Method for preparing thiodiglycolic acid

A technology for thiodiglycolic acid and dibutyl thiodiglycolic acid, which is applied in the field of preparation of thiodiglycolic acid, can solve the problems of serious environmental pollution, consumption of extraction solvent, poor product purity, etc. The effect of high rate and short production cycle

Inactive Publication Date: 2011-04-06
三门峡奥科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The biggest disadvantage of this process is the high cost. It is necessary to neutralize the chloroacetic acid with alkali to form sodium chloroacetate, and then acidify the sodium thiodiacetate formed by the reaction of sodium chloroacetate and sodium sulfide, resulting in a large amount of sodium chloride. The waste liquid is not easy to handle and causes serious environmental pollution
In addition, the process operation is complicated, the product yield is only 76%, the product purity is poor, the color is not good, and a large amount of extraction solvent is consumed

Method used

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  • Method for preparing thiodiglycolic acid

Examples

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Embodiment 1

[0027] A kind of preparation method of thiodiglycolic acid, it comprises the following steps: in flask, add dimethyl thiodiglycolate 100g, mass percent concentration is 5% hydrochloric acid 200ml, after refluxing 3h, distill and reclaim 50ml methanol and water, remaining The reaction mixture was crystallized by cooling, and dried by suction filtration to obtain about 78 g of white granular powder thiodiglycolic acid (melting point 128-131 ° C), and 174 g of mother liquor. The yield of this step is 92.5%, and the purity is 99.7%.

Embodiment 2

[0029] A kind of preparation method of thiodiglycolic acid, it comprises the following steps: in flask, add dimethyl thiodiglycolate 100g, mass percentage concentration is the sulfuric acid 400ml of 5%, after reflux 4h, distill out 250ml methanol and water, remaining The reaction mixture was crystallized by cooling, and dried by suction filtration to obtain about 77g of white granular powder thiodiglycolic acid (melting point 128-131°C) and 176g of mother liquor. The yield of this step is 91.3%, and the purity is 99.6%.

Embodiment 3

[0031] A kind of preparation method of thiodiglycolic acid, it comprises the following steps: add thiodiglycolic acid diethyl ester 116g in the flask, mass percent concentration is 10% phosphoric acid 200ml, after refluxing 6h, distill out 60ml ethanol and water, remaining The reaction mixture was crystallized by cooling, and dried by suction filtration to obtain about 76 g of white granular powder thiodiglycolic acid (melting point 128-131 ° C), and 176 g of mother liquor. The yield of this step is 90.2%, and the purity is 99.6%.

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Abstract

The invention discloses a method for preparing thiodiglycolic acid, which comprises the following steps: adding thiodiglycolic acid dialkyl ester in acidic liquid; heating and refluxing for 1 to 6 hours; recovering a byproduct, namely alcohol, and water; and cooling the residual reaction mixture, crystallizing, filtering and drying and obtaining finished product. The thiodiglycolic acid dialkyl ester may be thiodiglycolic acid dimethyl ester, thiodiglycolic acid diethyl ester, thiodiglycolic acid dipropyl ester or thiodiglycolic acid dibutyl ester. In the method, the process is simple, the reaction yield is high, the product colour and luster and purity are high, extractant is not used, the mother liquid can be recycled, and the environment in an entire preparation process is good. The method has a bright industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of thiodiglycolic acid. Background technique [0002] Thiodiglycolic acid has important uses in industry, and is an important intermediate in the synthesis of thiophene-2,5-dicarboxylic acid, polyethylenedioxythiophene, etc. It is an important raw material for the production of brighteners, high-efficiency agricultural fungicides and anticancer drugs, and is a fine and special chemical intermediate that is currently hotly developed in China. [0003] Its traditional synthetic method is to use chloroacetic acid and sodium sulfide as raw materials, neutralize chloroacetic acid with alkali to sodium chloroacetate, react sodium chloroacetate and sodium sulfide to generate sodium thiodiacetate, and then acidify and extract. To obtain thiodiglycolic acid. Its reaction formula is as follows: [0004] [0005] [0006] [0007] The biggest di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/20
Inventor 赵松芳兀吉康袁淑芳辛安波
Owner 三门峡奥科化工有限公司
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