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Clean production method of N-cyanoethylaniline

A technology of cyanoethylaniline and clean production, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as refractory high COD wastewater, reduce discharge, eliminate adverse effects, and design rationally Effect

Active Publication Date: 2011-11-16
JIANGSU HELIRUI TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The invention provides a clean production method of N-cyanoethylaniline to solve the problem of producing a large amount of difficult-to-handle high COD wastewater in the production process

Method used

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  • Clean production method of N-cyanoethylaniline

Examples

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Comparison scheme
Effect test

Embodiment 1

[0023] Put 4,200 parts of bottom water into the reactor, start stirring, and then add 300 parts of zinc chloride, 12 parts of hydroquinone, 150 parts of sodium bicarbonate, 100 parts of hydrochloric acid (mass concentration 31%), 2700 parts of aniline, acrylonitrile 1740 parts, after heating up to 60°C, start to heat up slowly, uniformly heat up to 95°C in about 10 hours, keep warm for 10 hours, turn off stirring, let stand for 45 minutes, separate the water layer to the mother liquor water storage tank, and produce 4800 parts of mother liquor water. After the separation, 12 parts of sodium bicarbonate was added to the reaction product with stirring until the pH value was about 4. Acrylonitrile was recovered under vacuum to obtain 195 parts of a mixture of acrylonitrile and water, including 70 parts of acrylonitrile and 125 parts of water. The reaction product recovered from acrylonitrile is sucked into the aniline evaporator, heated to 100°C, flushed with 100°C steam, and 800...

Embodiment 2

[0026] Drop into 4500 parts of the mother liquor water of embodiment 1, start stirring, drop into 300 parts of zinc chloride successively, 12 parts of hydroquinone, 150 parts of sodium bicarbonate, 100 parts of hydrochloric acid (mass concentration 31%), 2700 parts of aniline, acrylonitrile 1740 parts, after heating up to 60°C, start to heat up slowly, uniformly heat up to 95°C in about 10 hours, keep warm for 10 hours, turn off stirring, let stand for 45 minutes, separate the mother liquor water to the mother liquor water storage tank. Produce 4800 parts of mother liquor water, after separation, 12 parts of sodium bicarbonate are added to the reaction product under stirring until the pH value is about 5. . 195 parts of a mixture of acrylonitrile and water were recovered under vacuum, including 70 parts of acrylonitrile and 125 parts of water. Inhale N-cyanoethylaniline into the aniline evaporator, raise the temperature to 125°C, pour in steam at 125°C, distill 800 parts of t...

Embodiment 3

[0029]Drop into 4700 parts of the mother liquor water of embodiment 2, start stirring, drop into 300 parts of zinc chloride successively, 12 parts of hydroquinone, 150 parts of sodium bicarbonate, 100 parts of hydrochloric acid (mass concentration 31%), 2700 parts of aniline, acrylonitrile 1740 parts, after heating up to 60°C, start to heat up slowly, uniformly heat up to 95°C in about 10 hours, keep warm for 10 hours, turn off stirring, let stand for 45 minutes, separate mother liquor water to mother liquor water storage tank, and produce 4800 parts of mother liquor water. After the separation, 13 parts of sodium bicarbonate was added under stirring until the pH value was about 6. 195 parts of a mixture of acrylonitrile and water were recovered under vacuum, including 70 parts of acrylonitrile and 125 parts of water. Inhale N-cyanoethylaniline into the aniline evaporator, raise the temperature to 150°C, pour in steam at 150°C, distill 800 parts of distillate, and take samples...

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Abstract

The invention discloses a clean production method of N-cyanoethylaniline. The method comprises the following steps: synthesizing N-cyanoethylaniline by utilizing aniline and acrylonitrile as raw materials in the presence of hydrochloric acid and zinc chloride; after the reaction, adding sodium bicarbonate into the mixture of which the water layer is separated out so as to recycle acrylonitrile, pumping steam into the mixture without acrylonitrile to distill, adding sodium carbonate or sodium bicarbonate after distillation, and evenly mixing the solution to obtain N-cyanoethylaniline; and recycling aniline and N-cyanoethylaniline from the distillate of distillation, and recycling water generated in the reaction. In the method, according to the practical applications of N-cyanoethylaniline, the content of aniline in a product is reduced to eliminate the negative influences on the subsequent application of N-cyanoethylaniline; and the output of high concentration wastewater can be reduced in the production, the design of the reaction steps is reasonable and the aim of clean production can be effectively achieved.

Description

technical field [0001] The invention relates to a production method of N-cyanoethylaniline, in particular to a clean production method of N-cyanoethylaniline. Background technique [0002] N-cyanoethylaniline is an important chemical raw material and intermediate, widely used in fine chemical products such as dyes, such as synthetic intermediates N-cyanoethyl-N-benzylaniline, N-cyanoethyl-N- Acetoxyethylaniline, the former is used to synthesize C.I.288 orange, and the latter can be used to synthesize C.I.30 orange, both of which are the most commonly used disperse dyes. [0003] The most commonly used synthesis method of N-cyanoethylaniline is to take aniline and acrylonitrile as main raw materials, synthesize N-cyanoethylaniline under the catalysis of acetic acid (or hydrochloric acid) and zinc chloride, reclaim acrylonitrile, add water to cool down and crystallize , filtered, washed. [0004] The reaction formula is as follows: [0005] [0006] In the prior art, wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/24C07C253/30
Inventor 高立江景雪苹陶彬彬靡云祥陈田木阮海兴
Owner JIANGSU HELIRUI TECH DEV CO LTD
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