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Method for recovering 7-aminocephalosporanic acid (7-ACA) from 7-ACA mother liquor

A technology of aminocephalosporanic acid and mother liquor, which is applied in the field of medicine, can solve the problems of cumbersome steps and high cost, and achieve the effects of simple process, low cost and high yield

Active Publication Date: 2015-03-11
华北制药河北莱欣药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned 7-ACA recovery process has the disadvantages of cumbersome steps, high cost, etc.
[0006] At present, there is a lack of a simple, low-cost method for effectively reclaiming the 7-ACA mother liquor

Method used

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  • Method for recovering 7-aminocephalosporanic acid (7-ACA) from 7-ACA mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take 10L of 7-ACA mother liquor (7-ACA content 1300μg / mL), adjust the pH to 7.0 with 3mol / L ammonia water, concentrate by nanofiltration 4 times; Science and Technology New Materials Technology Co., Ltd.) adsorption, the adsorption flow rate is 2BV / h (1BV refers to 1 times the resin column volume), the resin column capacity is 500mL, and a total of 12.82g is adsorbed. 3% sodium bicarbonate aqueous solution is used at 0.5BV / h speed analysis. Start collecting at 0.75BV and stop at 2.25BV. Adjust the pH of the collected analytical solution 0.75-2.25BV (total 750mL) with 10% hydrochloric acid to produce crystals, grow the crystals for 30 minutes, filter through a suction filter bottle, wash with 50ml×2 purified water, and then wash with 50ml×2 acetone . Suction filtration for 30 minutes, put into a vacuum drying oven and dry at 40° C. for 2 hours to obtain 8.02 g of 7-ACA product, which was detected by HPLC with a content of 99.10%.

Embodiment 2

[0024] Take 10 L of 7-ACA mother liquor (7-ACA content 1350 μg / mL), and adjust the pH to 7.0 with 3 mol / L ammonia water. Concentrate 4.5 times by nanofiltration, control the temperature at 5-10°C, and adsorb through LXT-032 resin (adsorption flow rate 2BV / h). The speed analysis of h starts to collect from 0.75BV and stops at 2.25BV. Adjust the pH of the collected analytical solution 0.75-2.25BV (total 750mL) with 10% hydrochloric acid until the crystals appear, grow the crystals for 30 minutes, continue to add 10% hydrochloric acid to pH=5.00, stop the dripping, and the temperature drops below 5°C. Cultivate the crystal for 30 minutes. After filtering through a suction filter flask, wash with 50ml×2 purified water, and then wash with 50ml×2 acetone. Suction filtration for 30 minutes, put into a vacuum drying oven and dry at 40° C. for 2 hours to obtain 8.12 g of 7-ACA product, which was detected by HPLC with a content of 99.00%.

Embodiment 3

[0026] Take 10 L of 7-ACA mother liquor (7-ACA content 1400 μg / mL), and adjust the pH to 7.0 with 3 mol / L ammonia water. Concentrate 5 times by nanofiltration, control the temperature at 5-10°C, and adsorb it through LXT-032 resin (adsorption flow rate 2BV / h). The speed analysis of h starts to collect from 0.75BV and stops at 2.25BV. Adjust the pH of the collected analytical solution 0.75-2.25BV (total 750mL) with 10% hydrochloric acid until the crystals appear, grow the crystals for 30 minutes, continue to add 10% hydrochloric acid to pH=5.00, stop the dripping, and the temperature drops below 5°C. Cultivate the crystal for 30 minutes. After filtering through a suction filter flask, wash with 50ml×2 purified water, and then wash with 50ml×2 acetone. Suction filtration for 30 minutes, put into a vacuum drying oven and dry at 40° C. for 2 hours to obtain 8.04 g of 7-ACA product, which was detected by HPLC with a content of 99.13%.

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Abstract

The invention discloses a method for recovering 7-aminocephalosporanic acid (7-ACA) from 7-ACA mother liquor. The method comprises the following steps of a, adjusting a pH value of a 7-ACA mother liquor to 7 by alkali and carrying out condensation treatment at concentration multiple of 4-5, b, controlling a temperature in a range of 5-10 DEG C, adsorbing the concentrated 7-ACA mother liquor by LXT-032 resin, and carrying out resolving by a resolving agent, c, adding acid into the material liquid subjected to resolving and carrying out crystallization, and d, filtering the crystals, and carrying out washing and drying to obtain a 7-ACA finished product. The method for recovering 7-ACA has the advantages of simple processes, low cost, energy saving, environmental protection, high 7-ACA product yield and high purity.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for recovering 7-aminocephalosporanic acid from 7-aminocephalosporanic acid mother liquor. Background technique [0002] 7-Aminocephalosporanic acid (abbreviated as 7-ACA) is an important intermediate for the production of semi-synthetic cephalosporins such as cefotaxime, cefuroxime, cefoperazone, ceftriaxone, cefazolin, and cefepime. as follows: [0003] [0004] At present, the production methods of 7-ACA mainly include chemical methods and enzymatic methods. Enzymatic production of 7-ACA has a simple process and convenient operation, and is currently the most commonly used method. When 7-ACA is produced by enzymatic method, after the 7-ACA crystals in the reaction liquid are separated by solid-liquid separation equipment, part of 7-ACA still remains in the remaining 7-ACA mother liquor. Direct discharge of the mother liquor with residual 7-ACA not only causes w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18C07D501/12
CPCC07D501/12C07D501/18
Inventor 侯红杰韦卫军王梦谭程俊山胡斌李建强王刚于佩恩
Owner 华北制药河北莱欣药业有限公司
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