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Method for recovering aminothiazoly loximate

A technology of aminothiaxamic acid and recovery method, which is applied in the field of medicine, can solve the problems of three wastes without reasonable recovery and treatment plan, high pressure on environmental protection, waste of cost, etc., and achieve considerable profits, reduce the pressure on production and environmental protection, and reduce the cost and difficulty of treatment.

Active Publication Date: 2020-08-18
SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process produces a lot of three wastes, and there is no reasonable recovery and treatment plan for the three wastes, resulting in unnecessary waste of costs and greater pressure on environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Concentration by electrodialysis: After the hydrolyzed solution (mainly composed of reverse osmosis water, mainly containing inorganic salts and unseparated aminothiaxamic acid at the end of acid adjustment) after hydrolysis of the cyclized ester is concentrated by electrodialysis equipment, concentrated liquid;

[0049] (2) Pre-decolorization: Take 1000g of the concentrated solution and add dropwise liquid alkali to adjust to pH=6.5, add 10g of activated carbon, 1g of sodium sulfite and 0.5g of EDTA for decolorization, the decolorization temperature is 34°C, and the decolorization time is 2.5h. The filtrate was added dropwise with 20wt.% chlorinated hydrochloric acid at 25°C to adjust the pH to 2.5, and suction filtered to obtain 100 g of a one-step crude product of aminothioxamic acid;

[0050](3) Anti-adjustment and decolorization: Dissolve 100g of the one-step crude product of aminothiaxamic acid in 550g of water, add liquid caustic soda dropwise for anti-adjust...

Embodiment 2

[0055] (1) Concentration by electrodialysis: After the hydrolyzed solution (mainly composed of reverse osmosis water, mainly containing inorganic salts and unseparated aminothiaxamic acid at the end of acid adjustment) after hydrolysis of the cyclized ester is concentrated by electrodialysis equipment, concentrated liquid;

[0056] (2) Pre-decolorization: Take 1100g of the concentrated solution and add dropwise liquid alkali to adjust to pH=6.8, add 13g of activated carbon, 1.3g of sodium sulfite and 0.7g of EDTA for decolorization, the decolorization temperature is 37°C, and the decolorization time is 3h. After the decolorization is completed, filter the activated carbon. The filtrate was added dropwise with 30wt.% chlorinated hydrochloric acid at 30°C to adjust the pH to 2.6, and filtered with suction to obtain 102 g of a one-step crude product of aminothioxamic acid;

[0057] (3) Anti-adjustment and decolorization: Dissolve 102g of the one-step crude product of aminothioxam...

Embodiment 3

[0062] (1) Concentration by electrodialysis: After the hydrolyzed solution (mainly composed of reverse osmosis water, mainly containing inorganic salts and unseparated aminothiaxamic acid at the end of acid adjustment) after hydrolysis of the cyclized ester is concentrated by electrodialysis equipment, concentrated liquid;

[0063] (2) Pre-decolorization: Take 2000g of the concentrated solution and add dropwise liquid alkali to adjust to pH=7.0, add 20g of activated carbon, 2g of sodium sulfite and 1g of EDTA for decolorization, the decolorization temperature is 36°C, and the decolorization time is 2.7h. After the decolorization is completed, filter the activated carbon, and the filtrate Add 25 wt.% chlorinated hydrochloric acid dropwise at 28°C to adjust the pH to 2.8, and filter with suction to obtain 203 g of a one-step crude product of aminothioxamic acid;

[0064] (3) Anti-adjustment and decolorization: Dissolve 203g of the one-step crude product of aminothiaxamic acid in...

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a method for recovering aminothiazoly loximate. Hydrolysate generated in the aminothiazoly loximate production process is subjected to electrodialysis concentration to obtain a concentrated solution, the concentrated solution is pre-decolorized to obtain an aminothiazoly loximate one-step crude product, the aminothiazoly loximate one-step crude product is subjected to reverse adjustment decolorization to obtain an aminothiazoly loximate two-step crude product, and the aminothiazoly loximate two-step crude product is refined to obtain an aminothiazoly loximate finished product. The reverse-regulation decolorization comprises the following steps: dissolving the aminothiazoly loximate one-step crude product in water, dropwise adding liquid caustic soda to perform reverse-regulation, dissolved clarification, and decolorizing to obtain an aminothiazoly loximate two-step crude product. According to the method, qualified aminothiazoly loximate product can be recycled, the wastewater treatment amount is reduced, the process is efficient, simple, environmentally friendly and high in profit, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for recovering aminothiaxamic acid. Background technique [0002] Amthioxamic acid is mainly used in the synthesis of third-generation and fourth-generation cephalosporins. It has good medicinal curative effect and little side effects on humans. It has broad application prospects and high added value. [0003] At present, most of the continuous industrial production processes for the preparation of aminothioxamic acid intermediates are relatively stable, using oximation, alkylation, chlorination, cyclization, and hydrolysis processes. The liquid will contain some products, which are generally treated according to the three wastes. [0004] Chinese patent CN 103012312 A discloses a method for recycling waste water from the production of aminothiaxamic acid, which converts oximation and methylation into a one-step reaction. The steps are: oximation and methyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/593
CPCC07D277/593
Inventor 王瑞阴华栋李佳刘承鑫张增佳
Owner SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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