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Preparation method of isophthalonitrile

A technology of isophthalonitrile and isophthalic acid is applied in chemical instruments and methods, ammonia-carboxylic acid reaction preparation, organic compound/hydride/coordination complex catalyst, etc. problems such as low temperature, to achieve the effect of short reaction route, low reaction temperature and simple preparation

Inactive Publication Date: 2019-05-17
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem of the production of aromatic dicyanonitrile in the prior art, provide a kind of preparation method of isophthalonitrile, the process raw material is cheap and easy to get, the reaction route is short, the product is easy to handle, and catalyst preparation Simple, low reaction temperature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Preparation of ethylmethylimidazole dihydrogen phosphate ionic liquid: Add 0.1mol 1-methylimidazole into a three-neck flask, add 0.1mol diethyl phosphate dropwise, continue stirring for 2 hours after the addition, and react to obtain colorless transparent ions Liquid 1-methyl-3-ethylimidazolium ethyl phosphate; NaOH twice the number of moles of 1-methyl-3-ethylimidazolium ethyl phosphate is dissolved in ethanol and added dropwise to 1-methanol In the ethanol solution of 3-ethylimidazolium ethyl phosphate, a white precipitate is produced, which is filtered to obtain a colorless transparent liquid, and an equimolar phosphoric acid solution is added to the liquid, a small amount of solid is produced, and the liquid is obtained by filtering again; the above liquid Evaporated to remove water and alcohol, and then vacuum-dried to obtain the product ethylmethylimidazolium dihydrogen phosphate, with a yield of 97%;

[0020] Add 50g of isophthalic acid into the nitrilation react...

Embodiment 2

[0022] Preparation of ethylmethylimidazolium dihydrogen phosphate ionic liquid: Add 0.5mol 1-methylimidazole into a three-neck flask, add 0.5mol diethyl phosphate dropwise, continue stirring for 1.5h after the addition, and the reaction is colorless and transparent Ionic liquid 1-methyl-3-ethylimidazolium ethyl phosphate; NaOH twice the number of moles of 1-methyl-3-ethylimidazolium ethyl phosphate was dissolved in ethanol and added dropwise to 1- In the ethanol solution of methyl-3-ethylimidazolium ethyl phosphate, a white precipitate is produced, which is filtered to obtain a colorless transparent liquid, and an equimolar phosphoric acid solution is added to the liquid, a small amount of solid is produced, and the liquid is obtained by filtering again; the above The liquid was evaporated to remove water and alcohol, and then vacuum-dried to obtain the product 1-methyl-3-ethylimidazolium ethyl phosphate with a yield of 98%;

[0023] Add 100g of isophthalic acid into the nitri...

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Abstract

The invention relates to a preparation method of isophthalonitrile. The preparation method of isophthalonitrile comprises the following steps: adding isophthalic acid to a cyanation reactor, and adding an ethyl methylimidazolium dihydrogen phosphate ionic liquid accounting for 15%-50% by volume of isophthalic acid; introducing ammonia, and performing a reaction; after the reaction, performing distillation purification on a crude isophthalonitrile product to obtain isophthalonitrile. The ethyl methylimidazolium dihydrogen phosphate ionic liquid serves as a solvent and a catalyst to be used forpreparing isophthalonitrile from isophthalic acid by cyanation, compared with the prior art, the raw materials are easily available, the operation is simple, the catalyst is simple to prepare, and thereaction temperature is reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of isophthalonitrile. Background technique [0002] Aromatic dibasic nitriles are fine chemical intermediates with a wide range of uses. Using the chemical activity of the cyano group, they can be used to synthesize a series of pesticides, medicines, dyes, spices, etc., and are widely used in various fields of the national economy. [0003] The traditional preparation methods of aromatic dibasic nitriles include sandmeyer reaction, direct cyanation of halogenated hydrocarbons and cyanides, dehydration of aromatic aldehydes through aldoxime or gas-phase catalytic ammoniation, etc. These methods generally have long reaction routes, complicated processes, and difficult separation and purification. , serious pollution, especially raw materials are difficult to obtain or more expensive reagents need to be used, so the production cost is higher, and it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/22C07C255/51B01J31/02
CPCY02P20/54
Inventor 孙海龙
Owner SINOPEC YANGZI PETROCHEM
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