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Preparation method of cyclohexanone-oxime

A technology of cyclohexanone oxime and cyclohexanone, which is applied in the field of preparation of cyclohexanone oxime, can solve the problems of low conversion rate of cyclohexanone oxime, low selectivity of cyclohexanone oxime, difficulty in separation of oximation catalyst, etc.

Active Publication Date: 2013-11-06
杭州怡鸿化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects that the oximation catalyst existing in the preparation method of cyclohexanone oxime is difficult to separate, and the conversion rate of cyclohexanone and the selectivity of cyclohexanone oxime are low, and provide a A new preparation method of cyclohexanone oxime, which not only facilitates the separation of oximation catalyst, but also can improve the conversion rate of cyclohexanone and the selectivity of cyclohexanone oxime

Method used

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  • Preparation method of cyclohexanone-oxime
  • Preparation method of cyclohexanone-oxime

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preparation example Construction

[0012] The preparation method of cyclohexanone oxime provided by the present invention comprises, under the presence of oximation catalyst and water, make cyclohexanone, ammonia and hydrogen peroxide contact reaction in organic solvent, wherein, described organic solvent is low carbon alkane and The mixed solvent of low carbon alcohol, described low carbon alkane is C 3 -C 10 Alkanes, the lower alcohols are C 3 -C 10 alcohol.

[0013] According to the present invention, although as long as C 3 -C 10 Alkanes and C 3 -C 10 The mixed solvent of alcohol is used as an organic solvent, which can improve the conversion rate of cyclohexanone and the selectivity of cyclohexanone oxime and promote the separation of the oximation catalyst, but in order to obtain better comprehensive effects, preferably, the low Carbon alkane is C 5 -C 10 Alkanes, the lower alcohols are C 3 -C 8 alcohol.

[0014] The present invention is not particularly limited to the amount of the lower alka...

Embodiment 1

[0036] This example is used to illustrate the preparation method of cyclohexanone oxime provided by the present invention.

[0037] Mix n-heptanol and n-hexane evenly at a weight ratio of 9:1 to obtain a composite solvent for later use.

[0038] according to figure 1 The method shown prepares cyclohexanone oxime. Continuously feed cyclohexanone, ammonia, hydrogen peroxide (concentration: 27.5% by weight), composite solvent and oximation catalyst TS-1 into the ammoximation reactor, wherein the flow rates of the above-mentioned materials are 10920kg / h, 2012kg / h, 15127kg / h, 33000kg / h and 2500kg / h. The temperature of the reaction system is controlled at 80-90° C., and the pressure is controlled at 0.35-0.4 MPa. The residence time of the material in the ammoximation reactor was 1.2 hours, and a reaction product containing oximation catalyst TS-1 was obtained. The resulting reaction product containing the oximation catalyst TS-1 is continuously introduced into a decanter for se...

Embodiment 2

[0041] This example is used to illustrate the preparation method of cyclohexanone oxime provided by the present invention.

[0042] Mix iso-octanol and n-octane evenly in a weight ratio of 3:2 to obtain a composite solvent for future use.

[0043] according to figure 1 The method shown prepares cyclohexanone oxime. Continuously feed cyclohexanone, ammonia, hydrogen peroxide (concentration: 27.5% by weight), composite solvent and oximation catalyst TS-1 into the ammoximation reactor, wherein the flow rates of the above-mentioned materials are 10920kg / h, 2012kg / h, 15127kg / h, 33000kg / h and 2500kg / h. The temperature of the reaction system is controlled at 77-85° C., and the pressure is controlled at 0.3-0.35 MPa. The residence time of the material in the ammoximation reactor was 1.5 hours, and a reaction product containing oximation catalyst TS-1 was obtained. The resulting reaction product containing the oximation catalyst TS-1 is continuously introduced into a decanter for ...

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Abstract

The invention provides a preparation method of cyclohexanone-oxime. According to the method, cyclohexanone, ammonia and hydrogen peroxide undergo a contact reaction in an organic solvent in the presence of an oximation catalyst and water, wherein the organic solvent is a mixed solvent of light alkane and lower alcohol; the light alkane is C3-C10 alkane; and the lower alcohol is C3-C10 alcohol. By the adoption of the preparation method to prepare cyclohexanone-oxime, high conversion rate of cyclohexanone and selectivity of cyclohexanone-oxime can be obtained, oximation catalyst is separated from a product containing cyclohexanone-oxime without membrane separation. Thus, recycling of the oximation catalyst is realized. The preparation method has an industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of cyclohexanone oxime. Background technique [0002] Cyclohexanone oxime is a key intermediate for the synthesis of caprolactam and an important chemical raw material, mainly used as a raw material for the preparation of nylon 6 monomer for fiber nylon 6 and engineering plastics. At present, there are four main methods for the preparation of cyclohexanone oxime: HSO method (hydroxylamine sulfate method), HPO method (hydroxylamine phosphate method), NO reduction method and ammonia oximation method. Compared with the other three methods, the ammoximation method is relatively simple and does not produce ammonium sulfate by-product, so it has recently received more and more attention from the caprolactam industry. At present, the vast majority of domestic preparations of caprolactam choose the ammonia oximation method. Specifically, in the presence of an oximation catalyst and water, cyclohexanone, ammonia an...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/04
CPCY02P20/584
Inventor 赵承军赵云
Owner 杭州怡鸿化工科技有限公司