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Preparation process of cyclohexanone-oxime

A technology for the preparation of cyclohexanone oxime, which is applied in oxime preparation, chemical recovery, organic chemistry, etc., can solve the problems of increased energy consumption, and achieve the effects of reduced consumption, high quality, and low energy consumption

Inactive Publication Date: 2010-07-21
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in order to obtain 99.975% cyclohexanone oxime in the industry, it is necessary to design a deketone and alcohol removal tower to remove residual ketones and alcohols, resulting in an increase in energy consumption

Method used

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  • Preparation process of cyclohexanone-oxime
  • Preparation process of cyclohexanone-oxime

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: as figure 1 Shown, technological process of the present invention comprises the steps:

[0024] a.10920kg / h cyclohexanone, 2012kg / h ammonia, 15127kg / h 27.5% hydrogen peroxide enter the ammoximation reactor at the same time, in the presence of molecular sieve catalyst TS-1 and solvent tert-butanol (TBA) and 80~90℃ , Under the condition of 0.4~0.6Mpa, ammoximation reaction occurs;

[0025] b. When the conversion rate of cyclohexanone in the above reaction is 99.5%, it is separated by filtration, wherein the catalyst separated by filtration returns to the ammoximation reactor and continues to be used as catalyst recycling, and the filtrate separated by filtration goes to the tert-butanol distillation tower for distillation. The solvent tert-butanol that goes out is returned to the ammoximation reactor and continues to be used as a reaction solvent for recycling;

[0026] c. the mixed solution of cyclohexanone / cyclohexanone oxime / water coming out from the bo...

Embodiment 2

[0030] Embodiment 2: the difference between this embodiment and embodiment 1 is that the cyclohexane extractant is replaced by n-hexane extractant.

Embodiment 3

[0031] Embodiment 3: The difference between this embodiment and Example 1 is that the 13.8% hydroxylamine phosphate of 457kg / h is used to replace the 19.7% hydroxylammonium sulfate of 457kg / h during the second step oximation, obtained after ammonia neutralization and separation The salt-containing heavy phase is sent to hydroxylamine to prepare and recover phosphate.

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Abstract

The invention discloses a preparation process of cyclohexanone-oxime. The process comprises the following steps: carrying out ammoximation under the condition of the existence of catalyst and tertiary butanol solvent, and filtering, distilling and leaching when the conversion ratio of cyclohexanone is 99.5% in the ammoximation; then adding hydroxylamine for performing oximation reaction; and finally neutralizing and filtering to obtain the cyclohexanone-oxime solution when the conversion ratio of the cyclohexanone is 100%. The process combines two different kinds of the oximation reactions to ensure that the conversion ratio of the cyclohexanone reaches to 100%, solves the defect that the cyclohexanone can not be fully converted in the existing ammoximation process, reduces the consumption of hydrogen peroxide and eliminates safety hidden troubles brought by excessive hydrogen peroxide. Compared with the traditional process, the process of the invention abrogates working procedures such as regenerating extractant by rectification, removing ketone, dealcoholization tower, regenerating cyclohexanone-oxime by rectification and the like, saves equipment investment and reduces energy consumption; and as for a device by which the annual cyclohexanone-oxime yield is 100,000 tons, the saved equipment investment is close to ** million yuan, and the saved energy sources such as water, electricity, steam and the like are close to ** yuan.

Description

technical field [0001] The invention relates to a preparation process of cyclohexanone oxime, further comprising preparing cyclohexanone oxime through two-step oximation reaction and extraction with an inert solvent. Background technique [0002] Cyclohexanone oxime is an important intermediate for the preparation of caprolactam. At present, the processes for preparing cyclohexanone oxime in the world mainly include HSO method (hydroxylamine sulfate method), HPO method (hydroxylamine phosphate method), NO reduction method and ammonia oximation method. [0003] The NO reduction method and the HSO method are used less and less because of the by-product of low-value ammonium sulfate; the HPO method is not favored because the process is too complicated and the operation is difficult. Only the ammoximation method is more and more popular because of its simple process, no by-product ammonium sulfate, and easy operation. [0004] But the ammoximation method also has a fatal short...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/04C07C249/08
CPCY02P20/584
Inventor 赵承军张玉新王素霞
Owner 河北美邦工程科技股份有限公司
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