Production of hexyl lactam in ion liquid

A technology of ionic liquid and caprolactam, which is applied in the field of preparation of caprolactam, to achieve the effect of reducing production cost, reducing loss and realizing the control of reaction rate

Active Publication Date: 2006-05-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to address the above-mentioned problems faced by the current development of ammonium sulfate-free by-product rearrangement technology, and propose a method for preparing caprolactam by liquid-phase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] This embodiment illustrates that the present invention can be used in [bmim]BF 4 The rearrangement was carried out in a biphasic system with / toluene.

[0033] Add hydrophilic [bmim]BF to a 100ml round bottom flask 4 12.0ml of ionic liquid, 24.0ml of toluene and 6.0ml of acetic anhydride, temperature controlled oil bath at 70°C, magnetic stirring, 15.0ml of 2.0mol / L cyclohexanone oxime-toluene solution was added dropwise, reacted for 5.0min, static phase separation. The ionic liquid phase is diluted with water and then extracted with chloroform, the relative content of each substance in the toluene phase and the chloroform extract is analyzed by gas chromatography, and the absolute amount of caprolactam in the organic phase is determined by internal standard method. The conversion rate of cyclohexanone oxime is 100.0%, the selectivity of caprolactam is 94.6%, the total selectivity of caprolactam and cyclohexanone is 97.7%, 22.5% of caprolactam is in the toluene phase, ...

Embodiment 2

[0035] This example illustrates that the present invention can be used in [emim]BF 4 / Benzene two-phase system implementation.

[0036] Add hydrophilic [emim]BF to a 100ml round bottom flask 4 8.0ml of ionic liquid, 4.0ml of toluene, and 4.0ml of acetic anhydride were added in an oil bath at 80°C with magnetic stirring, and 30ml of 0.20mol / L cyclohexanone oxime-toluene solution was added dropwise, reacted for 10.0min, and then separated into phases. The conversion rate of cyclohexanone oxime was 100.0%, and the selectivity of caprolactam was 88.4%.

Embodiment 3

[0038] This example illustrates that the present invention can be used in [bupy]BF 4 / xylene two-phase system.

[0039] Add hydrophilic [bupy]BF to a 100ml round bottom flask 4 8.0ml of ionic liquid, 40.0ml of xylene and 4.0ml of acetic anhydride were added dropwise in an oil bath at 70°C with magnetic stirring, and 10.0ml of 2.0mol / L cyclohexanone oxime-xylene solution was added dropwise, reacted for 15.0min, and then separated into phases. The conversion rate of cyclohexanone oxime was 100.0%, and the selectivity of caprolactam was 82.7%.

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Abstract

Production of caprolactam in ion liquid is carried out by Beckmann rearrangement reacting of cyclohexanone-oxime in ion liquid and organic solvent two-phase system, extracting ion liquid by organic solvent, transferring caprolactam into organic solvent, separating caprolactam from catalyst by solvent extraction. It has higher conversion rate and selectivity, no by products and circulating use.

Description

technical field [0001] The invention relates to a method for preparing caprolactam in ionic liquid. Specifically, it relates to a method for preparing caprolactam through liquid-phase Beckmann rearrangement reaction of cyclohexanone oxime in the presence of ionic liquid. Background technique [0002] Caprolactam is an important organic chemical raw material with wide application. About 90% of caprolactam in the world is prepared from cyclohexanone oxime through Beckmann rearrangement reaction. The traditional Beckmann rearrangement reaction process is: use fuming sulfuric acid to make cyclohexanone oxime form caprolactam salt of sulfuric acid, and in order to obtain a high yield of caprolactam, it is necessary to add excess sulfuric acid, and then neutralize the mixture with ammonia water to obtain ammonium sulfate and caprolactam . In a typical industrial rearrangement process, the conversion of cyclohexanone oxime is almost 100%, and the selectivity to caprolactam is 99%...

Claims

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Application Information

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IPC IPC(8): C07D223/10C07D201/04
CPCY02P20/52
Inventor 张伟吴巍胡合新闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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