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Method for recovering 2-mercaptobenzothiazole from crystallization mother liquor of ceflriarone sodium

A technology of mercaptobenzothiazole and crystallization mother liquor, applied in the direction of organic chemistry and the like, can solve the problems of cumbersome process operation, large and high-salt wastewater, environmental damage, etc., and achieve the effects of reducing environmental pollution, reducing production costs, and reducing waste discharge.

Active Publication Date: 2012-02-15
石药集团中诺药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process achieves the purpose of recovering 2-mercaptobenzothiazole, it has to be purified and refined repeatedly, the process operation is cumbersome, the energy consumption is high, and a large amount of high-salt wastewater is produced at the same time, which causes certain damage to the environment and brings great environmental protection. pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] ①In a 2000mL round bottom flask, add 1600mL of ceftriaxone sodium mother solution, and add sulfuric acid solution with a mass concentration of 98% to adjust the pH=5.0;

[0025] ②The mother liquor obtained in step ① is heated and distilled, and 1200 mL of solvent is evaporated, and the residual solution after distillation is set aside;

[0026] ③Reduce the temperature of the residual solution obtained in step ② to 10°C, a small amount of solids are precipitated, filter, remove the solids, and use the filtrate for later use;

[0027] 4. the water that adds 4 times of filtrate volumes in step 3. gained filtrate is stirred, and a large amount of solids are separated out;

[0028] ⑤ Filter out the solid obtained in step ④, wash with water, and dry to obtain the target product 2-mercaptobenzothiazole, weighing 12.1 g, with a recovery rate of 93.9%; sampling and HPLC detection, the content is 98.12%.

Embodiment 2

[0030] ①In a 2000mL round bottom flask, add 1600mL of ceftriaxone sodium mother solution, and add sulfuric acid solution with a mass concentration of 85% to adjust the pH=3.0;

[0031] ②The mother liquor obtained in step ① is heated and distilled, and 1280 mL of solvent is evaporated, and the residual solution after distillation is set aside;

[0032] ③Reduce the temperature of the residual solution obtained in step ② to 5°C, a small amount of solid precipitates, filter, filter out the solid, and use the filtrate for later use;

[0033] 4. the water that adds 3 times of filtrate volumes in step 3. gained filtrate is stirred, and a large amount of solids are separated out;

[0034] ⑤ Filter out the solid obtained in step ④, wash with water, and dry to obtain the target product 2-mercaptobenzothiazole, weighing 12.6g, with a recovery rate of 97.8%; sampling and HPLC detection, the content is 98.41%.

Embodiment 3

[0036] ①In a 2000mL round bottom flask, add 1600mL of ceftriaxone sodium mother solution, and add sulfuric acid solution with a mass concentration of 90% to adjust the pH=2.0;

[0037] ②The mother liquor obtained in step ① is heated and distilled, and 1440 mL of solvent is evaporated, and the residual solution after distillation is used for subsequent use;

[0038] ③Reduce the temperature of the residual solution obtained in step ② to 35°C, a small amount of solid precipitates, filter, filter out the solid, and use the filtrate for later use;

[0039] 4. Add water of 1 times the volume of the filtrate to the filtrate obtained in step 3. and stir, and a large amount of solids are precipitated;

[0040] ⑤ Filter out the solid obtained in step ④, wash with water, and dry to obtain the target product 2-mercaptobenzothiazole, which weighs 11.6 g and has a recovery rate of 90.1%. Sampling and HPLC detection reveals that the content is 98.52%.

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PUM

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Abstract

The invention discloses a method for recovering 2-mercaptobenzothiazole from crystallization mother liquor of ceflriarone sodium. The method comprises the following steps of: 1, regulating the pH value of the crystallization mother liquor of ceflriarone sodium to be 2.0-5.0 by using a sulfuric acid solution; 2, heating and distilling the mother solution obtained in the step 1, distilling out a solvent, controlling the solvent distilled out to be 75-90 percent of the total amount of the mother solution, and keeping the distilled residual solution for later use; 3, cooling the residual solution obtained in the step 2 to the temperature of between 0 and 35DEG C, filtering, and keeping filtrate for later use; 4, adding water in an amount which is 1 to 5 times volume of the filtrate into the filtrate obtained in the step 3, stirring, and separating out a solid; and 5, filtering out the solid obtained in the step 4, washing with water, and filtering to obtain the target product of 2-mercaptobenzothiazole. The method has the advantages of simple operation, high yield, low cost, light pollution and the like, and has a good application prospect.

Description

technical field [0001] The invention relates to a method for recovering 2-mercaptobenzothiazole, in particular to a method for recovering 2-mercaptobenzothiazole from ceftriaxone sodium crystallization mother liquor. Background technique [0002] 2-Mercaptobenzothiazole (also known as 2-mercaptobenzothiazole, product name Accelerator M) is an important vulcanization accelerator in the rubber industry, widely used in the manufacture of tires, tapes and other rubber products, and it It can also be used as electroplating additive, brightener, lubricating oil additive, metal preservative, etc. In the pharmaceutical industry, dibenzothiazole disulfide (promoter DM) produced by it is an important raw material for the production of cephalosporin antibiotic intermediates, mainly used to prepare cephalosporin active esters, such as AE-active esters, ceftazidime Active esters, cefazolan active esters, cefdinir active esters, cefixime active esters, etc. [0003] In the production pr...

Claims

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Application Information

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IPC IPC(8): C07D277/72
Inventor 马文婵卢华郝金恒薛磊磊殷力伟宁文玲李国平
Owner 石药集团中诺药业(石家庄)有限公司