Method utilizing cefotaxime acid waste-liquor to prepare 2, 2'-dithio-dibenzo thiazole

A technology of dithiodibenzothiazole and cefotaxime acid, applied in the direction of organic chemistry and the like, can solve the problems of lack of low cost and effective utilization of cefotaxime acid waste liquid, high cost and high energy consumption, and achieve good economic benefits , low cost and low energy consumption

Inactive Publication Date: 2012-12-05
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing recovery process of 2-mercaptobenzothiazole in cefotaxime production waste liquid is complicated to operate, and the obtained product needs multiple purifications, which

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (a) Add 13.56 g of 20% hydrogen peroxide solution dropwise to 450 ml of cefotaxime acid waste liquid, control the reaction temperature to 10°C, and the reaction time to 60 min, wherein the dropping process is controlled at 60 minutes;

[0021] (b) After the reaction was completed, the temperature was lowered to 0°C, the crystal growth time was 60 min, vacuum filtration or centrifugal filtration, and the filter cake was vacuum-dried at 40°C for 2 h to obtain 2,2′-dithiodibenzothiazole 28.38 g. Its melting point is 179°C, and its purity is 98.5% as detected by high-performance liquid chromatography, which meets the technical requirements for superior products in GB / T 11408-89. It can be used as a vulcanization accelerator for the vulcanization process of rubber.

Embodiment 2

[0023] (a) Add 7.52 g of 50% aqueous hydrogen peroxide solution dropwise to 450 ml of cefotaxime acid waste liquid, control the reaction temperature to 35°C, and the reaction time to 120 min, wherein the dropping process is controlled at 30 minutes;

[0024] (b) After the reaction was completed, the temperature was lowered to 10°C, the crystal growth time was 30 min, vacuum filtration or centrifugal filtration, and the filter cake was vacuum-dried at 40°C for 2 h to obtain 2,2′-dithiodibenzothiazole 29.63 g, with a melting point of 180°C, detected by high performance liquid chromatography, with a purity of 98.6%, meeting the technical requirements for superior products in GB / T 11408-89, and can be used as a vulcanization accelerator for vulcanization of rubber.

Embodiment 3

[0026] (a) Add 10.25 g of 30% aqueous hydrogen peroxide solution dropwise to 450 ml of cefotaxime acid waste liquid, control the reaction temperature to 25°C, and the reaction time to 90 min, wherein the dropping process is controlled at 45 minutes;

[0027] (b) After the reaction was completed, the temperature was lowered to 5°C, the crystal growth time was 40 min, vacuum filtration or centrifugal filtration, and the filter cake was vacuum-dried at 40°C for 2 h to obtain 2,2′-dithiodibenzothiazole 29.72 g, with a melting point of 180°C, detected by high performance liquid chromatography, with a purity of 98.7%, meeting the technical requirements for superior products in GB / T 11408-89, and can be used as a vulcanization accelerator for vulcanization of rubber.

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PUM

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Abstract

The invention discloses a method utilizing cefotaxime acid waste-liquor to prepare 2, 2'-dithio-dibenzo thiazole. The method comprises the following steps of (a) dropwise adding an aqueous hydrogen peroxide solution into the cefotaxime acid waste-liquor, wherein the addition quantity of the aqueous hydrogen peroxide solution is determined based on 2-thiol group benzothiazole in the cefotaxime acid waste-liquor, and the molar ratio between the 2-thiol group benzothiazole and hydrogen peroxide is 1:0.5-1.5; under the condition of 10-35 DEG C, reacting for 60-120 minutes; (b) after the reaction is finished, lowering the temperature to 0-10 DEG C, growing crystal for 30-60 minutes, and filtering; and a filter cake is dried, obtaining the 2, 2'-dithio-dibenzo thiazole. The method has the advantages of low cost, waste utilization, energy saving and environmental protection, the obtained product has high yield and purity. The prepared 2, 2'-dithio-dibenzo thiazole can be used as a vulcanization accelerator to be used for vulcanization processing of rubber.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a method for preparing 2,2'-dithiodiphenyl. Background technique [0002] The AE-active ester method is the most commonly used method to produce cefotaxime acid because of its simple process and convenient operation. The synthesis route of the method is as follows: 7-aminocephalosporanic acid (formula Ⅰ) and AE-active ester (formula Ⅱ) undergo a substitution reaction in the presence of triethylamine to generate 2-mercaptobenzothiazole (formula Ⅲ ) and cefotaxime triethylamine (formula Ⅳ), then acidified with hydrochloric acid to obtain the product cefotaxime acid (formula Ⅴ) [0003] . [0004] After the reaction is completed and the cefotaxime acid is extracted, the remaining waste liquid contains a large amount of 2-mercaptobenzothiazole, an organic solvent, and triethylamine hydrochloride. Shi Qizeng and others reported a method for recovering 2-mercaptobenzothi...

Claims

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Application Information

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IPC IPC(8): C07D277/78
Inventor 张军立刘倩姚宝林王玉红高俊艳
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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