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A method for recovering d-p-hydroxyphenylglycine in amoxicillin production waste liquid

A technology of p-hydroxyphenylglycine and amoxicillin, which is applied to the recovery of D-p-aminophenylglycine in the waste liquid of amoxicillin synthesized by enzymatic method. In the field of phenylglycine, it can solve the problems of not being able to satisfy amoxicillin manufacturers, increase the service life of the resin, increase the recycling cost, etc., and achieve the effects of low processing cost, energy consumption, environmental protection, and low energy consumption

Active Publication Date: 2016-06-22
AMICOGEN CHINA BIOPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent provides a method for reclaiming and utilizing the effective components in the mother liquor of amoxicillin, there are still deficiencies in the process, for example, adjusting the pH of the mother liquor back and forth will inevitably lead to chemically unstable 6-APA and The change of 6-APA and D-HPG, which are both amphoteric compounds, affects their reuse, and both 6-APA and D-HPG are amphoteric compounds. The amoxicillin mother liquor contains more impurities and is directly passed through the macroporous resin. The elution will inevitably lead to an increase in the remaining impurities that cannot be eluted in the pores, which will affect the service life of the resin. Secondly, the use of ultrafiltration membranes and nanofiltration membranes will also greatly increase the cost of recycling.
[0004] The mother liquor after reaction in the enzymatic amoxicillin process needs to be crystallized and post-processed to obtain the product. Not many Chinese patents focus on the recycling of amoxicillin mother liquor, which cannot meet the needs of manufacturers who produce amoxicillin by enzymatic method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The first step, resin pretreatment;

[0039]717 resin (manufactured by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30 mL, and 2 BV of 1 mol / L HCl aqueous solution was used to pass through the resin, washed with 4 to 6 BV of deionized water until the pH of the dripping solution was 8, and then 1 mol / L of HCl was used. 2BV of NaOH aqueous solution to exchange the resin into OH type, wash with 4-6BV of deionized water until the dripping solution pH=6;

[0040] LK207 resin (produced by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30mL, soaked in 2BV of absolute ethanol for 24h, and washed until the dripping liquid had no alcohol smell, passed through the resin with 1BV of 1mol / L NaOH aqueous solution, and used Wash with deionized water until the pH of the dripping solution is 7, then use 1BV of 1mol / L HCl aqueous solution to pass through the resin, and wash with 2-3BV of deionized water until the pH of the drippin...

Embodiment 2

[0048] The first step, resin pretreatment;

[0049] 717 resin (produced by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30mL, and 1mol / L HCl aqueous solution was used to pass through the resin at 2BV, washed with 4-6BV deionized water until the pH of the dripping solution was 7, and then 1mol / L HCl solution was used to 2BV of NaOH aqueous solution to exchange the resin into OH type, wash with 4-6BV of deionized water until pH=5 of the dripping solution;

[0050] LK207 resin (produced by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30mL, soaked in 2BV of absolute ethanol for 24h, and washed until the dripping liquid had no alcohol smell, passed through the resin with 1BV of 1mol / L NaOH aqueous solution, and used Wash with deionized water until the pH of the dripping solution is 7, then use 1BV of 1mol / L HCl aqueous solution to pass through the resin, and wash with 2-3BV of deionized water until the pH of the dripping s...

Embodiment 3

[0059] The first step, resin pretreatment;

[0060] 717 resin (manufactured by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30 mL, and 2 BV of 1 mol / L HCl aqueous solution was used to pass through the resin, washed with 4 to 6 BV of deionized water until the pH of the dripping solution was 8, and then 1 mol / L of HCl was used. 2BV of NaOH aqueous solution to exchange the resin into OH type, wash with 4-6BV of deionized water until pH=5 of the dripping solution;

[0061] LK207 resin (produced by Shandong Lukang Like Pharmaceutical Co., Ltd.) was packed into a column of 30mL, soaked in 2BV of absolute ethanol for 24h, and washed until the dripping liquid had no alcohol smell, passed through the resin with 1BV of 1mol / L NaOH aqueous solution, and used Wash with deionized water until the pH of the dripping solution is 7, then use 1BV of 1mol / L HCl aqueous solution to pass through the resin, and wash with 2-3BV of deionized water until the pH of the dri...

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Abstract

The invention discloses a method for recovering D-p-hydroxyphenylglycine in amoxicillin production waste liquid by use of ion exchange resin. The method comprises the following steps: firstly, exchanging D-p-hydroxyphenylglycine onto the resin by use of the ion exchange resin, dissolving D-p-hydroxyphenylglycin by use of a 0.5mol / L aqueous hydrochloric acid solution, and meanwhile, concentrating the solution; secondly, purifying the desorption solution by use of macroporous adsorption resin, and drying the dripping liquid to obtain a finished product. The method is characterized in that D-p-hydroxyphenylglycine is concentrated and purified by use of the ion exchange resin, the process is greatly simplified, the recovery effect is good, the energy is saved, the environment can be protected, and the subsequent production process of synthesizing amoxicillin by use of an enzyme method is further perfected.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to the recovery of D-p-aminophenylglycine in amoxicillin waste liquid synthesized by enzymatic method, in particular to a method of enzymatically synthesizing D-p-hydroxybenzene in amoxicillin waste liquid by resin recycling Glycine method. Background technique [0002] Usually amoxicillin synthesis methods include chemical synthesis and enzyme-catalyzed synthesis (hereinafter referred to as enzymatic method). Chemical synthesis involves too many organic solvents and relatively harsh and complicated reaction conditions, which have been gradually replaced by enzymatic synthesis of amoxicillin. At present, most domestic manufacturers have invested in enzymatic production lines. In the enzymatic synthesis of amoxicillin, in order to increase the conversion rate of the core material 6-APA, by increasing the amount of active side chain D-hydroxyphenylglycine methyl ester, D-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/36C07C227/40
Inventor 刘庆文林炳旺王玲
Owner AMICOGEN CHINA BIOPHARM CO LTD
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