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Application of alkyl quaternary phosphonium salt ionic liquid in adipic acid synthesis of adiponitrile

An ionic liquid and adiponitrile technology, which is applied in the field of adiponitrile synthesis, can solve the problems of reactor corrosion, difficulty in industrialization, and increase in production costs, and achieve the effects of reducing corrosion, strong complexation ability, and reducing impact

Active Publication Date: 2020-04-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst faces a series of problems: firstly, a large amount of phosphoric acid and phosphoric acid ester will cause certain corrosion to the reactor and affect normal production; secondly, this type of liquid catalyst is easily soluble in the reaction system, causing catalyst loss and increasing Production cost; finally, phosphoric acid, etc. will generate polymers in the reaction, affecting heat transfer
It is reported in the literature that ethylmethylimidazolium dihydrogen phosphate ionic liquid is used in the nitrilation of adipic acid to prepare adiponitrile. The author conducts discontinuous reaction through the reactor and feeds ammonia gas in batches at the same time. The operation steps are complicated and are not conducive to scale-up. Production, difficult to achieve industrialization (CN 201710540292.1)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0024] Synthesis of ionic liquid 1,3-dimethylimidazole methyl phosphate salt: under the protection of high-purity nitrogen, N-methylimidazole and trimethyl phosphate were mixed at a ratio of 1:12, and microwave (heating power: 2kW h) was heated to reflux After reacting for 1 h, microwave, wash with ether three times, distill off the residual ether under reduced pressure, and dry to obtain the product.

Embodiment 2

[0026] Synthesis of ionic liquid morpholine methyl phosphate salt: under the protection of high-purity nitrogen, mix morpholine and trimethyl phosphate at a ratio of 1:12, heat and reflux with microwave (heating power 2kW·h) for 1h, and wash with ether for 3 times , The remaining ether was distilled off under reduced pressure, and the product was obtained after drying.

Embodiment 3

[0028] Synthesis of ionic liquid N-methylmorpholine methyl phosphate salt: under the protection of high-purity nitrogen, N-methylmorpholine and trimethyl phosphate were mixed at a ratio of 1:12, and microwave (heating power: 2kW·h) was heated to reflux reaction After 1h, wash with ether three times, distill off residual ether under reduced pressure, and obtain the product after drying.

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PUM

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Abstract

The invention provides an application of alkyl quaternary phosphonium salt ionic liquid in adipic acid synthesis of adiponitrile. The alkyl quaternary phosphonium salt ionic liquid is prepared from alkyl quaternary phosphonium salt through alkylation reaction and a corresponding imidazole and phosphate one-step method, at a certain temperature, an ionic liquid catalyst, adipic acid and adiponitrile are added into a reaction kettle, excessive ammonia gas is introduced, reaction is performed for a certain period of time, and the product adiponitrile is obtained. The method for synthesizing the ionic liquid is simple, and the operation process is convenient. The prepared ionic liquid is not easy to volatilize, difficult to oxidize and easy to recycle; the ionic liquid has relatively high polarity and strong complexing power; anions and cations can be freely combined, and the structure is easy to control; and the ionic liquid is not flammable or combustible and has relatively high thermalstability.

Description

technical field [0001] The invention belongs to the technical field of adiponitrile synthesis, and in particular relates to the application of a plasma-modified alkyl quaternary phosphonium salt ionic liquid in the synthesis of adiponitrile from adipic acid and ammonia. Background technique [0002] As an important chemical raw material, adiponitrile can react with hydrogen to form hexamethylenediamine, and hexamethylenediamine and adipic acid react under strict material ratio to form nylon 66 salt. Therefore, adiponitrile, as an important intermediate in the synthesis of nylon 66, is the most important and most valuable industrial use of adiponitrile. [0003] At present, the methods for synthesizing adiponitrile mainly include electrolytic dimerization of acrylonitrile (AN), butadiene (BD) and catalytic amination of adipic acid (ADA). Among them, the adipic acid ammonification method is the first industrialized method for the synthesis of adiponitrile. At present, the met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/22C07C255/04B01J31/02
CPCB01J31/0282B01J31/0284B01J31/0298C07C253/22C07C255/04
Inventor 黄家辉张少华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI