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Preparation method of thioglycolic acid

A technology of thioglycolic acid and chloroacetic acid, applied in the field of preparation of thioglycolic acid, can solve problems such as difficulty in preparation of thioglycolic acid, poor safety, etc., and achieve the effects of large synthesis conversion rate, high safety, and high product yield

Inactive Publication Date: 2016-01-06
严兴扬
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AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to overcome the difficulties in the preparation of mercaptoacetic acid at present, and the disadvantages of poor safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The reaction was carried out in a 1L four-necked flask equipped with a stirring blade, a thermometer and a dropping funnel: the reaction temperature was controlled by a water bath. Prepare 467 grams of 15% sodium hydrosulfide solution and 237 grams of 20% chloroacetic acid solution. Put all the sodium hydrosulfide into a four-necked flask, add the chloroacetic acid solution in the dropping funnel, add the chloroacetic acid dropwise to the sodium hydrogensulfide solution, the reaction temperature is about 20°C, the dropping time is 1 hour, and the dropping is completed. The reaction solution was warmed to 35°C over 0.5 hours. During the whole reaction process, hydrogen sulfide gas is introduced into the reaction area, the gas volume is about 0.4-0.6L / min.

[0016] Acidify the above reaction solution with concentrated hydrochloric acid to a pH value of 2, extract with an extractant, distill off the solvent under normal pressure, and then distill under reduced pressure to...

Embodiment 2

[0018] The solution preparation and dropwise addition process is the same as in Example 10. The dropwise addition temperature is about 25°C. After the dropwise addition is completed, the reaction is continued for about 1 hour at the same temperature. During the whole reaction process, hydrogen sulfide gas is introduced into the reaction area, the gas volume is about 0.4-0.6L / min.

[0019] The process of acidification, extraction and distillation is the same as above, the yield of the product is greater than 90%, and the purity is greater than 99%.

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Abstract

The invention relates to a preparation method of thioglycolic acid. The method comprises the following steps: adding a chloroacetic acid solution to a sodium sulfhydrate solution in a dropwise manner at normal temperature under normal pressure, and continuously introducing a certain amount of H2S gas in the dropwise addition process and a subsequent reaction process. A high product yield can be obtained through the method. The method has the advantages of simple apparatus and process, low raw material cost, and high synthesis conversion rate being greater than 90%.

Description

technical field [0001] The invention relates to a preparation method of thioglycolic acid. Background technique [0002] Under normal circumstances, there are two main ways to prepare thioglycolic acid by using the sodium hydrosulfide method: one is the low-temperature method, and the other is the high-pressure method. [0003] In the low temperature method, the initial reaction temperature of sodium hydrosulfide and chloroacetic acid is 5-10°C, and the dropwise addition time is 1 hour. After 1 hour of dropwise addition, the temperature rose to about 20°C, and then to 35°C after 1 hour, and was kept at this temperature until the reaction was completed. Because the initial stage of the reaction needs to be reacted for a period of time at low temperature, it is unfavorable for production operation. The reaction time of this method is also longer. Therefore, it is difficult to implement this process in industrialized production. [0004] In the high-pressure method, since t...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C323/52
Inventor 严兴扬
Owner 严兴扬
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