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Preparation method of adiponitrile

A technology of adiponitrile and adipic acid, applied in the field of preparation of adiponitrile, can solve the problems of high reaction temperature, serious side reactions, long reaction time, etc., and achieves reduction of side reactions, improvement of yield, reduction of time and temperature Effect

Inactive Publication Date: 2019-01-15
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method of producing adiponitrile from adipic acid used in industry is usually carboxylic acid ammonification method. The widely used process is to heat and dissolve carboxylic acid or its derivatives in an open system, and then continuously inject ammonia gas into the solution , so that the system reacts in the presence of catalysts such as phosphoric acid or phosphate. This process has problems such as high reaction temperature, long reaction time, and serious side reactions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 0.1mol 1-methylimidazole into a three-necked flask, add 0.1mol diethyl phosphate dropwise, continue stirring for 2 hours after the addition, and react to obtain a colorless and transparent ionic liquid 1-methyl-3-ethane imidazole ethyl phosphate;

[0025] (2) Dissolve NaOH twice the number of moles of 1-methyl-3-ethylimidazolyl ethyl phosphate in ethanol, and add dropwise to the ethanol solution of 1-methyl-3-ethylimidazolium ethyl phosphate In the process, a white precipitate was produced, which was filtered to obtain a colorless transparent liquid, and equimolar phosphoric acid solution was added to the liquid, a small amount of solid was produced, and the liquid was obtained by filtration again;

[0026] (3) The above-mentioned 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 97%;

[0027] (4) Add 50g of adipic acid into the nitrilation reactor, and add...

Embodiment 2

[0029] (1) Add 0.5mol 1-methylimidazole to a three-necked flask, add 0.5mol diethyl phosphate dropwise, continue stirring for 1.5 hours after the addition, and react to obtain a colorless and transparent ionic liquid 1-methyl-3-ethane imidazole ethyl phosphate;

[0030] (2) Dissolve NaOH twice the number of moles of 1-methyl-3-ethylimidazolyl ethyl phosphate in ethanol, and add dropwise to the ethanol solution of 1-methyl-3-ethylimidazolium ethyl phosphate In the process, a white precipitate was produced, which was filtered to obtain a colorless transparent liquid, and equimolar phosphoric acid solution was added to the liquid, a small amount of solid was produced, and the liquid was obtained by filtration again;

[0031] (3) Evaporating the above liquid to remove water and alcohol, and then vacuum drying to obtain the product 1-methyl-3-ethylimidazolium ethyl phosphate, with a yield of 98%;

[0032] (4) Add 100g of adipic acid into the nitrilation reactor, and add 20mL of et...

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PUM

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Abstract

Belonging to the field of organic synthesis, the invention discloses a preparation method of adiponitrile. The specific steps include: (1) preparation of ethyl methylimidazole dihydrogen phosphate ionic liquid; and (2) application of the ethyl methylimidazole dihydrogen phosphate ionic liquid as a solvent and catalyst to the preparation process of adiponitrile by cyanation of adipic acid. The reaction time and temperature are reduced to certain extent, so that side reactions are decreased and the yield is increased.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of adiponitrile. Background technique [0002] Adiponitrile is a very important chemical intermediate, and its derivatives have a very wide range of uses. For example, one of its derivatives, hexamethylenediamine, is the basic raw material for the production of nylon 66, etc. [0003] The traditional method of producing adiponitrile from adipic acid used in industry is usually carboxylic acid ammonification method. The widely used process is to heat and dissolve carboxylic acid or its derivatives in an open system, and then continuously inject ammonia gas into the solution , so that the system reacts in the presence of catalysts such as phosphoric acid or phosphate. This process has problems such as high reaction temperature, long reaction time, and serious side reactions. [0004] Ionic liquids have many excellent properties. Many ionic liquids ...

Claims

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Application Information

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IPC IPC(8): C07C255/04C07C253/22C07C253/34
CPCC07C253/22C07C253/34C07C255/04Y02P20/54
Inventor 孙海龙
Owner SINOPEC YANGZI PETROCHEM
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