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A kind of n-cyanoethylaniline zero-emission production process

A cyanoethylaniline and production process technology, which is applied in the field of N-cyanoethylaniline production process, can solve the problems of affecting the quality of production varieties, many operation steps, and high processing costs, and achieve high economic and social benefits. The effect of obvious cost reduction and product yield increase

Active Publication Date: 2017-10-10
JIANGSU JIHUA CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The production method of traditional N-cyanoethylaniline is to adopt hydrochloric acid, acetic acid, sulfuric acid, zinc chloride or aluminum chloride etc. as catalyzer, use hydroquinone to synthesize as polymerization inhibitor, the mother liquor water after the synthesis and The washing water is discharged after sewage treatment, and the aniline and N-cyanoethylaniline in the mother liquor water are not used, so the product yield is low, and the sewage belongs to high COD wastewater, and the treatment cost is high
At present, domestic manufacturers mostly adopt the method improved by the water phase production method. Generally, zinc chloride is added as a cocatalyst, which requires operations such as steam distillation, stratification, and neutralization. The operation is complicated, the operation steps are many, and the energy consumption is large. The content of N, N-dicyanoethylaniline in N-cyanoethylaniline is high (generally more than 2%), which will affect the quality of subsequent production varieties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the 1000ml autoclave, add the mother liquor water and washing water of comparative example 1, zinc chloride 0.2g, hydroquinone 0.1g, aniline 140g, acrylonitrile 80g and the acrylonitrile (comprising aqueous phase) of recovery in comparative example 1 ). The temperature was raised to 110° C. and kept for 20 hours, and excess acrylonitrile was distilled under normal pressure, and 14.8 g of acrylonitrile and 21 g of water were recovered. The reaction mass was slowly cooled to 25° C., vacuum filtered and washed with a small amount of water to obtain 211 g (100 percent) of the product, 475 ml of mother liquor, and 60 ml of washing water. Product yield 97%, N, N-dicyanoethylaniline 1.4%. The mother liquor water was used for the next test and the operation was repeated.

Embodiment 2

[0017] In a 1000ml autoclave, add the mother liquor water and washing water of Example 1, zinc chloride 0.05g, aluminum trichloride 0.1g, hydroquinone 0.1g, aniline 140g, acrylonitrile 80g and the recovery in Example 1 of acrylonitrile (including the aqueous phase). The temperature was raised to 110° C. and kept for 20 hours, and excess acrylonitrile was distilled under normal pressure, and 15.1 g of acrylonitrile and 20.5 g of water were recovered. The reaction mass was slowly cooled to 25° C., vacuum filtered and washed with a small amount of water to obtain 213 g (100 percent) of the product, 472 ml of mother liquor, and 55 ml of washing water. The product yield is 97.9%, and N,N-dicyanoethylaniline is 1.2%. The mother liquor water was used for the next test and the operation was repeated.

Embodiment 3

[0019] In a 1000ml autoclave, add the mother liquor water and washing water of Example 2, 0.2g of hydrochloric acid, 0.1g of hydroquinone, 140g of aniline, 80g of acrylonitrile and the recovered acrylonitrile (including the water phase) in Example 2. The temperature was raised to 110° C. and kept for 20 hours, and excess acrylonitrile was distilled under normal pressure to recover 15 g of acrylonitrile and 19 g of water. The reaction mass was slowly cooled to 25° C., vacuum filtered and washed with a small amount of water to obtain 212 g (100 percent) of the product, 470 ml of mother liquor, and 60 ml of washing water. The product yield is 97.4%, and N,N-dicyanoethylaniline is 1.4%. The mother liquor water was used for the next test and the operation was repeated.

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Abstract

The invention discloses a zero-emission production process for N-cyanoethylaniline. The process uses aniline and acrylonitrile as raw materials, and adds a catalyst and hydroquinone to synthesize N-cyanoethylaniline in the water phase. After the reaction Recover excess acrylonitrile under normal pressure, slowly cool down to below 25°C after recovery, filter and wash the product with a small amount of water. Mother liquor water and washing water are collected as the bottom water of the next reaction. When feeding the next reaction, add catalyst and hydroquinone according to the residual amount of catalyst and hydroquinone in the mixed bottom water. The total amount of catalyst and the first feeding amount Equal, the content of N-cyanoethylaniline obtained by filtration is more than or equal to 98%, and the content of N, N-dicyanoethylaniline is less than or equal to 1.5%. There is no discharge of three wastes in the production process, and it is truly a zero-emission process.

Description

technical field [0001] The present invention relates to the production technology of N-cyanoethylaniline. Background technique [0002] N-cyanoethylaniline is an important fine chemical raw material and intermediate, which can be used in the synthesis of fine chemical intermediates such as dyes and pesticides, such as: N-cyanoethyl-N-acetoxyethylaniline, N-cyano Ethyl-N-benzylaniline, N-cyanoethyl-N-benzoyloxyethylaniline, N-cyanoethyl-N-ethylaniline and other products are widely used in the dye and pesticide industries. [0003] The production method of traditional N-cyanoethylaniline is to adopt hydrochloric acid, acetic acid, sulfuric acid, zinc chloride or aluminum chloride etc. as catalyzer, use hydroquinone to synthesize as polymerization inhibitor, the mother liquor water after the synthesis and The washing water is discharged after sewage treatment, and the aniline and N-cyanoethylaniline in the mother liquor water are not utilized, so the product yield is low, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/24C07C253/30C07C253/34
Inventor 陆洪汇屠国锋周洪斌刘道明
Owner JIANGSU JIHUA CHEMICAL CO LTD
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