Preparation method of heterogeneous cyclohexanone oxime

A cyclohexanone oxime, heterogeneous technology, applied in oxime preparation, organic chemistry and other directions, can solve the problems of high operating cost, high energy consumption, low production capacity, etc., to reduce energy consumption, reduce impurity content, and ensure efficient utilization Effect

Pending Publication Date: 2019-06-28
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a low energy consumption, high production capacity, low cost heterogeneous Phase cyclohexanone oxime preparation method

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  • Preparation method of heterogeneous cyclohexanone oxime

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Embodiment 1

[0028] refer to figure 1 The shown process flow diagram of the present invention, a method for preparing heterogeneous cyclohexanone oxime, comprises the following steps:

[0029] (1) Ammoximation reaction

[0030] Add the titanium-silicon molecular sieve catalyst into the ammonia oximation reactor, add ammonia and hydrogen peroxide into the first-stage pipeline reactor, and add cyclohexanone into the second-level pipeline reactor. In the first-level pipeline reactor, ammonia and hydrogen peroxide are added to the catalyst Under the action of the reaction, hydroxylamine is first generated, and then reacts with the free cyclohexanone added from the secondary pipeline reactor, then circulates back to the reactor for further aging to generate cyclohexanone oxime, and obtains cyclohexanone oxime mainly containing cyclohexanone oxime, catalyst, water , a mixed solution of a small amount of ammonia; the temperature in the ammonia oximation reactor and the external circulation pipel...

Embodiment 2

[0040] refer to figure 1 The shown process flow diagram of the present invention, a method for preparing heterogeneous cyclohexanone oxime, comprises the following steps:

[0041] (1) Ammoximation reaction

[0042] The titanium-silicon molecular sieve catalyst is directly added to the ammonia oximation reactor, ammonia and hydrogen peroxide are added to the first-stage pipeline reactor, and cyclohexanone is added to the second-level pipeline reactor. In the first-level pipeline reactor, ammonia and hydrogen peroxide are Under the action of the catalyst, hydroxylamine is first generated, and then reacts with the free cyclohexanone added from the secondary pipeline reactor, then circulates back to the reactor for further aging to generate cyclohexanone oxime, and obtains cyclohexanone oxime mainly containing cyclohexanone oxime, catalyst, A mixed solution of water and a small amount of ammonia; the temperature in the ammonia oximation reactor and the external circulation pipeli...

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Abstract

The invention discloses a preparation method of heterogeneous cyclohexanone oxime. The method includes the following steps that ammonia and hydrogen peroxide react to generate hydroxylamine under theeffect of a catalyst, then the hydroxylamine reacts with cyclohexanone to generate cyclohexanone oxime, cyclohexanone oxime is extracted in an extraction phase to complete the separation of an organicphase and an inorganic phase, the extraction phase enters subsequent processes after filtering, and after being subjected to membrane separation, and extraction-phase catalyst slurry is returned to an ammoximation reaction kettle to participate in a catalytic reaction again. The ammoximation reaction is performed in a solvent-free state, the use of organic solvents is avoided, the energy consumption is low, there are fewer side reactions and fewer by products, and the subsequent refining process has small pressure. As there is no solvent, the reaction space is saved, and compared with the solvent-containing ammoximation reaction using the same device for production, the yield is improved. A hydroxylamine mechanism serves as a reaction mechanism, the conversion frequency of the hydroxylamine mechanism is about 2.5 times of that of an imine mechanism at 80 DEG C, and the conversion rate of cyclohexanone is high.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanone oxime, in particular to a method for preparing heterogeneous cyclohexanone oxime, belonging to the technical field of chemistry and chemical engineering. Background technique [0002] Cyclohexanone oxime is an important intermediate in the production of caprolactam. It is prepared by the ammoximation reaction of ammonia, hydrogen peroxide, and cyclohexanone. Cyclohexanone oxime is rearranged by Beckmann to obtain caprolactam. The preparation of cyclohexanone oxime by cyclohexanone ammoximation is a method commonly used in the caprolactam industry because of its simple preparation process, no by-product ammonium sulfate, no corrosion of pipelines, and environmental friendliness. At present, the production of cyclohexanone oxime by the cyclohexanone ammoximation method adopts a homogeneous reaction in the presence of an inert solvent such as tert-butanol. This reaction process has many and com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C249/14C07C251/44
Inventor 张玉新金作宏吴洪太高文杲王素霞
Owner 河北美邦工程科技股份有限公司
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