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A kind of cephalexin crystallization mother liquor recovery method

A recovery method, the technology of cephalexin, which is applied in the fields of chemical industry and medicine, can solve the problems of low product purity, high cost, and low yield, and achieve the effects of high product purity and yield, efficient recovery, and low cost

Active Publication Date: 2022-03-15
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the pyrolysis, the feed solution did not effectively remove phenylglycine. In the process of adjusting the pH to 3-5, phenylglycine was co-crystallized and precipitated with 7-aminodesacetoxycephalosporanic acid, resulting in low product purity.
[0011] Therefore, the existing cephalexin crystallization mother liquor treatment methods all fail to effectively remove the phenylglycine in the crystallization mother liquor or lysate at first, and there are problems such as large pollution, high cost, low yield, and low product purity.

Method used

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  • A kind of cephalexin crystallization mother liquor recovery method
  • A kind of cephalexin crystallization mother liquor recovery method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Under stirring at 25°C, add ammonia solution to 1L of cephalexin crystallization mother liquor, keep the pH value at 7.65, add 90 g of penicillin G acylase, carry out the cleavage reaction of cephalexin for 15 minutes to obtain a lysate, and filter the lyse with suction Afterwards, 980 mL of lysed liquid was obtained, and the conversion rate of cephalexin was 99.4%;

[0042] (2) Under stirring, add sulfuric acid to the lysed liquid obtained in step (1), adjust the pH to 6.7, and cool to 5°C at a cooling rate of 5°C / h to precipitate the phenylglycine in the lysed liquid Precipitated, obtained 960mL clear liquid and phenylglycine solid after suction filtration;

[0043] (3) Under stirring, add sulfuric acid to the clear liquid separated in step (2) at a rate of 14.4mL / h, adjust the pH value to 3.9, and heat up to 30°C, then perform suction filtration, wash and dry, The 7-aminodesacetoxycephalosporanic acid product was obtained.

[0044] The results show that based o...

Embodiment 2

[0046] (1) Under stirring at 40° C. and 300 rpm, sodium hydroxide solution is added to 1 L of cephalexin crystallization mother liquor, and the pH value is maintained at 8.0, 70 g of penicillin G acylase is added, and the cleavage reaction of cephalexin is carried out for 20 minutes to obtain a lysate. After the lysate was centrifuged, 990 mL of the lysate clear liquid was obtained, and the conversion rate of cephalexin was 99.5%;

[0047] (2) Under the action of stirring at 300rpm, hydrochloric acid is added to the lysed clear liquid obtained in step (1), the pH value is adjusted to 6.5, and cooled to 10° C. at a cooling rate of 10° C. / h to make the benzene in the lysed clear liquid Glycine was precipitated, and after centrifugation, 970 mL of clear liquid and phenylglycine solid were obtained;

[0048] (3) Under 300rpm stirring, add hydrochloric acid to the clear liquid separated in step (2) at a rate of 20mL / h, adjust the pH value to 3.7, and heat up to 35°C, then centrifug...

Embodiment 3

[0051] (1) Under stirring at 15°C and 220rpm, potassium hydroxide solution was added to 1L of cephalexin crystallization mother liquor, and the pH value was maintained at 7.8, 60 g of penicillin G acylase was added, and the cleavage reaction of cephalexin was carried out for 45 minutes to obtain a lysate. After the lysate was filtered under normal pressure, 995 mL of the lysed clear liquid was obtained, and the conversion rate of cephalexin was 99.1%;

[0052] (2) Under the action of stirring at 220rpm, phosphoric acid is added to the lysed clear liquid obtained in step (1), the pH value is adjusted to 7, and cooled to 7° C. at a cooling rate of 4° C. / h, so that the benzene in the lysed clear liquid is Glycine was precipitated out, and 975mL of clear liquid and phenylglycine solid were obtained after normal pressure filtration;

[0053] (3) Under the action of stirring at 220rpm, add phosphoric acid to the clear liquid separated in step (2) at a rate of 30mL / h, adjust the pH v...

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Abstract

The invention discloses a method for recovering cephalexin crystallization mother liquor. Under stirring at 15-40°C, an alkaline regulator is added to the cephalexin crystallization mother liquor to maintain a pH value of 7-8, and a lyase is added to carry out cephalexin cleavage reaction and solid-liquid separation , add the acid regulator to the clear liquid, adjust the pH value to 6-7, and lower the temperature to 5-10°C to precipitate the phenylglycine, separate the solid and liquid, add the acidic regulator to the clear liquid, adjust the pH value to 3-4 and heated up to 20-40°C to obtain 7-aminodesacetoxycephalosporanic acid crystalline product. In the present invention, the phenylglycine in the lysate is preferentially crystallized and separated by cooling and crystallization, the purity of which is >99%, and the yield is about 5%, and the purity of the obtained 7-aminodesacetoxycephalosporanic acid is >99%, and the recovery rate is 90%. above. The invention does not introduce water and VOC substances, has no pollution to the environment, realizes the clean recovery of crystallization mother liquor, and has high separation and recovery efficiency.

Description

technical field [0001] The invention belongs to the technical fields of medicine and chemical industry, and in particular relates to a method for recovering cephalexin crystallization mother liquor. Background technique [0002] The molecular formula of cephalexin is C 16 h 17 N 3 o 4 S, 7-aminodesacetoxy cephalosporanic acid (abbreviated 7-ADCA) is an important intermediate for the synthesis of cephalexin, and its molecular formula is C 8 h 10 N 2 o 3 S, whose structure is: [0003] [0004] Due to the large environmental pollution caused by chemical methods, the current pharmaceutical production of cephalexin mainly adopts enzymatic synthesis and crystallization, separation and purification, using water as a solvent, without using organic solvents, and the process is green and environmentally friendly. After separation and purification of cephalexin crystallization, the crystallization mother liquor mainly contains about 12-15g / L cephalexin, 1-4g / L 7-aminodesace...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/12C07D501/18C07C227/40C07C229/36C12P13/04C12P35/02
CPCC07D501/12C07D501/18C07C227/40C12P13/04C12P35/02C07C229/36
Inventor 侯宝红尚泽仁张军立龚俊波段志钢吴送姑胡卫国李中华王新辉藏飞
Owner TIANJIN UNIV
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