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Process for recovering triphenyl phosphine oxide and 2-mercaptobenzothiazole from production waste liquid of cephalothin active ester

A technology for mercaptobenzothiazole and triphenylphosphine oxide, which is applied in the field of recovering triphenylphosphine oxide and 2-mercaptobenzothiazole, can solve the problems of poor product purity, high recovery cost, low recovery rate, etc. The effect of large implementation value and potential social and economic benefits, easy operation and high recovery rate

Inactive Publication Date: 2008-10-22
ZHEJIANG UNIV OF TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method procedure is loaded down with trivial details, and does not relate to the recovery method of triphenylphosphine oxide (Liu Huiling, Zhou Ding, Zhang Zhanping, Han Hongbin, Liu Guihua, the method for reclaiming 2-mercaptobenzothiazole from cefotaxime sodium production waste residue. Chemical Environmental Protection, 1999 , 19(5), 303.)
The several methods mentioned above have certain limitations, mainly reflected in the low recovery rate, cumbersome operation, poor product purity, high energy consumption, and high recovery costs.

Method used

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  • Process for recovering triphenyl phosphine oxide and 2-mercaptobenzothiazole from production waste liquid of cephalothin active ester
  • Process for recovering triphenyl phosphine oxide and 2-mercaptobenzothiazole from production waste liquid of cephalothin active ester

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1 reclaims the method for triphenylphosphine oxide and 2-mercaptobenzothiazole from ceftazidime active ester production waste liquid (theoretical amounts of TPPO and M are respectively 166.8g and 118.0g)

[0023] Add 4% sodium hydroxide aqueous solution dropwise at 10°C to 2L of waste liquid produced by ceftazidime side chain acid and dibenzothiazole disulfide under the action of triphenylphosphine, adjust the pH value to 10-11, and continue stirring after dropping React for 30 minutes, static layering. The organic layer was decompressed to recover the organic solvent, and the obtained solid waste residue weighed 250.0 g. Recrystallized with 125 g of toluene to obtain 155.0 g of white crystalline solid. The product was triphenylphosphine oxide. The rate is 92.9%. Heat the water layer to 65°C, use 12% hydrochloric acid to adjust the pH value of the system to 1.0-2.0, a white solid precipitates, filter while hot, wash with water, and dry to obtain 117.0 g of w...

Embodiment 2

[0024] Embodiment 2 reclaims the method for triphenylphosphine oxide and 2-mercaptobenzothiazole from ceftazidime active ester production waste liquid (theoretical amounts of TPPO and M are respectively 168.0g and 105.0g)

[0025] Add 4% sodium hydroxide aqueous solution dropwise to 2L of waste liquid produced by ceftazidime side chain acid and dibenzothiazole disulfide under the action of triphenylphosphine, adjust the pH value to 11-12 at 0°C, and continue stirring after dropping Reaction for 1.0 hour, static layering. The organic layer was decompressed to recover the organic solvent, and the obtained solid waste residue weighed 245.0 g. It was recrystallized with 2450 g of n-hexane to obtain 108.0 g of a white crystalline solid. The product was triphenylphosphine oxide. The recovery rate was 64.3%. Heat the water layer to 50°C, use 18% hydrochloric acid to adjust the pH of the system to 1.0-2.0, a white solid precipitates, filter while hot, wash with water, and dry to obta...

Embodiment 3

[0026] Embodiment 3 reclaims the method for triphenylphosphine oxide and 2-mercaptobenzothiazole from AE active ester production waste liquid (theoretical amounts of TPPO and M are respectively 165.0g and 95.0g)

[0027] Add 10% sodium hydroxide aqueous solution dropwise at 40°C to 2L waste liquid produced by aminothiaxamic acid and dibenzothiazole disulfide under the action of triphenylphosphine, adjust the pH value to 11-12, and continue stirring for 1.5 hours after dropping , static stratification. The organic layer was decompressed to recover the organic solvent, and the obtained solid waste residue weighed 256.0 g. It was recrystallized with 128 g of n-propanol to obtain 134.1 g of a white crystalline solid. , and the recovery rate was 81.3%. Heat the water layer to 40°C, use 15% hydrochloric acid to adjust the pH of the system to 1.0-2.0, a white solid precipitates, filter while hot, wash with water, and dry to obtain 93.0 g of white powder solid, the product is 2-merca...

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Abstract

The invention discloses a method for recycling triphenyl phosphine oxide and 2-mercaptobenzothiazole from the production waste liquid of cephalosporin active ester, which includes the following steps: 1 to 10 percent sodium hydroxide solution is added drop by drop into the production waste liquid of the cephalosporin active ester under 0 to 80 DEG C; the pH value of the system is adjusted to be 10 to 12, and then the waste liquid is mixed fully for 0.5 to 6 hours, standing still and layering; an organic layer is decompressed to recycle an organic solvent; the solid waste slag is recrystallized directly to obtain the triphenyl phosphine oxide; the 2-mercaptobenzothiazole is extracted and obtained from water layer by a using acid neutralization method. The recycling method of the invention has the advantages of the simple operation, the high recycling rate, the good product purity, the good atom economy, etc., which effectively solves the problems existing in the prior art, such as the complicated operation, the high energy consumption, the low yield rate, the serious environment pollution, etc., thus having a wide implementary value and potential social economic benefits.

Description

(1) Technical field [0001] The invention relates to a method for recovering triphenylphosphine oxide and 2-mercaptobenzothiazole from cephalosporin active ester production waste liquid. (2) Background technology [0002] Cephalosporin active ester is an important intermediate for the preparation of cephalosporins. The main process for producing cephalosporin active ester is to prepare by reacting cephalosporin side chain acid (II) with dibenzothiazole disulfide (DM) under the action of triphenylphosphine Cephalosporin active ester (III), produces a large amount of waste liquids in the production process, and its main component is by-product triphenylphosphine oxide and 2-mercaptobenzothiazole, they all are important pharmaceutical intermediate raw materials, but because post-processing trouble , The cost of recycling is high, and many companies transfer waste to other places or discharge it directly, resulting in serious environmental pollution. Research and development of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53C07D277/72
Inventor 钟为慧吴登泽林福亮苏为科吴华悦顾士崇
Owner ZHEJIANG UNIV OF TECH
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