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Method for directly recovering 7-ACA from 7-ACA crystal mother liquid

A crystallization mother liquor, 7-ACA technology, applied in the direction of organic chemistry, can solve the problems of unstable product quality, long process flow, complicated operation, etc., and achieve the effect of easy industrial application, simple process operation, and reduce environmental pollution

Active Publication Date: 2016-11-16
TIANJUSHI ENG TECH GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of long process flow, complicated operation, low yield, unstable product quality and high cost in the process of recovering 7-ACA from the crystallization mother liquor in the prior art, the present invention provides a method for reclaiming 7-ACA from the crystallization mother liquor. Method for Direct Recovery of 7-ACA

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 400ml of the mixed resin of XDA-1 resin and XDA-9 resin, wherein the volume ratio of XDA-1 resin and XDA-9 resin is 6.4:3.6, into a jacketed glass adsorption column (Ф40×500mm).

[0022] 1) Take 10L of 7-ACA crystallization mother liquor with a content of 1485mg / L and cool it down to 5°C in a 25L jacketed reactor, adjust the pH to 7.0 with ammonia water, pass through the mixed resin column, and pass through the resin at 8°C at a flow rate of 1BV / h The column has a processing capacity of 10L. After adsorption, the residual amount of 7-ACA is 0.07mg / ml.

[0023] 2) After the adsorption is completed, use 1% sodium bicarbonate aqueous solution to desorb at 5°C. The desorption volume is 650ml, and the desorption concentration is 21.38mg / ml. Filter and dry to obtain 7-ACA13.77g with a purity of 99.4%.

Embodiment 2

[0025] Put 200ml of LXT-32 resin into a jacketed glass adsorption column (Ф30×500mm).

[0026] 1) Take 6L of 7-ACA crystallization mother liquor with a content of 1517mg / L and cool it down to 7°C in a 10L jacketed reactor. ℃ through the resin column, the processing capacity is 6L, after adsorption, the residual 7-ACA content of 7-ACA is 0.09mg / ml.

[0027] 2) After the adsorption is completed, use 0.8% sodium carbonate aqueous solution to desorb at 9°C. The desorption volume is 410ml, and the desorption concentration is 20.61mg / ml. , and dried to obtain 7-ACA8.3g with a purity of 99.1%.

Embodiment 3

[0029] Put 400ml of mixed resin of LX-16 resin and LX-18 resin, wherein the volume ratio of LX-16 resin to LX-18 resin is 7:3, and put it into a jacketed glass adsorption column (Ф40×500mm).

[0030] 1) Take 10L of 7-ACA crystallization mother liquor with a content of 1485mg / L in a 25L jacketed reactor and cool it down to 8°C, adjust the pH to 6.9 with ammonia water, pass through the mixed resin column, and pass through the resin at 4.5°C at a flow rate of 1BV / h The column has a processing capacity of 10L. After adsorption, the residual amount of 7-ACA is 0.07mg / ml.

[0031] 2) After the adsorption is completed, use a mixed solution of 4.5% sodium bicarbonate aqueous solution and 4.5% sodium carbonate aqueous solution with a volume ratio of 1:1 for desorption at 8°C. The desorption volume is 650ml, and the desorption concentration is 21.41mg / ml. The liquid was cooled to 7°C, adjusted to pH 4.2 with hydrochloric acid to crystallize, filtered with suction, and dried to obtain 13...

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Abstract

The invention relates to a method for directly recovering 7-ACA from 7-ACA crystal mother liquid, and belongs to the technical field of medicines. A resin adsorption method is adopted for neutralizing the cooled crystal mother liquid, and then adsorption is directly performed through macroporous resin; concentration is performed, the absorption temperature is controlled to be 2-10 DEG C, the flow rate is controlled to be 0.2BV / h-3BV / h, and then a desorbing agent is used for desorption, wherein the desorption temperature is 2-10 DEG C; and then acidification crystallization is performed, sucking filtration is performed, and then drying is performed, so that the 7-ACA is obtained. The method disclosed by the invention can effectively reduce the production cost and the environmental pollution of the 7-ACA, green production of the 7-ACA can be realized, and the method has high economic and social benefits.

Description

technical field [0001] The invention belongs to the technical field of medicine and relates to the preparation of 7-ACA, in particular to a method for directly recovering 7-ACA from 7-ACA crystallization mother liquor. The invention has short technological process, simple operation, high yield, high purity, The product quality is stable and the cost is low. By using the method of the invention, while realizing the recovery, the purification of 7-ACA is also realized, that is, the recovery and the purification are carried out simultaneously. Background technique [0002] 7-ACA is 7-aminocephalosporanic acid, which is the most commonly used nucleus in cephalosporins and an important intermediate for semi-synthetic cephalosporin antibiotics. It can be used for semi-synthetic ceftriaxone, cefotaxime, cefazolin, cefepime and other dozens of antibiotics. It occupies a huge market because of its excellent antibacterial selectivity and safety, and occupies a very important position ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18
CPCC07D501/18
Inventor 孟祥凯陈平武亚锋刘哲封赵永杰刘金涛邢茜韩志杰甄崇礼姚振永
Owner TIANJUSHI ENG TECH GROUP
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