Ammoximation reaction and separation coupling process and device

An ammoximation reaction and process technology, applied in oxime preparation, organic chemistry, etc., can solve the problems of easy short circuit of reaction materials, degradation of catalyst performance, low reaction conversion rate, etc., to reduce energy consumption, simplify internal structure, and improve reaction efficiency. The effect of process safety

Active Publication Date: 2015-01-07
河北美邦工程科技股份有限公司
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Problems solved by technology

The disadvantage of this method is that the reaction feed liquid needs to be transported to the outside of the reactor, resulting in increased energy consumption. During the transport of the catalyst, the shear of the pump will cause the catalyst to wear, resulting in a decline in catalyst performance and catalyst loss.
Another ammoximation reaction separation process is that the filter is in the reactor, and the cyclohexanone ammoximation is reacting while the reaction product is separated from the catalyst. The biggest disadvantage of this separation method is that the reaction material is easy to short circuit. Some reaction raw materials are removed from the reactor together with the reaction product without reaction, resulting in low reaction conversion rate and serious back-mixing in the reactor.

Method used

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  • Ammoximation reaction and separation coupling process and device

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Embodiment 1

[0030] see figure 1 The installation schematic diagram of the ammoximation reaction and separation device of the present invention provided, the process of the present invention comprises the following steps:

[0031] (1) Add raw materials to reactor 1 in molar ratio (1~2):(1~2):1:(3~3.5)

[0032] Ammonia gas A, hydrogen peroxide B, cyclohexanone C, solvent tert-butanol D and appropriate amount of catalyst titanium-silicon molecular sieve E, adjust the temperature in the reactor 1 to 75-95°C, the pressure to 0.3-0.6Mpa, and establish a cycle;

[0033] (2) Control the temperature and pressure of the reactor 1 to meet the above conditions, continuously add the catalyst titanium silicon molecular sieve E to the reactor 1, and react the materials. On the external pipeline of the reactor 1, the raw material ammonia A and hydrogen peroxide B continuously enter the pipeline reactor 5, the raw material cyclohexanone C and the solvent tert-butanol D continuously enter the pipeline rea...

Embodiment 2

[0041] The difference between embodiment 2 and embodiment 1 is that a group of pipeline reactors 5 continuously add raw materials cyclohexanone C and solvent tert-butanol D, and two groups of pipeline reactors 6 continuously use raw materials ammonia gas A and hydrogen peroxide B. to join.

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Abstract

The invention discloses an ammoximation reaction and separation coupling process which comprises the following steps: continuously adding reaction raw materials and a solvent in different groups outside a reaction kettle into a pipeline reactor for reaction, mixing the components in a mixer, and subsequently feeding the mixture into the reaction kettle for sufficient reaction, wherein the upper part of the reaction kettle is a reaction zone, and the lower part of the reaction kettle is a filtration separation zone; separating a reaction product, namely, cyclohexanone-oxime from a catalyst in the filtration separation zone, feeding the separated cyclohexanone-oxime into a later process, and circulating the catalyst back to the reaction kettle for continuous reaction through equipment such as the pipeline reactor outside the reaction kettle. Backwashing is performed once every 10-300 seconds, so that the continuity of reaction separation is ensured. As the raw materials sufficiently contact the catalyst, the reaction is complete, and the conversion rate of cyclohexanone can be 99.9-100%. The whole set of reaction separation devices is reasonable in arrangement and stable in reaction.

Description

technical field [0001] The invention relates to an ammoximation reaction process, in particular to a reaction and separation coupling process for preparing cyclohexanone oxime by ammoximation. Background technique [0002] Cyclohexanone oxime is an important raw material for the preparation of caprolactam. The processes for preparing cyclohexanone oxime mainly include HSO method (hydroxylamine sulfate method), HPO method (hydroxylamine phosphate method), NO reduction method and ammoximation method. The NO reduction method and the HSO method are less and less used due to the low value of the by-products; the HPO method is gradually replaced by the cyclohexanone ammoximation method in industrial production due to its complicated process and difficult operation. The cyclohexanone ammoximation process has more and more industrial applications due to its simple process, easy operation and few by-products. The cyclohexanone ammoximation method refers to the reaction of cyclohexa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44
Inventor 高文杲宛捍东金作宏王海东张玉新王富民
Owner 河北美邦工程科技股份有限公司
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