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Method for treating L-p-hydroxyphenylglycine desalting mother liquor by adopting bipolar membrane electrodialysis technology

A L-p-hydroxyphenylglycine and bipolar membrane technology, which is applied in the field of treatment technology of chemical and pharmaceutical production waste liquid, can solve the problems of not taking into account the problem of membrane fouling, reducing the service life of membrane, membrane fouling, etc., so as to improve the quality, The effect of reducing pollution and reducing environmental pollution

Inactive Publication Date: 2011-02-09
石药集团中诺药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There has been a literature report (searched from the Internet, the medical community, the chemical drug pharmaceutical forum, published on March 15, 2010) "Research on the process conditions of converting p-toluenesulfonic acid sodium salt by bipolar membrane electrodialysis ", the method used in the report did not take into account the fouling of the membrane, but simply considered the Na in the idealized sodium p-toluenesulfonate solution. + removal, and in the actual production process, the Fe in the mother liquor 3+ , Ca 2+ , Mg 2+ It will cause great pollution to the membrane and reduce the service life of the membrane

Method used

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Embodiment 1

[0013] Embodiment 1: adopt bipolar membrane electrodialysis technology of the present invention to process the method for L-p-hydroxyphenylglycine desalination mother liquor, it comprises the following steps:

[0014] ①Pretreatment process of the desalted mother liquor: firstly dilute the desalted mother liquor by 0.5 times with pure water, because as the separation time changes, the total volume in the salt chamber (acid chamber) in the bipolar membrane device will decrease, forming a solution Crystals are precipitated in a supersaturated state, so the desalted mother liquor must be diluted. Use NaOH to adjust the pH value to 11, then heat to 60°C, filter, and use an atomic absorption spectrophotometer to measure the desalted mother liquor diluted 0.5 times. After this step, Fe 3+ Concentration was reduced to 3.389mg / kg from 12.12mg / kg before treatment, then the filtrate was carried out Ca 2+ Ions, Mg 2+ With the removal of ions, the total amount (sum) of calcium and magnes...

Embodiment 2

[0015] Embodiment 2: the method of adopting bipolar membrane electrodialysis technology of the present invention to process L-p-hydroxyphenylglycine desalination mother liquor, it comprises the following steps: 1. the pretreatment process of desalination mother liquor: first measure desalination mother liquor 600mL, add pure water 900mL (diluted 1.5 times), then adjust the pH value of the desalted mother liquor to 11 with NaOH, heat to 60°C (or 65°C), filter, and then pass the filtrate through the column to remove Ca in the mother liquor 2+ and Mg 2+ . ②Bipolar membrane electrodialysis separation process: adopt the two-chamber method to recover p-toluenesulfonic acid in the mother liquor, add the treated desalted mother liquor to the salt chamber (acid chamber), add 500mL of pure water to the alkali chamber, and then drop Add 1g (or 1.5g) of NaOH solution with a weight percentage concentration of 30%, to reduce the energy consumption in the initial stage of separation, turn o...

Embodiment 3

[0016] Embodiment 3: the method of adopting bipolar membrane electrodialysis technology of the present invention to process L-p-hydroxyphenylglycine desalination mother liquor, it comprises the following steps: 1. the pretreatment process of desalination mother liquor: first measure desalination mother liquor 600mL, add pure water 300mL (diluted 0.5 times), then adjust the pH value of the desalted mother liquor to 12 with NaOH, heat to 60 ° C, filter, and then pass the filtrate through the column to remove Ca in the mother liquor 2+ and Mg 2+ . ②Bipolar membrane electrodialysis separation process: adopt the two-chamber method to recover p-toluenesulfonic acid in the mother liquor, add the treated desalted mother liquor to the salt chamber (acid chamber), add 500mL of pure water to the alkali chamber, and then drop Add 1g (or 1.2g) of NaOH solution with a weight percentage concentration of 30%, to reduce the energy consumption in the initial stage of separation, turn on the pu...

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Abstract

The invention discloses a method for treating an L-p-hydroxyphenylglycine desalting mother liquor by adopting a bipolar membrane electrodialysis technology, comprising the following steps of diluting the desalting mother liquor, regulating a pH value thereof to be alkaline, heating, filtering, and using cation exchange resin to remove inpurity ions in the mother liquor; separating the mother liquor after impurity ion removal by adopting bipolar membrane electrodialysis to respectively obtain liquid alkali and a resolution agent; secondly using the obtained liquid alkali in alkali regulation or an activation treatment process of cation exchange resin in the last step, and using the obtained resolution agent for production of L-p-hydroxyphenylglycine again. Therefore, various components reach closed cycle without causing material loss. The method is beneficial to recovering valuable substances in the mother liquor, lowers the environmental pollution and also avoids introduction of new impurities, thereby improving the quality of a product.

Description

technical field [0001] The invention relates to a method for recycling waste liquid in the production of p-hydroxyphenylglycine, which belongs to the treatment process of waste liquid in chemical and pharmaceutical production. In particular, a method for treating L-p-hydroxyphenylglycine desalination mother liquor by adopting bipolar membrane electrodialysis technology. Background technique [0002] L-p-Hydroxyphenylglycine is a white or off-white crystalline powder, slightly soluble in water, easily soluble in acid or alkali solution. As an important pharmaceutical intermediate, it is an important production process for the synthesis of semi-synthetic penicillins, cephalosporins and β-lactam semi-synthetic antibiotics. It is also an important raw material for the manufacture of amoxicillin. etc. main side chains. The basic process of producing L-p-hydroxyphenylglycine is to dissolve the racemic mixture of p-hydroxyphenylglycine with p-toluenesulfonic acid to obtain p-hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36B01D61/48C07C227/40
CPCY02A20/124
Inventor 张士文李凯王景娜
Owner 石药集团中诺药业(石家庄)有限公司
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