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A kind of hydroxyphenylglycine centrifugal mother liquor treatment device and method

A technology of hydroxyphenylglycine mother and p-hydroxyphenylglycine, which is applied in the field of resource recycling and utilization, can solve the problems of complicated equipment and inability to separate o-hydroxyphenylglycine, and achieves the effects of improving operation efficiency, good environmental protection and good economic benefits.

Active Publication Date: 2022-05-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The resin method is mostly used in the separation of phenol and salt in the mother liquor of p-hydroxyphenylglycine, and is rarely used in the separation and recovery of p-hydroxyphenylglycine and salt. The invention patent CN201310375423.7 introduces a strong acidic cation exchange resin continuous chromatographic separation method , this method can separate p-hydroxyphenylglycine and ammonium sulfate solids from hydroxyphenylglycine mother liquor, but this method needs 20 separation units, the equipment is relatively complicated, and o-hydroxyphenylglycine cannot be separated

Method used

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  • A kind of hydroxyphenylglycine centrifugal mother liquor treatment device and method
  • A kind of hydroxyphenylglycine centrifugal mother liquor treatment device and method
  • A kind of hydroxyphenylglycine centrifugal mother liquor treatment device and method

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Effect test

Embodiment 1

[0034] The waste water is the mother liquor (para-hydroxyphenylglycine) obtained by centrifuging the reaction solution after synthesizing p-hydroxyphenylglycine by one-step method of phenol, glyoxylic acid and sulfamic acid, removing phenol and crystallizing the p-hydroxyphenylglycine after post-treatment. The mass concentration of glycine is 1.17%, the mass concentration of o-hydroxyphenylglycine is 2.85%, and the mass concentration of ammonium sulfate is 20%). 5m, each resin tower is filled with D113 resin, and the volume of filled resin is 5m 3 , the control mother liquor flow is 14m 3 / h, the total mother liquor volume is 140m 3 , the amount of mother liquor can make 3 to 4 resin towers saturated. After the adsorption tower is saturated, desorb with hot water, control the hot water temperature to be 50 °C, and the hot water elution flow rate to be 4 m 3 / h, the specific steps are as follows:

[0035] 1. Refer to Figure 4 , the first resin tower 3 and the second resin...

Embodiment 2

[0044] The hydroxyphenylglycine centrifugal mother liquor (para-hydroxyphenylglycine mass concentration 1.18%, o-Hydroxyphenylglycine mass concentration 2.87%, ammonium sulfate mass concentration 20%) was first passed through the filter to remove insoluble particles, and then entered the resin tower, as described in Example 1. The above method is operated, the difference is: the first resin tower 3 is filled with H103 type resin, the second resin tower 4 and the third resin tower 5 are filled with 105 type resin, and each tower is filled with 5m resin 3 , the control mother liquor flow is 14m 3 / h, the total mother liquor volume is 140m 3, p-hydroxyphenylglycine and o-hydroxyphenylglycine were adsorbed on the resin. The adsorbed wastewater enters the MVR, and is concentrated and crystallized to obtain ammonium sulfate solid (yield 99.0%, purity 99.3%). The resin saturated with adsorption is desorbed with hot water, the temperature of the hot water is controlled to be 55 °C, ...

Embodiment 3

[0046] The hydroxyphenylglycine centrifugal mother liquor (para-hydroxyphenylglycine mass concentration 1.23%, o-Hydroxyphenylglycine mass concentration 2.97%, ammonium sulfate mass concentration 18%) was first passed through the filter to remove insoluble particles, and then entered the resin tower, as described in Example 1. The above method is operated, the difference is: the first resin tower 3 is filled with H103 type resin, the second resin tower 4 and the third resin tower 5 are filled with 511 type resin, and each tower is filled with 5m resin 3 , the control mother liquor flow is 13m 3 / h, the total mother liquor volume is 130m 3 , p-hydroxyphenylglycine and o-hydroxyphenylglycine were adsorbed on the resin. The adsorbed wastewater enters the MVR, and the ammonium sulfate solid obtained by concentrating and crystallizing (98.9% yield, 99.2% purity). The resin saturated with adsorption is desorbed with hot water, the temperature of the hot water is controlled to be 6...

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Abstract

The invention discloses a treatment device and method for hydroxyphenylglycine centrifugal mother liquor. The device includes a mother liquor pool, a filter, a resin tower, an eluent storage tank, a desorption liquid collection pool, graded concentration equipment, an ammonium sulfate solid collection tank, p-Hydroxyphenylglycine crystallization collection pool, o-hydroxyphenylglycine crystallization collection pool and MVR evaporator; the water inlet of the filter is communicated with the mother liquor pool; the resin tower is composed of several resin tower units; when the resin tower unit is saturated with adsorption As an eluting tower, it is respectively connected with the eluent storage tank and the desorption liquid collection pool, and the other resin tower units are connected in series to form an adsorption tower, which is connected with the filter outlet and the MVR evaporator through pipelines. The invention realizes continuous production, the recovery rate of p-hydroxyphenylglycine is 87.8%, the purity is 99.0%, the recovery rate of o-hydroxyphenylglycine is 88.1%, the purity is 95.0%, the ammonium sulfate solid yield is 99.1%, and the purity is 99.5%.

Description

(1) Technical field [0001] The invention belongs to the field of resource recovery and utilization in the p-hydroxyphenylglycine production industry. (2) Background technology [0002] p-Hydroxyphenylglycine, molecular formula C 8 H 9 NO 3 , the relative molecular mass of 167.16, the melting point of 240 ℃ (decomposition), is an important raw material for the synthesis of antibiotics amoxicillin, cefadroxil, cefoperazone, cefuroxime and cefadroxil. The method that utilizes phenol, glyoxylic acid and sulfamic acid one-step method to synthesize p-Hydroxyphenylglycine is well used in industrial production at present, and the reaction equation is as follows: [0003] [0004] The reaction uses water as a solvent, and a small amount of o-hydroxyphenylglycine is generated along with the side reaction. At the same time, a large amount of ammonium sulfate is generated during the reaction process and the pH adjustment process of the post-reaction treatment. Since p-hydroxyphen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/40C07C229/36C01C1/24
CPCC07C227/40C01C1/24C07C229/36
Inventor 丁成荣葛淑婷张国富吕井辉赵以勇
Owner ZHEJIANG UNIV OF TECH