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Preparation method of cyclohexanone-oxime

A technology of cyclohexanone oxime and cyclohexanone amidoxime is applied in the field of preparation of cyclohexanone oxime, and can solve the loss of titanium silicon molecular sieve, low cyclohexanone conversion rate and cyclohexanone oxime selectivity, catalyst pore volume and ratio The effect of avoiding the loss of titanium-silicon molecular sieve, high cyclohexanone oxime selectivity, and high cyclohexanone conversion rate

Active Publication Date: 2013-09-11
BEIJING ENERGY ENG TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are following problems in these processes using shaped titanium-silicon molecular sieves: the formation of titanium-silicon molecular sieves and the use of binders in the molding process not only cause the loss of titanium-silicon molecular sieves, but also affect the pore volume and specific surface area of ​​the catalyst. influences
Yet, in the actual production process according to the method for this patent application, because resin content is too high (usually 50-99 weight %) in the catalyst bed layer, make the conversion rate of cyclohexanone and cyclohexanone in the ammoximation process of cyclohexanone Ketoximes are less selective

Method used

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  • Preparation method of cyclohexanone-oxime

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preparation example Construction

[0015] The preparation method of the cyclohexanone oxime according to the present invention comprises: under the cyclohexanone ammoximation reaction condition, make the reaction raw material that contains cyclohexanone, ammonia, hydrogen peroxide and solvent pass through the polyhedron in the fixed-bed reactor Each catalyst bed layer contains titanium silicate molecular sieve and resin, along the flow direction of the reaction raw material in the reactor, the content of the resin in the catalyst bed layer increases, and at least part of the catalyst The weight percentage of the resin in the bed layer is less than 50%.

[0016] According to a preferred embodiment of the present invention, along the flow direction of the reaction raw materials in the reactor, the total height of the catalyst bed with the weight percentage of the resin less than 50% is the total height of the catalyst bed. 5 to 90% of the height, more preferably 10 to 80%, even more preferably 20 to 60%.

[0017...

Embodiment 1

[0037] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.

[0038] (1) Preparation of composite catalyst

[0039] In the polymerization reactor, add Ti-MWW molecular sieve powder, styrene, divinylbenzene and gasoline, stir and mix evenly, when the water bath is heated to 60°C, add benzoyl peroxide, and react at 90°C for 6 hours to obtain The block composite catalyst is then crushed to obtain composite catalyst particles with a particle size of 1-3 mm, then added to 250 milliliters of 1,2-dichloroethane to swell, keep swelling for 5 hours at normal temperature, and then pour out 1 , 2-dichloroethane, and then add 200 ml of ethyl acetate for solvent extraction, the extraction temperature is 55 ° C, the extraction time is 4 hours, and the extraction is repeated three times to obtain a composite catalyst of titanium silicon molecular sieve and resin.

[0040] Composite catalysts A1-A3 of titanium-silicon molecular sieves...

Embodiment 2

[0061] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.

[0062] (1) Preparation of composite catalyst

[0063] In the polymerization reactor, add Ti-MWW molecular sieve powder, TS-1 titanium silicon molecular sieve powder, styrene, divinylbenzene and amyl alcohol, stir and mix evenly, when the water bath is heated to 60°C, add azobisisobutanol , reacted at 100°C for 6 hours to obtain a block composite catalyst, and then crushed to obtain composite catalyst particles with a particle size of 1-3 mm, and then added 250 ml of 1,2-dichloroethane to swell. Keep swelling for 5 hours, then pour out 1,2-dichloroethane, then add 200 milliliters of xylene to carry out solvent extraction, the extraction temperature is 55 ° C, the extraction time is 4 hours, and the extraction is repeated three times to obtain Composite catalyst of titanium silicate molecular sieve and resin.

[0064] Composite catalysts A4-A7 of titanium-sil...

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Abstract

The invention provides a preparation method of cyclohexanone-oxime, which is implemented in a way that: under reaction conditions of cyclohexanone ammoximation, a reaction raw material containing cyclohexanone, ammonia, hydrogen peroxide and solvent passes through a plurality of catalyst bed layers in a fixed-bed reactor; each catalyst bed layer contains a titanium-silicon molecular sieve and resin; in the flow direction of the reaction raw material in the reactor, the resin content in the catalyst bed layer increases progressively; and the weight percent of at least part of resin in the catalyst bed layer is less than 50%. The preparation method provided by the invention can obtain higher cyclohexanone conversion rate and cyclohexanone-oxime selectivity.

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. [0003] Since titanium-silicon molecular sieve catalysts play a very important role in the selective oxidation of organic compounds, as a preparation method for cyclohexanone oxime, it has been proposed to use hydrogen peroxide and ammonia to react cyclohexanone oxime in the presence of titanium-silicon molecular sieve catalysts. A method for ammoximation of ketones. The advantage of this method is that it does not need to use ammonia to neutralize sulfuric acid like the previous method of oximation with hydroxylamine sulfate. [0004] In the process of cyclohexanone ammoximation to prepare cyclohexanone oxime, titanium-silicon...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/04B01J31/38
Inventor 曲良龙董维正王月金芃澔南方陈健
Owner BEIJING ENERGY ENG TECH
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