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Process for recovering 6-APA and salt from 6-APA mother liquor

A 6-APA, mother liquor technology, applied in the direction of alkali metal chloride, ammonium chloride, ammonium halide, etc., can solve the problems of unreported recovery, high COD, waste of resources, etc., to achieve the effect of resource utilization

Active Publication Date: 2016-07-06
INNER MONGOLIA CHANGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The 6-APA mother liquor contains a certain amount of 6-APA. If the wastewater is discharged directly, on the one hand, the COD of the discharged wastewater will be higher, and on the other hand, it will cause a waste of resources.
Although this patent reported the use of nanofiltration membrane to recover 6-APA in the mother liquor, there was no report on the recovery of the salt in the dialysate

Method used

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  • Process for recovering 6-APA and salt from 6-APA mother liquor
  • Process for recovering 6-APA and salt from 6-APA mother liquor
  • Process for recovering 6-APA and salt from 6-APA mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] RBA (the butyl acetate phase containing penicillin after activated carbon decolorization and water washing) alkalization, cracking of penicillin, extraction of lysate, crystallization of 6-APA and adjustment of pH of 6-APA mother liquor The acid is hydrochloric acid.

[0022] (1) Removal of solvent in 6-APA mother liquor

[0023] The solvent in the 6-APA mother liquor is removed by vacuum distillation, the temperature of the feed liquid is 45°C, and the vacuum degree is 0.087MPa. After removing the solvent, acetone, n-butanol, n-butyl acetate and methyl alcohol in the 6-APA mother liquor The content of isobutyl ketone was 30, 85, 96 and 5 ppm respectively.

[0024] (2) Adjustment of pH of 6-APA mother liquor

[0025] The temperature of the above-mentioned 6-APA mother liquor after solvent removal was lowered, and when the temperature dropped to 10° C., 20% ammonia water was added to the mother liquor to adjust the pH of the feed solution to 6.8.

[0026] (3) Nanofilt...

Embodiment 2

[0039] Sodium hydroxide is used in the alkalinization of RBA (the butyl acetate phase containing penicillin after activated carbon decolorization and water washing), the cracking of penicillin, the extraction of the lysate, the crystallization of 6-APA and the adjustment of the pH of the 6-APA mother liquor , the acid used is hydrochloric acid.

[0040] (1) Removal of solvent in 6-APA mother liquor

[0041] The solvent in the 6-APA mother liquor is removed by vacuum distillation, the temperature of the feed liquid is 48°C, and the vacuum degree is 0.088MPa. After removing the solvent, acetone, n-butanol, n-butyl acetate and methyl alcohol in the 6-APA mother liquor The contents of isobutyl ketone were 32, 87, 85 and 5 ppm, respectively.

[0042] (2) Adjustment of pH of 6-APA mother liquor

[0043] The temperature of the 6-APA mother liquor after removing the solvent was lowered. When the temperature dropped to 10° C., 30% sodium hydroxide solution was added to the mother liq...

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Abstract

The invention relates to a method for recovering 6-APA and salt from a 6-APA mother liquor, belongs to the technical field of pharmaceuticals. The process comprises the following steps: using a nanofiltration membrane for concentrating the 6-APA mother liquor; recovering 6-APA from a nanofiltration concentrate; recovering ammonium chloride or sodium chloride from a 6-APA nanofiltration dialyzate; meanwhile, recovering condensation water in an evaporative crystallization process. Compared with the prior art, the invention has the advantages that 6-APA and sodium chloride or ammonium chloride are recovered from the 6-APA mother liquor, steam condensation water of feed liquid is obtained while evaporating the recovered salt, the condensation water can be recycled into the workshop, to achieve the resource utilization of 6-APA mother liquor.

Description

technical field [0001] The invention relates to a method for recovering 6-APA and salts, in particular to a method for recovering 6-APA and salts from 6-APA mother liquor, and belongs to the technical field of pharmacy. Background technique [0002] The methods for preparing 6-APA include chemical cleavage and biological enzyme catalysis. The process route of chemical cracking is: under extremely low temperature conditions, first convert the carboxyl group of penicillin into silicon ester for protection, and then activate the amide on the side chain, by forming penicillin to replace imide ether derivatives, and then Under certain conditions, the selective hydrolysis gives 6-APA. The biological enzyme catalysis method uses penicillin as raw material, and under the action of penicillin acylase, penicillin is cracked into 6-APA and phenylacetic acid. 6-APA and phenylacetic acid were separated by solvent extraction, followed by crystallization, washing and drying to obtain 6-A...

Claims

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Application Information

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IPC IPC(8): C07D499/42C07D499/18C01D3/04C01C1/16
CPCC01C1/164C01D3/04C07D499/18C07D499/42
Inventor 陈顺记陈英新眭谦王继明郭建明韩贺东张冀袁照勋卜发兵
Owner INNER MONGOLIA CHANGSHENG PHARMA
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