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Method for recycling mother liquid of cefalexin synthesized by enzymatic method

A technology of cephalexin mother liquor and enzymatic synthesis, which is applied in the field of resource recycling in the cephalexin mother liquor production industry, to achieve the effects of reducing costs, avoiding decomposition reactions, and saving energy

Active Publication Date: 2016-12-14
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, lack a kind of simple to operate, with low cost, the method for the effective reclaiming cephalexin mother liquor of environmental protection

Method used

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  • Method for recycling mother liquid of cefalexin synthesized by enzymatic method

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Experimental program
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Effect test

Embodiment 1

[0035] Take 2.6L of cephalexin mother liquor, adjust the pH to 2.52 with 25% sulfuric acid, and control the temperature at 21°C. Then, after resin adsorption, the adsorption flow rate is 1.5BV / h, the resin column capacity is 500mL, and a total of 2600mL is adsorbed, about 39g of cephalexin. After washing the resin column with 1BV of water, analyze it with 20% ethanol solution with pH=1.0 at a rate of 1BV / h, control the temperature at 21°C, and collect 0.75BV. Adjust the pH of 0.75 BV of the collected analytical solution (total 375 mL) with 15% ammonia water to crystal out, and grow the crystal for 30 minutes. Continue to add 15% ammonia water dropwise to pH=4.50, stop the dropwise addition, lower the temperature to 9.5° C., and grow the crystal for 30 minutes. Vacuum suction filtration, at a temperature of 40 ° C, dried for 2 hours to obtain cephalexin 38.0g, the recovery rate of cephalexin was 97.4%, (remarks: 1BV refers to 1 times the resin column volume) was detected by hi...

Embodiment 2

[0038] Take 2.6L of cephalexin mother liquor, adjust the pH to 2.60 with 25% sulfuric acid, and control the temperature at 21°C. Then, after resin adsorption, the adsorption flow rate is 1.5BV / h, the resin column capacity is 500mL, and a total of 2600mL is adsorbed, about 39g of cephalexin. After the resin column was washed with 1BV of water, it was analyzed with 20% ethanol solution with pH=1.0 at a rate of 1BV / h, and the temperature was controlled at 20°C. Collect 0.75BV to end. Adjust the pH of 0.75 BV of the collected analytical solution (total 375 mL) with 15% ammonia water to crystal out, and grow the crystal for 30 minutes. Continue to add 15% ammonia water dropwise to pH=4.50, stop the dropwise addition, lower the temperature to 8.5° C., and grow the crystal for 30 minutes. Vacuum suction filtration, at temperature 40 ℃, dry 2 hours, obtain cephalexin 37.8g, cephalexin recovery rate 96.9%, (1BV refers to the resin column volume of 1 times) through HPLC detection, cep...

Embodiment 3

[0041]Take 2.6L of cephalexin mother liquor, adjust the pH to 2.55 with 25% sulfuric acid, and control the temperature at 22°C. Then, after resin adsorption, the adsorption flow rate is 1.5BV / h, the resin column capacity is 500mL, and a total of 2600mL is adsorbed, about 39g of cephalexin. After washing the resin column with 1BV of water, analyze it with 20% ethanol solution with pH=1.0 at a rate of 1BV / h, control the temperature at 21°C, and collect 0.75BV. Adjust the pH of 0.75 BV of the collected analytical solution (total 375 mL) with 15% ammonia water to crystal out, and grow the crystal for 30 minutes. Continue to add 15% ammonia water dropwise to pH=4.50, stop the dropwise addition, lower the temperature to 9.0° C., and grow the crystal for 30 minutes. Vacuum suction filtration, at temperature 40 ℃, dry 2 hours, obtain cephalexin 38.0g, cephalexin recovery rate 97.4%, (remark: 1BV refers to the resin column volume of 1 times) detects through high-performance liquid chr...

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Abstract

The invention discloses a method for recycling mother liquid of cefalexin synthesized by an enzymatic method. The method provided by the invention comprises the following steps: 1) adjusting the pH value of the mother liquid of the cefalexin to 2.0 to 3.0 by using acid liquid at a certain temperature; 2) adsorbing, washing and desorbing the mother liquid to obtain a desorbed solution; 3) crystallizing the desorbed solution by ammonia water, filtering, washing and drying to obtain the finished product of the cefalexin; 4) distilling the filtrate in the step 3) under reduced pressure; 5) recycling ethanol obtained by distillation and the mother liquid after distillation for preparation of a desorbing agent next time and dissolution of 7-ADCA before synthesis. The preparation method provided by the invention is simple to operate, low in cost, energy-saving and environmentally friendly; meanwhile, the yield of the cefalexin prepared by the method is higher than that of the cefalexin prepared by a method without recycling the mother liquid.

Description

technical field [0001] The invention relates to a method for recycling cephalexin mother liquor, and belongs to the field of resource recycling in the cephalexin mother liquor production industry. Background technique [0002] Enzymatic production of cephalexin is the most economical method with simple process and convenient operation. The synthesis route of the method is as follows: 7-ADCA is synthesized by enzymes and phthalic anhydride methyl ester salt to form cephalexin, and then crystallized with ammonia water to obtain the product cephalexin. [0003] After the reaction is completed, after the cephalexin is extracted, a large amount of cephalexin is not extracted in the mother liquor. The conventional method is to add a certain amount of β-naphthol in the mother liquor to form a double salt with the cephalexin, and the compound The salt crystals are filtered out, dissolved again, and the cephalexin is extracted with dichloromethane. After crystallization, it is inser...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22
CPCC07D501/22
Inventor 侯红杰刘崧杨晓斌杨梦德王明波
Owner NORTH CHINA PHARMA COMPANY
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