methanol, mix well, control the system temperature at -5°C with ice-salt mixture, stir and pass 3wt% O 3 / O 2 Mixed gas 0.1m 3 After 2.5 hours of ozonation reaction, stop the reaction (the amount of ozone is about 0.34mol), and pass nitrogen gas 0.2m 3 / h1-2min to exclude ozone, and the obtained ozonide turns blue with starch / potassium iodide test paper;

[0019] Take another four-neck bottle, add 43.5g of 40% glyoxal aqueous solution and 100ml of acetic acid, stir and heat to keep the temperature at 35°C;

[0020] Then dropwise add the ozonide (ice water protection) that the first step reaction makes, control the flow rate and make it dropwise in 2 hours, continue to react for about 4 hours until detecting no longer discoloration with starch / potassium iodide test paper, knowing that peroxide has reacted completely;

[0021] Methanol, acetic acid and part of water were...

Embodiment 2

[0023] Take by weighing 29.6g maleic acid (0.30mol), be dissolved in 400ml acetic acid, then add 100ml methyl alcohol, after mixing uniformly, control system temperature between-3 ℃ with ice-salt water mixture, stir and pass 3wt% O 3 / O 2 Mixed gas 0.1m 3 / h for ozonation reaction 2.5 hours to stop the reaction (the amount of ozone is about 0.34mol), nitrogen 0.2m 3 / h1-2min to exclude ozone, and the obtained ozonide turns blue with starch / potassium iodide test paper;

[0024] Take another four-neck bottle, add 43.5g of 40% glyoxal aqueous solution and 100ml of acetic acid, stir and heat to keep the temperature at 35°C;

[0025] Then dropwise add the ozonide (ice water protection) that the first step reaction makes, control the flow rate and make it dropwise in 2 hours, continue to react for about 4 hours until detecting no longer discoloration with starch / potassium iodide test paper, knowing that peroxide has reacted completely;

[0026] 250ml of distilled water was added...

Embodiment 3

[0028] Weigh 29.4g maleic anhydride (0.30mol) and 5ml water, dissolve in 350ml acetic acid, then add 150ml methanol, mix well, control the system temperature between 3°C with ice-salt mixture, stir and pass 3wt% O 3 / O 2 Mixed gas 0.1m 3 After 2.5 hours of ozonation reaction, stop the reaction (the amount of ozone is about 0.34mol), and pass nitrogen gas 0.2m 3 / h1-2min to exclude ozone, and the obtained ozonide turns blue with starch / potassium iodide test paper;

[0029] Take another four-neck bottle, add 43.5g of 40% glyoxal aqueous solution and 100ml of acetic acid, stir and heat to keep the temperature at 35°C;

[0030] Then dropwise add the ozonide (ice water protection) that the first step reaction makes, control the flow rate and make it dropwise in 2 hours, continue to react for about 4 hours until detecting no longer discoloration with starch / potassium iodide test paper, knowing that peroxide has reacted completely;

[0031] Methanol, acetic acid and part of water...

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PUM

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Abstract

This invention has disclosed a kind of method to use maleic acid ozonide to oxidize glyoxal in order to gain glyoxylic acid. This method succeeds in combining maleic acid ozonide oxidizing method with other glyoxal catalyzed oxidizing method, devised a new way of to use maleic acid ozonide to oxidize glyoxal in order to gain glyoxylic acid, it has high concentration and purity with the simple step. This method craft is simple, the whole course reflects mild condition, the supplies are saved, and pollution-free to the environment, help industrialization to cosmically produce.

Description

technical field [0001] The invention relates to a method for using maleic acid ozonide to oxidize glyoxal to synthesize glyoxylic acid. Background technique [0002] Glyoxylic acid (OHCCOOH) has the properties of both aldehyde and carboxylic acid, and is an important organic chemical raw material intermediate and biochemical reagent. Dozens of fine chemical products can be derived from glyoxylic acid, which are widely used in medicine, spices, pesticides, paints, papermaking, food additives and other fields; the application of glyoxylic acid in leather, electronics, and electroplating is in the development stage. In the past ten years, due to the continuous expansion of the application fields of glyoxylic acid downstream products, the market demand for glyoxylic acid has continued to increase, and the output has grown rapidly. The production of glyoxylic acid in my country is relatively backward, and the contradiction between supply and demand is very ...

Claims

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Application Information

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IPC IPC(8): C07C51/34C07C59/147
CPCC07C51/34
Inventor 吾满江·艾力孙自才张亚刚董昕徐同玉胡书明努尔买买提
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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