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Method of recovering o-aminobenzoic acid from mother liquid or waste water

An anthranilic acid, waste water technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high energy consumption and large consumption of ethyl acetate

Inactive Publication Date: 2007-03-07
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The anthranilic acid production mother liquor contains about 0.4% of anthranilic acid. The existing production process usually adopts ethyl acetate extraction method to recover, and the recovery rate is only about 63%. At the same time, due to the high solubility of ethyl acetate in water, it takes The ethyl acetate in the wastewater is recovered by distillation, so the energy consumption is high and the loss of ethyl acetate is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Get anthranilic acid synthetic mother liquor 500ml, anthranilic acid concentration is 4500mg / L, add sulfuric acid or sodium hydroxide and regulate mother liquor pH and be 7-8; Get weakly basic ion exchange resin (335 produced by Shanghai Huazhen Technology Trading Company Type weakly basic ion exchange resin) 10ml column, treated with dilute sulfuric acid and dilute sodium hydroxide solution to form OH type and then adsorbed. The adsorption temperature is 5°C, the flow rate is 2BV / h, and the concentration of anthranilic acid in the adsorbed water is 765mg / L. The recovery rate was 83%. After saturated adsorption, use 2% sodium hydroxide solution to desorb at a temperature of 35° C. and a flow rate of 2 BV / h to obtain a sodium anthranilate solution with a desorption rate of 98.6%.

Embodiment 2

[0016] Get anthranilic acid synthesis mother liquor 500ml, anthranilic acid concentration is 4500mg / L, add sulfuric acid or sodium hydroxide and regulate mother liquor PH=7; Basic ion-exchange resin) 10ml column, after treatment with dilute potassium hydroxide solution and dilute hydrochloric acid into Cl type, adsorption, adsorption temperature 40 ℃, flow rate 4BV / h, the concentration of anthranilic acid in the adsorbed water is 990mg / L, the recovery rate 78%. After saturated adsorption, use 4% sodium hydroxide solution to desorb at a temperature of 45° C. and a flow rate of 3 BV / h to obtain a sodium anthranilate solution with a desorption rate of 98.6%.

Embodiment 3

[0018] Get anthranilic acid synthesis mother liquor 500ml, anthranilic acid concentration is 4500mg / l, add sulfuric acid to adjust mother liquor PH=3;

[0019] Get strong polarity macroporous adsorption resin (NKA-2 type strong polarity macroporous adsorption resin of the styrene-diethylbenzene structure produced by Tianjin Nankai Chemical Factory) 10ml packing column, pretreatment is as follows: successively with 4% hydrochloric acid, Acetone, 4% sodium hydroxide solution and washed to neutral.

[0020] Adsorption: The adsorption temperature is 25°C, the flow rate is 3BV / h, the concentration of anthranilic acid in the adsorbed water is 1080mg / l, and the recovery rate is 76%. After saturated adsorption, use 4% sodium hydroxide solution to desorb at a temperature of 90° C. and a flow rate of 1 BV / h to obtain a sodium anthranilate solution with a desorption rate of 98.6%.

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Abstract

The invention discloses a recycling method of o-aminobenzoic acid from mother liquid or waste water, which comprises the following steps: loading weak alkaline ion exchanging resin or phenylethene-diethyl benzene strong-polar large-hole adsorbing resin in the adsorbing column; adding acid or alkaline to adjust pH value for mother liquid or waste water; assembling adsorbing column under 5-40 deg.c with flow speed at 2-4BV / h; eluting through 2-6% sodium hydroxide solution under 25-45 deg.c with flow speed at 2-3BV / h; recycling sodium o-aminobenzoic solution.

Description

technical field [0001] The present invention relates to the recovery of anthranilic acid, specifically, the recovery of anthranilic acid in mother liquor or waste water by means of resin adsorption and desorption. Background technique [0002] The anthranilic acid production mother liquor contains about 0.4% of anthranilic acid. The existing production process usually adopts ethyl acetate extraction method to recover, and the recovery rate is only about 63%. At the same time, due to the high solubility of ethyl acetate in water, it takes The ethyl acetate in the waste water is recovered by distillation, so the energy consumption is high and the loss of ethyl acetate is large. Contents of the invention [0003] The present invention is a kind of use weak alkaline or macroporous adsorption resin to absorb anthranilic acid under the conditions of pH 2-8, 5-40 ℃, and flow rate 2-4BV / h, and then use dilute lye (with sodium hydroxide solution as Representative), or organic solv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/56C07C227/40
CPCC07C227/40C07C229/56
Inventor 赵玉明陈飞陶阳宇
Owner NANJING UNIV
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