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Production method of high-yield thioglycolic acid

A technology of thioglycolic acid and production method, applied in the production field of high-yield thioglycolic acid, can solve problems such as difficulty in handling electrolyte, increased cost, low yield, etc., and achieves inhibiting thioglycolic acid oxidation reaction, improving yield, and reducing side reactions Effect

Active Publication Date: 2019-03-05
山东沾化金嘉利化工科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because thioglycolic acid contains -SH bonds, it is prone to oxidation reaction to generate dithiodiacetic acid in the production process, resulting in low yield, which is also a technical bottleneck restricting domestic thioglycolic acid production enterprises.
Therefore, how to prevent the oxidation of thioglycolic acid is the key to improving the yield of thioglycolic acid and reducing the production cost of thioglycolic acid. Zhang Zhan et al. used a self-made zinc amalgam reduction column to reduce the thioglycolic acid synthesis solution, reducing dithiodiacetic acid to Thioglycolic acid, U.S. Patent (US: 2594030-1952-4-22) also adopts reduction method to process thioglycolic acid oxidation product, Luo Yanhui adopts self-made electrolyzer to carry out reduction research to thioglycolic acid oxidation product, these experimental results show that although reduction method can improve The yield of thioglycolic acid, but increased the cost, and brought difficulties in the handling of zinc salts, electrolytes, etc., so how to prevent the generation of dithiodiacetic acid is the best way to improve the yield of thioglycolic acid

Method used

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  • Production method of high-yield thioglycolic acid

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Comparison scheme
Effect test

Embodiment 1

[0029] The method for producing high-yield thioglycolic acid by the sodium hydrosulfide method is formed by reacting the following mass parts of synthetic liquid and reducing agent: 200 parts of synthetic liquid, 9 parts of sodium sulfite, and 40 parts of water.

[0030] Among them, the synthetic liquid is a mixture of sodium chloroacetate and sodium hydrosulfide with a molar ratio of 1:1.1.

[0031] The mass concentration of sodium chloroacetate is 50%, and the mass concentration of sodium hydrosulfide is 27%.

[0032] The production method includes the following steps:

[0033] (1) Add 9.0 parts of sodium sulfite to 40 parts of water and stir to dissolve;

[0034] (2) Add the solution obtained in step (1) to the reactor together with 200 parts of synthetic liquid;

[0035] (3) React at 68°C for 16 minutes, and then lower the temperature to 45°C;

[0036] (4) Acidify with 30.0% hydrochloric acid to a pH of 1.1 to obtain an aqueous solution of thioglycolic acid;

[0037] (5) Extract with i...

Embodiment 2

[0039] The method for producing high-yield thioglycolic acid by the sodium hydrosulfide method is formed by reacting the following mass parts of synthetic liquid and reducing agent: 220 parts of synthetic liquid, 4.0 parts of sodium borohydride, and 23.0 parts of water

[0040] Among them, the synthetic liquid is a mixed liquid composed of sodium chloroacetate and sodium hydrosulfide at a molar ratio of 1:1.2, the mass concentration of sodium chloroacetate is 50%, and the mass concentration of sodium hydrosulfide is 27%.

[0041] The production method includes the following steps:

[0042] (1) Add 4.0 parts of sodium borohydride to 23.0 parts of water and stir to dissolve;

[0043] The processing method includes the following steps:

[0044] (2) Add the solution obtained in step (1) to the reactor together with 220 parts of synthetic liquid;

[0045] (3) React at 70°C for 17 minutes, then lower the temperature to 45°C;

[0046] (4) Acidify with 29.0% hydrochloric acid to a pH of 1.1 to ob...

Embodiment 3

[0049] The method for producing high-yield thioglycolic acid by the sodium hydrosulfide method is formed by reacting the following mass parts of synthetic liquid and reducing agent: 250 parts of bottom liquid, 2.0 parts of ascorbic acid + 3.0 parts of sodium sulfite, and 30.0 parts of water.

[0050] Among them, the synthetic liquid is a mixed liquid composed of sodium chloroacetate and sodium hydrosulfide at a molar ratio of 1:1.3, the mass concentration of sodium chloroacetate is 50%, and the mass concentration of sodium hydrosulfide is 27%.

[0051] The processing method includes the following steps:

[0052] (1) Add 2.0 parts of ascorbic acid + 3.0 parts of sodium sulfite to 23.0 parts of water and stir to dissolve;

[0053] (2) Add the solution obtained in step (1) to the reactor together with 250 parts of synthetic liquid;

[0054] (3) React at 72°C for 15 minutes, then lower the temperature to 45°C;

[0055] (4) Acidify with 29.0% hydrochloric acid to a pH of 1.3 to obtain an aque...

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Abstract

The invention relates to a high-yield TGA (thioglycolic acid) preparation method. Raw materials including 200-300 parts by mass of a synthetic liquid, 3-9 parts by mass of a reducing agent and 10-50 parts by mass of water are subjected to a synthetic reaction. According to the method, the yield of TGA is increased by adding the reducing agent in the synthetic process, a TGA oxidation product is eliminated in the bud, the yield of the TGA is increased obviously, pressure for treating TGA oxidation product is reduced, and the production cost is reduced.

Description

Technical field [0001] The invention relates to a method for producing thioglycolic acid, in particular to a method for producing thioglycolic acid with a high yield. Background technique [0002] Thioglycolic acid, abbreviated as TGA, also known as thioglycolic acid, contains both sulfhydryl and carboxylic acid groups in its molecule. It is an important chemical raw material and chemical intermediate and is widely used in chemicals, light industry, and pharmaceuticals. , Oil extraction and mineral processing industries. With the development of fine chemicals, its application areas are expanding and the demand is also increasing rapidly. However, because the domestic production technology is relatively backward and the production capacity is small, especially high-quality thioglycolic acid mainly depends on imports. The industrial production of thioglycolic acid is mainly produced by the reaction of sulfur-containing nucleophiles and chloroacetate. According to the different nu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/02C07C323/52
CPCC07C319/02C07C323/52
Inventor 张广俊王景华崔洪友胡正岭刘勤学杨明刚周子彦宋峰
Owner 山东沾化金嘉利化工科技有限公司
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