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Method and device for preparing caprolactam through cyclohexanone oxime rearrangement reaction

A technology of cyclohexanone oxime and rearrangement reaction is applied in the field of chemical product production to achieve the effects of high energy efficiency, improved mass transfer and optimized reaction conditions

Active Publication Date: 2015-04-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the application of high gravity technology to the rearrangement reaction of cyclohexanone oxime to prepare caprolactam.

Method used

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  • Method and device for preparing caprolactam through cyclohexanone oxime rearrangement reaction
  • Method and device for preparing caprolactam through cyclohexanone oxime rearrangement reaction
  • Method and device for preparing caprolactam through cyclohexanone oxime rearrangement reaction

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Experimental program
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Effect test

Embodiment 1

[0025] The hot solvent is chloroform, the cyclohexanone oxime, chloroform, and the amidation liquid containing concentrated sulfuric acid or fuming sulfuric acid enter the cyclohexanone oxime inlet 11, the hot solvent inlet 10 and the amidation liquid inlet 14 respectively into the third The liquid phase mixer 5 performs mixing, and then enters the supergravity reactor 8 to continue mixing. The volume ratio of chloroform and cyclohexanone oxime is 6:1, the acid oxime ratio of the mixed liquid after mixing is 1.3:1 (molar ratio), the rotor speed of the supergravity reactor is 2000 rpm, and the mixing temperature is 65°C. The mixed liquid passes through the supergravity reactor liquid outlet 3 to the subsequent rearrangement reactor 13 for further rearrangement reaction. The rearrangement reaction temperature is 71°C, the system pressure is 0.04MPa, and the subsequent rearrangement reaction stirrer revolutions is 500 Rpm. The materials leaving the subsequent rearrangement react...

Embodiment 2

[0027] The hot solvent is heptane, the volume ratio of heptane to cyclohexanone oxime is 10:1, the acid oxime molar ratio of the mixed solution after mixing is 0.9:1, and the rotor speed of the high gravity reactor 8 is 500 rpm , The mixing temperature is 70℃. The material leaving the supergravity reactor enters the subsequent rearrangement reactor 13 for further rearrangement reaction, the reaction temperature is 110°C, and the pressure is 0.25Mpa. The materials leaving the subsequent rearrangement reactor undergo crystallization, neutralization, extraction and purification processes to obtain caprolactam. The conversion rate of cyclohexanone oxime was 90%, and the selectivity of caprolactam was 88.7%.

Embodiment 3

[0029] The hot solvent is petroleum ether, the volume ratio of petroleum ether to cyclohexanone oxime is 18:1, the molar ratio of acid oxime is 1.2:1, the speed of the rotor of the supergravity reactor is 1200 rpm, and the mixing temperature is 65°C . The materials leaving the supergravity reactor flow into the subsequent rearrangement reactor 13 for further rearrangement reaction, the reaction temperature is 65°C, and the system pressure is 0.001Mpa. The materials leaving the subsequent rearrangement reactor undergo crystallization, neutralization, extraction and purification processes to obtain caprolactam. The conversion rate of cyclohexanone oxime was 100%, and the selectivity of caprolactam was 99.8%.

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Abstract

The invention relates to a method and a device for preparing caprolactam through a cyclohexanone oxime rearrangement reaction. The device comprises a three liquid phase mixer, a hypergravity reactor, and a subsequent rearrangement reactor. The preparation process comprises the steps that: cyclohexanone oxime, a heat extraction solvent, and a amidation solution are mixed in the three liquid phase mixer, wherein a mixing temperature is 40-80 DEG C, a volume ratio of the heat extraction solvent to cyclohexanone oxime is 5-20:1, and an acid-oxime molar ratio is 0.6-2.0:1. The mixed liquid is mixed and is subjected to a reaction in the hypergravity reactor; a mixed material left the hypergravity reactor is subjected to a further rearrangement reaction in the subsequent rearrangement reactor, wherein a reaction temperature is 60-120 DEG C and a reaction pressure is 0-0.3MPa; and a reaction product is subjected to processes of crystallization, neutralization, extraction, and refining, such that caprolactam is prepared. According to the invention, the three liquid phase mixer, the hypergravity reactor, and the subsequent rearrangement reactor are combined, such that mixing and reaction processes are reinforced, and cyclohexanone oxime conversion rate and caprolactam selectivity are improved.

Description

technical field [0001] The invention belongs to the technical field of chemical product production, and relates to a production technology of caprolactam, in particular to a method and a device for preparing caprolactam through a rearrangement reaction of cyclohexanone oxime that utilizes supergravity technology to strengthen the reaction process. Background technique [0002] Caprolactam (CPL) is an important organic chemical raw material, mainly used in the production of nylon-6 fiber and engineering plastics. More than 90% of caprolactam in the world is produced by cyclohexanone-hydroxylamine method. The cyclohexanone-hydroxylamine method is used to produce caprolactam. First, cyclohexanone and hydroxylamine are subjected to oximation reaction to produce cyclohexanone oxime, and then cyclohexanone oxime is subjected to liquid-phase Bekman rearrangement reaction to obtain caprolactam. The Bekman rearrangement of cyclohexanone oxime is a crucial process step and plays a k...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10C07D201/04
CPCY02P20/30
Inventor 潘九海陈建峰王志侃初广文杨根柱邹海魁王仲霞陈春凤冯建松
Owner CHINA PETROLEUM & CHEM CORP