Method for recovering 7-ADCA mother liquor

A technology of 7-ADCA and mother liquor recovery, applied in organic chemistry and other fields, can solve problems such as waste, and achieve the effects of less pollution, increased weight yield, and low operating pressure

Active Publication Date: 2017-01-11
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the reaction is completed and 7-ADCA is extracted, the mother liquor still contains a large amount of 7-ADCA that has not been extracted, and the remaining mother liquor will be discharged directly, which will cause waste
At present, there is a lack of a method for effectively recovering 7-ADCA mother liquor with simple operation and low cost

Method used

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  • Method for recovering 7-ADCA mother liquor
  • Method for recovering 7-ADCA mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take 60L of 7-ADCA mother liquor with a concentration of 490ug / ml, and adjust the pH of the mother liquor to 6.0 with 20% aqueous sodium hydroxide solution. The temperature was controlled at 20°C, and then adsorbed by macroporous resin, the adsorption flow rate was set at 1.0BV / h, and the resin column had a capacity of 12L. Then analyze with 2% sodium bicarbonate aqueous solution at a rate of 1.0 BV / h, and control the temperature at 20°C. The analyzed feed liquid is clarified by ultrafiltration, the pressure of ultrafiltration is 4bar, and the flux is 46LMH. The mixed dialysate after ultrafiltration is then concentrated by nanofiltration. The pressure of nanofiltration is 15bar, and the flux is 20LMH. The concentrated solution was 4L, the concentration was 6.20g / L, and the yield was 84.3%. The concentrated solution was directly reused until the 7-ADCA diexpannic acid was dissolved to replace 4 L of dissolved water, and the final 7-ADCA yield increased by 0.90%.

Embodiment 2

[0040] Take 60L of 7-ADCA mother liquor with a concentration of 420ug / ml, and adjust the pH of the mother liquor to 6.2 with 30% aqueous sodium hydroxide solution. The temperature was controlled at 21°C, and then adsorbed by macroporous resin, the adsorption flow rate was set at 1.1BV / h, and the resin column capacity was 12L. Then analyze with 3% sodium bicarbonate aqueous solution at a rate of 1.2BV / h, and control the temperature at 21°C. The analyzed feed liquid is purified by ultrafiltration, the pressure of ultrafiltration is 4.2bar, and the flux is 48LMH. The mixed dialysate after ultrafiltration is then concentrated by nanofiltration. The pressure of nanofiltration is 17bar, and the flux is 22LMH. 4 L of concentrated solution was obtained, the concentration was 5.57 g / L, and the yield was 88.4%. The concentrated solution was directly reused until the 7-ADCA diexpannic acid was dissolved to replace 4 L of dissolved water, and the final 7-ADCA yield increased by 0.80%.

Embodiment 3

[0042]Take 60L of 7-ADCA mother liquor with a concentration of 410ug / ml, and adjust the pH of the mother liquor to 6.5 with 30% aqueous sodium hydroxide solution. The temperature is controlled at 22°C, and then undergoes resin adsorption, the adsorption flow rate is 1.2BV / h, and the resin column capacity is 12L. Then analyze with 4% sodium bicarbonate aqueous solution at a rate of 1.5BV / h, and control the temperature at 22°C. The analyzed feed liquid is purified by ultrafiltration, the pressure of ultrafiltration is 4.4bar, and the flux is 50LMH. The mixed dialysate after ultrafiltration is then concentrated by nanofiltration. The pressure of nanofiltration is 20bar, and the flux is 25LMH. 4 L of concentrated solution was obtained, the concentration was 5.42 g / L, and the yield was 88.1%. The concentrated solution was directly reused until the 7-ADCA diexpannic acid was dissolved to replace 4 L of dissolved water, and the final 7-ADCA yield increased by 0.78%.

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Abstract

The invention discloses a method for recovering 7-ADCA mother liquor. The method is characterized by comprising the following steps that 1, the PH value of the 7-ADCA mother liquor is regulated with alkali liquor; 2, the 7-ADCA mother liquor is adsorbed with resin and then desorbed with a desorbing agent, and desorbed liquor is obtained; 3, the desorbed liquor is subjected to ultrafiltration treatment for impurity removal and clarification, and mixed dialysate is obtained; 4, the mixed dialysate is subjected to nanofiltration concentration, and concentrated liquor is obtained; the concentrated liquor is used for replacing part of purified water and reused for dissolution of 7-ADCA 7-phenylacetamido-3-desacetoxy cephalosporanic acid. The mother liquor obtained after a reaction is subjected to adsorption, desorption, ultrafiltration and nanofiltration, and the obtained concentrated liquor is used for dissolving penicillin 7-phenylacetamido-3-desacetoxy cephalosporanic acid. The method is easy to operate, low in cost, capable of saving energy and environmentally friendly, the yield is increased, and meanwhile 7-ADCA obtained after mother liquor recovery processing is high in purity.

Description

technical field [0001] The invention belongs to the field of resource recovery and utilization in the 7-ADCA mother liquor production industry. Background technique [0002] 7-ADCA is an intermediate of oral cephalosporins, mainly used in the synthesis of cephalexin, cefadroxil, cephradine and other antibiotics. The chemical name of 7-ADCA is 7-amino-3-desacetoxycephalosporanic acid, and its chemical structure is as follows: [0003] [0004] 7-ADCA is white or off-white crystalline powder. It is mainly used as an intermediate in the semi-synthesis of important cephalosporin antibiotics, and is used in the pharmaceutical industry to synthesize cephalexin, cephradine and cefadroxil, which are used in large quantities in the market. Cephalosporin raw materials have the characteristics of broad-spectrum antibacterial, enzyme resistance, and low toxicity. [0005] The process route of chemically synthesizing 7-ADCA using penicillin as raw material is widely used in industr...

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 侯红杰王捷胡刚于凯崔克娇孔祥坦崔正月
Owner NORTH CHINA PHARMA COMPANY
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