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Extraction and recovery method of p-hydroxyphenylglycine

A technology of p-hydroxyphenylglycine and hydroxyphenylglycine parent, which is applied in the field of extraction and recovery of p-hydroxyphenylglycine, can solve the problems of high cost of membrane material regeneration and reuse, unreported extraction, complicated operation process, etc., and achieves equipment income. Less, improve economy, simple operation steps

Active Publication Date: 2021-10-12
HENAN UNIVERSITY
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Problems solved by technology

However, this process is also for high-concentration p-hydroxyphenylglycine mother liquor, and the process uses a three-stage membrane separation device, the operation process is complicated, and the regeneration and reuse of membrane materials are expensive.
[0006] In addition, up to now, there is no report about the extraction of p-hydroxyphenylglycine in the low-concentration p-hydroxyphenylglycine mother liquor

Method used

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  • Extraction and recovery method of p-hydroxyphenylglycine

Examples

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Effect test

Embodiment 1

[0026] This example is aimed at the extraction of p-hydroxyphenylglycine in low-concentration p-hydroxyphenylglycine mother liquor, wherein the mass percentage of p-hydroxyphenylglycine is 5.0 wt%; the mass percentage of ammonium sulfate is about 39.1 wt%. The extraction steps are as follows:

[0027] (1) Precipitation and filtration stage: First, weigh 358.1 g of BaCl 2 . 2H 2 O was dissolved in a 1000 mL volumetric flask to prepare a barium chloride solution L with a concentration of 0.3053 g / mL 2 . Next, measure 220 mL of the above barium chloride solution L 2 , with 100 mL of low concentration p-hydroxyphenylglycine stock solution L 1 Under mechanical stirring, simultaneously add to the sedimentation filter device E1. Then, mechanical stirring was continued for 0.5 h, and then stood still for 12-24 h. Finally, filter the above-mentioned precipitate with a 800-mesh filter cloth to obtain 80.23 g of barium sulfate precipitate S1 and filtrate L 3 .

[0028] (2) Electr...

Embodiment 2

[0031] This example is aimed at the extraction of p-hydroxyphenylglycine in low-concentration p-hydroxyphenylglycine mother liquor, wherein the mass percentage of p-hydroxyphenylglycine is 5.0 wt%; the mass percentage of ammonium sulfate is about 39.1 wt%. The extraction steps are as follows:

[0032] (1) The operation steps in the sedimentation and filtration stage are the same as those in Example 1.

[0033] (2) Electrodialysis process: Take 100 mL of the above-mentioned mixed solution containing ammonium chloride, p-hydroxyphenylglycine and a small amount of barium chloride L3 Transfer to the first-stage electrodialysis unit E2, add 100 mL of 0.1 wt% HCl solution to the cathode chamber, and add 100 mL of 0.1 wt% NaOH solution to the anode chamber. Then, turn on the electrodialysis device and set the initial current density to 50.0mA / cm 2 , the voltage was 12.0V, the initial conductivity of the dense phase chamber was 11.19 mS / cm, the electrodialysis treatment temperature wa...

Embodiment 3

[0036] This example is aimed at the extraction of p-hydroxyphenylglycine in low-concentration p-hydroxyphenylglycine mother liquor, wherein the mass percentage of p-hydroxyphenylglycine is 5.0 wt%; the mass percentage of ammonium sulfate is about 39.1 wt%. The extraction steps are as follows:

[0037] (1) The operation steps in the sedimentation and filtration stage are the same as those in Example 1.

[0038] (2) Electrodialysis process: Take 100 mL of the above-mentioned mixed solution containing ammonium chloride, p-hydroxyphenylglycine and a small amount of barium chloride L 3 Transfer to the first-stage and one-stage electrodialysis device E2, add 100 mL of 1 wt% HCl solution to the cathode chamber, and add 100 mL of 1 wt% NaOH solution to the anode chamber. Then, turn on the electrodialysis device and set the initial current density to 30.0mA / cm 2 , the voltage was 6.0V, the initial conductivity of the dense phase chamber was 11.19 mS / cm, the electrodialysis treatment t...

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Abstract

The invention provides a method for extracting and recovering p-hydroxyphenylglycine. By adding barium salt, the sulfate ion in the mother liquor is precipitated, and the filtrate undergoes electrodialysis, evaporation and crystallization steps to obtain p-hydroxyphenylglycine product (p-hydroxyphenylglycine recovery Yield > 99.5%, purity > 80%) at the same time, nano-scale barium sulfate product was obtained. The present invention recovers high value-added p-hydroxyphenylglycine products from the dilute solution of p-hydroxyphenylglycine, and the product recovery efficiency is high; cheap barium salt effectively removes sulfate radicals in the mother liquor, and generates high value-added nano-scale barium sulfate products . The whole process has simple steps, convenient operation, low investment cost, and meets the technical requirements of industrial practical high-efficiency production.

Description

technical field [0001] The invention relates to the fields of fine chemical industry and pharmaceutical production, in particular to a method for extracting and recovering p-hydroxyphenylglycine. Background technique [0002] p-Hydroxyphenylglycine, formula C 8 h 9 NO 3 , is a pharmaceutical fine chemical, mainly used in the synthesis of β-lactam semi-synthetic antibiotics, such as amoxicillin (commonly known as amoxicillin), cefoperazone, cephradine, ceftrixin, ceftriaxone sodium and hydroxyl EPCP and 7ADCA and other antibiotic drugs. These drugs have a wide range of uses, can be injected or taken orally, and have killing effects on Gram-positive bacteria, Gram-negative bacteria, Toxoplasma, spirochetes, etc., and are broad-spectrum antibacterial and anti-inflammatory drugs. Diseases such as duodenal ulcer have satisfactory curative effect. [0003] The preparation methods of p-hydroxyphenylglycine mainly include benzaldehyde method, glyoxylic acid method and enzymatic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/40C07C227/42C07C229/36
CPCC07C227/40C07C227/42C07C229/36
Inventor 蒲彦锋杨浩侯明明王建红霍琳梦乔聪震
Owner HENAN UNIVERSITY
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