Preparation method of cyclohexanone-oxime

A technology of cyclohexanone oxime and cyclohexanone amidoxime, which is applied in the field of preparation of cyclohexanone oxime, can solve the loss of titanium silicon molecular sieve, the influence of catalyst pore volume and specific surface area, the conversion rate of cyclohexanone oxime and the selection of cyclohexanone oxime To solve the problems of low cyclohexanone oxime, high cyclohexanone oxime selectivity, improving cyclohexanone conversion rate and cyclohexanone oxime selectivity

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 example Construction

[0016] 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-silicon molecular sieve and resin, and the titanium-silicon molecular sieve contains Ti-MWW-F molecular sieve, along the flow direction of the reaction raw material in the reactor, in the catalyst bed layer The content of the resin is increasing, and the weight percentage of the resin in at least part of the catalyst bed is less than 50%.

[0017] In the present invention, the titanium-silicon molecular sieve may be entirely composed of Ti-MWW-F molecular sieves, or may contain other titanium-silicon molecular sieves conventionally used in the field. Containing Ti-MWW-F molecular sieve can further improve the conversion rate of c...

Embodiment 1

[0051] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.

[0052] (1) Preparation of composite catalyst

[0053] In the polymerization reactor, add Ti-MWW-F molecular sieve, 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, Obtain block composite catalyst, then crush to obtain composite catalyst microparticles with a particle size of 1-3 mm, then add 250 ml of 1,2-dichloroethane to swell, keep swelling at normal temperature for 5 hours, then pour out 1,2-dichloroethane, 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 .

[0054] Composite catalysts A1-A4 of titanium-silicon molecular sieves and resins were prepared accord...

Embodiment 2

[0072] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.

[0073] (1) Preparation of composite catalyst

[0074] According to the method of step (1) of Example 1, the difference is that the composite catalysts B1-B8 are prepared, and the feeding amount of materials in each preparation process is shown in Table 2 below.

[0075] Table 2

[0076]

[0077] (2) Preparation of cyclohexanone oxime

[0078] According to the order of composite catalyst B8 to composite catalyst B1, the composite catalyst that step (1) obtains is packed in diameter and is 20 millimeters, and length is in the fixed-bed reactor of 1200 millimeters, and total filling volume is 50 milliliters, and each The packing heights of the composite catalysts are the same. Then, the reaction raw material (made up of cyclohexanone, hydrogen peroxide, ammonia and water) is injected in the fixed bed reactor, makes the reaction raw material flow along the ...

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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; the titanium-silicon molecular sieve contains a Ti-MWW-F molecular sieve; 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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Patent Type & Authority Applications(China)
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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