Method for treating and recycling waste water in anthranilic acid production technology

A technology for the production process of anthranilic acid, which is applied in the field of treatment and recycling of anthranilic acid production process wastewater, and can solve the problem of wasting phthalimide, large consumption of ethyl acetate, and inability to realize o-amino benzoic acid Recycling of benzoic acid and phthalimide, etc., to achieve the effect of recycling waste

Inactive Publication Date: 2013-11-27
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Each ton of product will produce 15-18m of waste water 3 , the wastewater is reddish brown, CODc r 23000-24000mg / L, of which phthalimide is 7800-8100mg / L, the content of anthranilic acid is 6000-6500mg / L, and the content of sodium chloride is 100-120g / L. The salt content is high. The current treatment method is mainly to concentrate the process wastewater and treat it as a hazardous solid waste. Not only the treatment cost is high, but also the expensive phthalimide, anthranilic acid and Sodium chloride; or use ethyl acetate extraction method to recover, the recovery rate is only about 63%, and the consumption of ethyl acetate is relatively large, and the energy consumption is relatively high, so there is no economical and effective treatment method for the waste water of this process so far
[0010] Invention patents such as Zhao Yuming (ZL200610041529.3) adopted weakly basic ion exchange resins or styrene-divinylbenzene type strong polar resins, and proposed a method for reclaiming anthranilic acid from mother liquor or waste water. What the invention relates to is a kind of process waste water (CODc r 23000~24000mg / L), containing a large amount of inorganic salts, so the process of ion exchange adsorption cannot realize the resource utilization of anthranilic acid and phthalimide in wastewater
[0011] The invention patent applied by Meng Fanqiu and others (application number 201110073494.2) relates to a preparation method for recovering anthranilic acid from methyl anthranilate mother liquor wastewater, which is based on the mother liquor wastewater generated during the production of methyl anthranilate and the saccharin production process. The waste acid water that produces obtains anthranilic acid through preparation of copper salt, alkali dissolution, pressure filtration, decolorization, acid analysis, suction filtration, and drying. process wastewater

Method used

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  • Method for treating and recycling waste water in anthranilic acid production technology
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  • Method for treating and recycling waste water in anthranilic acid production technology

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Pack 20mL (about 15g, dry weight) of NDA150 resin and ZH01 resin into two adsorption columns (Φ20×250mm) with insulation jackets respectively.

[0031] Get 1000mL of reddish-brown process wastewater in the production of anthranilic acid and filter it, add 0.5ml of 1% sodium hydroxide solution dropwise, the pH is 7.92, and the upper column liquid COD Cr The content of anthranilic acid is 24170mg / L, the content of anthranilic acid is 6160mg / L, and the content of phthalimide is 7960mg / L. At 35±5℃, 640ml of column liquid is passed through the ZH01 resin column at a flow rate of 40mL / h. Grade effluent is light yellow, phthalimide content is 12.2mg / L, phthalimide content is 6014mg / L, COD Cr Reduced to 13990mg / L, after adding 0.5ml of 1% dilute hydrochloric acid dropwise, the pH was 5.08, and at 35±5°C, 400ml of the upper column liquid was passed through the NDA150 resin column at a flow rate of 40mL / h, and the secondary adsorption water was colorless, adjacent Phthalimide un...

Embodiment 2

[0035] Pack 200mL (about 150g, dry weight) of NDA150 resin and 300mL (about 225g, dry weight) of ZH01 resin into two adsorption columns (Φ35×500mm) with insulation jackets respectively.

[0036] Get 10L reddish-brown process wastewater in the production of anthranilic acid and filter, then add dropwise 5ml of 1% sodium hydroxide solution, the pH is 8.04, and the upper column liquid COD Cr The content of anthranilic acid is 23960mg / L, the content of anthranilic acid is 6210mg / L, and the content of phthalimide is 8026mg / L. At 5±5℃, 6400ml of column liquid is passed through the ZH01 resin column at a flow rate of 200mL / h. The grade effluent is pale yellow, the content of phthalimide is 14.7mg / L, the content of anthranilic acid is 6102mg / L, COD Cr Reduced to 14160mg / L, after adding 5ml of 1% dilute hydrochloric acid dropwise, the pH was 4.98, and 6400ml of the upper column liquid was passed through the NDA150 resin column at a flow rate of 200mL / h at 5±5°C, and the secondary adsorpt...

Embodiment 3

[0040] Change the ZH01 resin in Examples 1 and 2 in Examples 1 and 2 into FZH11, ZH124, ZH33 respectively, and change NDA150 resin into JX101 resin, CHA111 resin, AmberLiteXAD-7, XAD-4, XAD-2 resin respectively, Other operating conditions remained unchanged, and the results were basically the same except that the volume of each batch and the amount of recovery were changed.

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Abstract

The invention discloses a method for treating and recycling waste water in an anthranilic acid production technology. Through the adoption of the method provided by the invention, waste water in the anthranilic acid production technology can be treated, and recycled organic substances can be directly subjected to cyclic utilization; the CODCr being about 24000 mg / L of waste water before treatment is reduced to 80 mg / L below after treatment to reach the national-level emission standard; coarse sodium chloride salt can be recycled; resin is subjected to desorption and regeneration by using 4-6% of dilute sodium hydroxide solution or dilute hydrochloric acid, and a desorption solution can be taken as raw materials to be input in the acidizing step or degrading step of the original production technology, so that the product quality is not affected, 99% of anthranilic acid and phthalimide in the waste water can be recycled, and distilled effluent can be utilized repeatedly; waste water can be treated while the waste recycling can be realized.

Description

technical field [0001] The invention relates to a process wastewater (CODc) produced by degrading and acidifying phthalic anhydride and urea to produce phthalimide as raw materials to obtain anthranilic acid. r 23000~24000mg / L) treatment and recycling method for recovering organic matter. Specifically, it is the recycling of organic matter anthranilic acid and phthalimide in process wastewater, and at the same time realizes the purification and reuse of wastewater or discharges up to the standard, and finally realizes the treatment and protection of anthranilic acid production process wastewater. resourceful. Background technique [0002] The synthetic route applicable to this method is to use phthalic anhydride and excess urea as starting materials for amidation to obtain phthalimide, and then degrade it with sodium hypochlorite under alkaline conditions to obtain sodium anthranilic acid , to obtain anthranilic acid after acidification with hydrochloric acid, the main pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C07C229/56C02F103/36
Inventor 费正皓杨珊珊刘总堂吴秀红顾云兰孙玉凤邢蓉施卫忠
Owner YANCHENG TEACHERS UNIV
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