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Crystallization method of cephalosporins

A technology for antibiotics and cephalosporins, which is applied in the industrial production process of cephalosporins antibiotics. It can solve the problems of unfavorable quality and efficiency of downstream preparations, unsatisfactory crystal morphology, and uneven crystal particle size distribution, so as to improve equipment utilization and product yield. , Improve equipment utilization, good fluidity effect

Active Publication Date: 2018-01-19
NORTH CHINA PHARMA COMPANY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The crystallization process in the cephalosporin antibiotic production method usually adopts batch method crystallization, as the crystallization method in the cephalexin production process disclosed in patent document CN103805671B and patent document CN102656274B is all batch method crystallization, includes static crystal growth step in the batch method crystallization process, However, it is easy to cause secondary nucleation, uneven crystal size distribution, unsatisfactory crystal morphology (imperfect crystal habit), low separation efficiency, low bulk density, and poor fluidity, which are not conducive to the quality and efficiency of downstream preparations

Method used

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  • Crystallization method of cephalosporins
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  • Crystallization method of cephalosporins

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Embodiment 1

[0043] Embodiment 1 is substantially the same as the steps of the above-mentioned specific examples, and different process parameters and conditions are as follows:

[0044] A crystallization method of cephalexin, the crystallization process is carried out continuously in 2 crystallization kettles, the crystallization reaction is first carried out in the primary crystallization kettle, and then introduced into the secondary crystallization kettle, the volume ratio of the primary crystallization kettle to the secondary crystallization kettle It is 1:2.

[0045] Specific steps are as follows:

[0046] A. Add water to the primary crystallization kettle, keep stirring and control the crystallization temperature at 25°C, add seed crystals, the mass ratio of water and seed crystals is 8:1, and add raw materials and ammonia water at the same time, so that the pH is controlled at 2.9; The raw material is obtained by dissolving the enzyme with 15% dilute sulfuric acid after separating...

Embodiment 2

[0050] The steps of embodiment 2 are substantially the same as embodiment 1, and different process parameters and conditions are as follows:

[0051] A crystallization method of cephalexin, the crystallization process is carried out continuously in two crystallization kettles, and the volume ratio of the primary crystallization kettle and the secondary crystallization kettle is 1:5.

[0052] Specific steps are as follows:

[0053] A. The crystallization temperature in the primary crystallization kettle is at 45°C, and the pH is controlled at 4.0; the mass ratio of adding water and seed crystals is 80:1, and the raw material is cephalosporin crude product slurry separation enzyme, and then use 20% dilute sulfuric acid Dissolved, the concentration is 200mg / ml. The flow rate of feedstock was 4000 L / h.

[0054] When the volume of the feed liquid in the primary crystallization kettle reaches 4 / 5 of the total volume, start to introduce the feed liquid in the primary crystallizatio...

Embodiment 3

[0057] The steps of embodiment 3 are substantially the same as embodiment 1, and different process parameters and conditions are as follows:

[0058] A crystallization method of cephalexin, the crystallization process is carried out continuously in two crystallization kettles, the volume ratio of the primary crystallization kettle and the secondary crystallization kettle is 1:3.

[0059] Specific steps are as follows:

[0060] A. The crystallization temperature in the primary crystallization kettle is at 35°C, and the pH is controlled at 3.5; the mass ratio of adding water and seed crystals is 50:1, and the raw material is 18% dilute sulfuric acid after the cephalosporin crude product slurry is separated from the enzyme Dissolved, the concentration is 140mg / ml. The flow rate of feedstock was 2500 L / h.

[0061] When the volume of the feed liquid in the primary crystallization tank reaches 70% of the total volume, start to import the feed liquid in the primary crystallization ...

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Abstract

Belonging to the field of industrial production technologies of beta-lactam antibiotics, the invention discloses a crystallization method of cephalosporins. The method is carried out in 2-4 crystallization kettles continuously. The method has the advantages of high continuation degree, simple operation and high production efficiency, and is suitable for large-scale industrialized production, improves equipment utilization rate and product yield, and the obtained cephalosporins finished product has an ideal short rod-like crystal form, and the crystals have the characteristics of good integrity, uniform granularity, high purity, good fluidity, and convenient separation, drying and packaging.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a crystallization method of β-lactam antibiotics, and belongs to the field of industrial production technology of cephalosporin antibiotics. Background technique [0002] Cephalosporin antibiotics are a class of semi-synthetic β-lactam antibiotics, which have broad-spectrum antibacterial effects and have antibacterial effects on both Gram-positive and Gram-negative bacteria. The content expands until it bursts and dissolves, thereby achieving the bactericidal effect. [0003] At present, the production method of cephalosporin antibiotics has been improved from the original chemical method to the enzymatic method. Compared with the traditional chemical method, enzymatic synthesis has obvious advantages in terms of cost reduction, process simplification, and environmental friendliness. The enzymatic synthesis process has been widely described in patent literature. Under the ca...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/12
Inventor 张军立龚俊波段志钢张锁庆王明波穆军明林兰兰刘倩张德江王新辉曹欢臧飞崔克娇段素英赵彬李小瑞宋斌
Owner NORTH CHINA PHARMA COMPANY
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