Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for recovering D-p-hydroxyphenylglycine from D-p-hydroxyphenylglycine crystallization mother liquor synthesized by an enzymic method

A p-hydroxyphenylglycine, recovery method technology, applied in the direction of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor product purity, low concentration multiple, high energy consumption, etc., and meet high assembly requirements , the effect of guaranteed yield

Active Publication Date: 2020-07-10
SHANXI WEIQIDA PHARMA IND
View PDF8 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method directly concentrates the mother liquor hydrolyzate by nanofiltration, which not only consumes a lot of energy and has a low concentration ratio, but also contains complex components in the mother liquor after concentration. The recovery of 6-APA and D-p-hydroxyphenylglycine by this method is inefficient and the purity of the product is poor. , for example according to its examples, the purity of D-p-hydroxyphenylglycine is about 95%

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Reclaim enzymatic synthesis of D-p-hydroxyphenylglycine in the mother liquor of D-p-hydroxyphenylglycine crystallization according to the following steps:

[0037] (1) Adsorption of D-p-hydroxyphenylglycine by macroporous adsorption resin

[0038] Resin activation: macroporous adsorption resin (LXT-053 resin from Xi'an Lanxiao Technology Co., Ltd.) soaked in methanol for 5 hours, filtered, and then rinsed with purified water to clean the resin surface, and then wet-packed, cylindrical column bed , the resin loading capacity is 900mL, and the aspect ratio is 8;

[0039] D-hydroxyphenylglycine adsorption: take 50L of D-hydroxyphenylglycine crystallization mother liquor, wherein the concentration of D-hydroxyphenylglycine is 23.54g / L, the conductivity is 118ms / cm, and the pH value is 4.9; use 20wt% hydrochloric acid The solution adjusts the pH of the mother liquor to 2±0.2, and then passes through the cylindrical resin column bed prepared above at a flow rate of 35L per h...

Embodiment 2

[0049] Reclaim enzymatic synthesis of D-p-hydroxyphenylglycine in the mother liquor of D-p-hydroxyphenylglycine crystallization according to the following steps:

[0050] (1) Adsorption of D-p-hydroxyphenylglycine by macroporous adsorption resin

[0051] Resin activation: macroporous adsorption resin (LXT-053 resin from Xi'an Lanxiao Technology Co., Ltd.) soaked in methanol for 5 hours, filtered, and then rinsed with purified water to clean the resin surface, and then wet-packed, cylindrical column bed , the resin loading capacity is 900mL, and the aspect ratio is 8;

[0052] D-hydroxyphenylglycine adsorption: Take 50L of D-p-hydroxyphenylglycine crystallization mother liquor, wherein the concentration of D-hydroxyphenylglycine is 26.37g / L, the conductivity is 118ms / cm, and the pH value is 5.1; use 20wt% hydrochloric acid The solution adjusts the pH of the mother liquor to 2±0.2, and then passes through the cylindrical resin column bed prepared above at a flow rate of 34L per...

Embodiment 3

[0061] Embodiment 3 (pilot test)

[0062] Reclaim enzymatic synthesis of D-p-hydroxyphenylglycine in the mother liquor of D-p-hydroxyphenylglycine crystallization according to the following steps:

[0063] (1) Adsorption of D-p-hydroxyphenylglycine by macroporous adsorption resin

[0064] Resin activation: macroporous adsorption resin (LXT-053 resin from Xi'an Lanxiao Technology Co., Ltd.) soaked in methanol for 5 hours, filtered, and then rinsed with purified water to clean the resin surface, and then wet-packed, cylindrical column bed , the resin loading capacity is 36L, and the aspect ratio is 8;

[0065] D-hydroxyphenylglycine adsorption: Take 2000L of D-hydroxyphenylglycine crystallization mother liquor, wherein the concentration of D-hydroxyphenylglycine is 21.92g / L, the conductivity is 119.5ms / cm, and the pH value is 5.1; use 20wt% Hydrochloric acid solution adjusts the pH of the mother liquor to 2±0.2, then passes through the above-mentioned cylindrical resin column ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
concentrationaaaaaaaaaa
particle sizeaaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for recovering D-p-hydroxyphenylglycine from D-p-hydroxyphenylglycine crystallization mother liquor synthesized by an enzymic method. The method comprises the following steps: (1) adsorbing D-p-hydroxyphenylglycine by adopting macroporous adsorption resin; (2) resolving the D-p-hydroxyphenylglycine from the resin; (3) recovering ammonium chloride from the residualliquid; and (4) crystallizing the D-p-hydroxyphenylglycine. The method is simple and convenient in process design, high in operability, good in recovery effect and excellent in product quality, the purity of the recovered D-p-hydroxyphenylglycine is 99.2% or above, and meanwhile, ammonium chloride is recovered.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a method for recovering D-p-hydroxyphenylglycine in an enzymatic synthesis of D-p-hydroxyphenylglycine crystallization mother liquor. Background technique [0002] D-hydroxyphenylglycine (p-hydroxylphenylglycine), chemical name D-α-amino p-hydroxyphenylacetic acid (referred to as D acid, D-HPG), molecular formula (OH)C 6 h 4 CH(NH 2 ) COOH, molecular weight 167.2. D-p-Hydroxyphenylglycine is a white flaky crystal with a melting point of 240°C (decomposition), slightly soluble in water and methanol, and easily soluble in acid or alkali solutions to form salts. D-HPG is an important pharmaceutical intermediate for the synthesis of β-lactam semi-synthetic broad-spectrum antibiotics, mainly used in the synthesis of penicillins and cephalosporins, such as: amoxicillin, cefadroxil, cefoperazone, cefpiramide, etc. [0003] The production process of D acid is that p-hydroxyphenylhydan...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36C07C227/40C07C227/42C01C1/16
CPCC07C227/40C07C227/42C01C1/164C07B2200/07C07C229/36
Inventor 齐宝亮杨波幸华龙刁夏任广宏葛小波刘国
Owner SHANXI WEIQIDA PHARMA IND