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A kind of preparation method of cyclohexanone oxime

A technology of cyclohexanone oxime and cyclohexanone, applied in the field of preparation of cyclohexanone oxime, can solve the problem of low cyclohexanone conversion rate and cyclohexanone oxime selectivity

Active Publication Date: 2018-09-28
HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD
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Problems solved by technology

[0005] The purpose of the present invention is to provide a new cyclohexanone oxime in order to overcome the shortcomings of the conversion rate of cyclohexanone and the low selectivity of cyclohexanone oxime when the existing ammoximation reaction is used to prepare cyclohexanone oxime. The preparation method of ketoxime

Method used

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  • A kind of preparation method of cyclohexanone oxime
  • A kind of preparation method of cyclohexanone oxime
  • A kind of preparation method of cyclohexanone oxime

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preparation example Construction

[0013] The preparation method of cyclohexanone oxime provided by the present invention comprises that in the presence of an oximation catalyst, cyclohexanone, ammonia and hydrogen peroxide are subjected to an ammoximation reaction in a solvent, wherein the solvent contains a small amount of an inert organic solvent of aqueous solution.

[0014] In the present invention, the aqueous solution containing a small amount of inert organic solvent means that the content of a small amount of inert organic solvent in the aqueous solution is not higher than 30% by weight based on the total weight of the aqueous solution.

[0015] According to the preparation method of cyclohexanone oxime provided by the present invention, the addition of an inert organic solvent in the ammoximation reaction system can improve the mass transfer and heterogeneous phase separation effect of the reaction system, thereby obtaining a higher reaction yield and subsequent suspension liquid separation efficiency...

specific Embodiment approach

[0027] According to a specific embodiment of the present invention, the preparation method of cyclohexanone oxime comprises sending cyclohexanone, ammonia, hydrogen peroxide, an inert organic solvent, additionally added water and an oximation catalyst into an ammoximation reactor for Ammoximation reaction, and the reaction product is extracted with the above-mentioned inert organic solvent, and then sent to a cyclone separator and a decanter for separation to obtain the oil phase containing cyclohexanone oxime and the water containing oximation catalyst and water phase, and the aqueous phase containing the oximation catalyst and water is returned to the ammoximation reactor to continue the ammoximation reaction.

[0028] The present invention will be described in detail below by way of examples.

[0029] In the following examples and comparative examples:

[0030] The oximation catalyst is a titanium-silicon molecular sieve (TS-1) catalyst, which is according to the document ...

Embodiment 1

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

[0037] The volume ratio of toluene to cyclohexanone in the mixed solution of cyclohexanone and toluene used in this embodiment is 5:100. First, add 100.00g of water and 3.00g of oximation catalyst (TS-1) into the glass reactor with stirring, then pass the mixture of cyclohexanone and toluene, ammonia and hydrogen peroxide (concentration is 27.5% by weight) through advection pump Continuously sent into the glass reactor, wherein, the flow rate of the above-mentioned several kinds of materials is 10.50g / h, 1.99g / h, 14.89g / h successively. The temperature of the reaction system is controlled at 86-90° C. and the pressure is controlled at 0.3-0.4 MPa. After the materials stay in the glass reactor for 70 minutes, a reaction product containing cyclohexanone oxime and an oximation catalyst (TS-1) is obtained. Then the obtained reaction product containing cycloh...

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Abstract

The invention provides a preparation method of cyclohexanone-oxime. In the method, in the presence of an oximation catalyst, cyclohexanone, ammonia and hydrogen peroxide are subjected to an ammoximation reaction in a solvent which is a water solution containing less amount of an inert organic solvent. The method is high in conversion rate of cyclohexanone and selectivity on cyclohexanone-oxime, is beneficial to subsequent treatment of products, and has great industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of cyclohexanone oxime. Background technique [0002] As an intermediate in the synthesis of caprolactam, cyclohexanone oxime is an important chemical raw material for the production of nylon-6 chips, nylon fibers, engineering plastics and plastic films. There are four main methods for preparing cyclohexanone oxime at home and abroad: hydroxylamine sulfate method (HSO method), nitric oxide reduction method (NO method), hydroxylamine phosphate method (HPO method) and ammonia oximation method. However, in view of the purpose of reducing equipment investment scale, improving safety and environmental protection, and saving energy and reducing consumption, among the current industrialized methods, there are very few manufacturers of HSO method, NO method and HPO method, and most manufacturers prefer the ammoximation method. The ammoximation method has mild reaction conditions, high yield, short production proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/44C07C249/04
CPCY02P20/584
Inventor 罗和安赵承军陈浩吴剑雷锋胜任成韵赵云
Owner HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD
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