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Method for recovering and treating waste liquid generated during 4-cyano benzyl chloride production

A recovery treatment and waste liquid recovery technology, which is applied in chemical instruments and methods, preparation of organic compounds, purification/separation of carboxylic acid nitriles, etc., can solve problems such as environmental pollution and occupying a large space, so as to reduce production costs and prevent pollution , the effect of cheap raw materials

Inactive Publication Date: 2014-07-02
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These industrial waste liquids have become a disgusting burden for factories to keep and discard. Some factories have to store them in barrels for a long time, which not only takes up a lot of space, but also sometimes causes environmental pollution due to leakage and waste liquid flow out.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100g of industrial waste liquid, 3g of zinc chloride and 600g of water into a 1000mL four-necked flask equipped with a thermometer, a condenser and an electromagnetic stirrer at the same time. After heating and reflux for 8 hours of hydrolysis reaction, cool to room temperature and separate layers, take the upper layer of water and solid The mixture was filtered to obtain 20 g of p-cyanobenzaldehyde white product with a purity of 95.5%.

[0027] Take 50 g of the solid oil in the lower layer, add 120 g of 20% glacial acetic acid aqueous solution and 15 g of urotropine, heat and reflux for 3 hours, add hydrochloric acid to adjust the pH of the solution to about 3, continue the reaction for 3 hours, cool to 80 ° C, and then add NaOH aqueous solution to make The pH of the solution was about 6, cooled to room temperature, and filtered to obtain 10 g of a yellow crude product with a purity of 88%.

[0028] A total of 30 g of the above-mentioned crude product was added, 15...

Embodiment 2

[0030] The operation method is basically the same as in Example 1, the only difference is that 100g of industrial waste liquid, 6g of zinc chloride and 500g of water are added to a 1000mL four-neck flask at the same time, and after 16 hours of reflux hydrolysis reaction, it is cooled to room temperature and separated, and the upper layer of water-solid mixture is taken Filter to obtain 27g p-cyanobenzaldehyde crude product, purity 95%.

[0031] Take 50 g of the solid oil in the lower layer, add 150 g of 25% glacial acetic acid aqueous solution and 20 g of urotropine, reflux for 3 h, add hydrochloric acid to adjust the pH of the solution to about 2, continue the reaction for 2 h, cool to 80 ° C, then add NaOH to make the solution The pH was about 6, continued cooling to room temperature, and filtered 16g of crude product with a purity of 88.9%.

[0032] Add 172g of 20% ethanol aqueous solution to 43g of the above-mentioned crude product, heat to reflux, cool and crystallize, fi...

Embodiment 3

[0034] The operation method is basically the same as in Example 1, the only difference is that 100g of industrial waste liquid, 5g of zinc chloride and 650g of water are added to a 1000mL four-neck flask at the same time, and after 18 hours of reflux hydrolysis reaction, it is cooled to room temperature and separated, and the upper layer of water-solid mixture is taken Filter to obtain 34g p-cyanobenzaldehyde product, the purity is 96.6%.

[0035] Take 50 g of solid oil in the lower layer, add 150 g of 30% glacial acetic acid aqueous solution and 25 g of urotropine, reflux for 3 h, add hydrochloric acid to adjust the pH of the solution to about 1, continue the reaction for 1 h, cool to 80 ° C, then add NaOH to make the solution The pH was about 7, continued to cool to room temperature, and the filtered 15g crude product had a purity of 90.6%.

[0036] Add 200g of 20% methanol aqueous solution to 49g of the above-mentioned crude product, heat to reflux, cool and crystallize, fi...

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Abstract

The invention relates to a method for recovering and treating waste liquid generated during 4-cyano benzyl chloride production. The method comprises the following steps of: firstly adding water and zinc chloride to industrial waste liquid generated during the production process of 4-cyano benzyl chloride used as the raw material of fluorescent brightener ER-II, carrying out hydrolysis reaction, cooling and filtering an upper-layer product to obtain a crude product A of 4-cyano benzaldehyde, and adding a glacial acetic acid aqueous solution and methenamine to a lower-layer oil product for oxidation reaction to obtain a crude product B of 4-cyano benzaldehyde; and purifying the crude products, heating and refluxing, cooling and crystallizing and drying to obtain the finished 4-cyano benzaldehyde product. The method provided by the invention solves the problem of large occupation area of the industrial waste liquid and prevents environmental pollution caused by the industrial waste liquid; the recovery treatment method recovers the chemical raw material 4-cyano benzaldehyde, and creates good economical benefit and social benefit; and the process is simple and is easy for industrial production.

Description

technical field [0001] The invention relates to a technology for producing fluorescent whitening agent ER-II, in particular to a method for recycling and treating waste liquid produced during the production of fluorescent whitening agent ER-II raw material p-cyano-benzyl chloride. Background technique [0002] The main raw material for the production of fluorescent whitening agent ER-II is p-cyano-benzyl chloride, which is mainly obtained from p-toluene cyanide through chlorination. Because the reaction conditions are difficult to control, not only p-cyano-benzyl chloride, but also p-cyano-dichlorobenzyl and p-cyanotrichlorobenzyl are obtained during the production process, and p-cyano-benzyl chloride can be obtained by separation as raw materials to produce fluorescent whitening Agent ER-II, and the remaining large amount of waste liquid contains p-cyanomonochlorobenzyl, dichlorobenzyl and, trichlorobenzyl and p-toluene cyanide, and a small amount of unknown substances. H...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/56C07C253/30C07C253/34
Inventor 武宝萍卢星河
Owner HUAIHAI INST OF TECH