Method for preparing cyclohexanone-oxime from cyclohexanone ammoximation

A technology for cyclohexanone amidoxime and cyclohexanone oxime, which is applied in the field of preparing cyclohexanone oxime by ammoximation of cyclohexanone, can solve the problems of easy clogging of catalyst and poor separation effect, and achieves the effect of solving the separation problem

Inactive Publication Date: 2013-10-23
WUHAN YOULIKE NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] In order to avoid the separation problem, the titanium-silicon molecular sieve catalyst can be prepared into particles with an average diameter of 10-50 microns, which can ensure high mechanical strength and avoid diffusion restrictions; at the same time, an external sintered filter for separating the reactant from the catalyst can be installed to solve the problem. The separation effect is not good, the catalyst is easy to clog and other problems

Method used

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  • Method for preparing cyclohexanone-oxime from cyclohexanone ammoximation
  • Method for preparing cyclohexanone-oxime from cyclohexanone ammoximation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] For the reaction process, see figure 1 , the specific feed parameters and material settlement conditions are as follows:

[0054] Cyclohexanone = 160.0 g / h

[0055] tert-butanol = 781.0 g / h

[0056] 30% by weight hydrogen peroxide = 194.3 g / h

[0057] Liquid ammonia = 60.9 g / h

[0058] Titanium silicon molecular sieve concentration = 2.0% by weight

[0059] The average residence time of materials in the reactor is 75 minutes, the reaction temperature is maintained at 83±1°C through jacket heat exchange, and the reaction pressure is maintained at 0.3MPa.

[0060] Maintain the temperature of the reaction product material entering the settler at 70°C, filter in a sintered filter, and backwash once every 20 seconds.

[0061] Its reaction result is as follows:

[0062] Cyclohexanone conversion rate: 97.5%

[0063] Conversion rate of hydrogen peroxide: 100%

[0064] Reaction selectivity based on cyclohexanone: 98.5%

[0065] Effective utilization rate of hydrogen per...

Embodiment 2

[0069] For the reaction process, see figure 1 , the specific feed parameters and material settlement conditions are as follows:

[0070] Cyclohexanone = 196.0 g / h

[0071] tert-butanol = 850.0 g / h

[0072] 30% by weight hydrogen peroxide = 249.3 g / h

[0073] Liquid ammonia = 51.0 g / h

[0074] Titanium silicon molecular sieve concentration = 2.5% by weight

[0075] The average residence time of materials in the reactor is 80 minutes, the reaction temperature is maintained at 75±1°C through jacket heat exchange, and the reaction pressure is maintained at 0.4MPa. The temperature of the reaction product material entering the sintered filter was maintained at 60° C., and the sintered filter was backwashed every 30 seconds.

[0076] The resulting reaction is as follows:

[0077] Cyclohexanone conversion rate: 96.3%

[0078] Conversion rate of hydrogen peroxide: 98.0%

[0079] Reaction selectivity based on cyclohexanone: 97.5%

[0080] Effective utilization rate of hydrogen ...

Embodiment 3

[0084] For the reaction process, see figure 1 , the specific feed parameters and material settlement conditions are as follows:

[0085] Cyclohexanone = 245.0 g / h

[0086] tert-butanol = 980.0 g / h

[0087] 30% by weight hydrogen peroxide = 311.7 g / h

[0088] Liquid ammonia = 85.0 g / h

[0089] Titanium silicon molecular sieve concentration = 4.0% by weight

[0090] The average residence time of materials in the reactor is 78 minutes, the reaction temperature is maintained at 88±1°C through jacket heat exchange, and the reaction pressure is maintained at 0.3MPa. Maintain the temperature of the reaction product material entering the sintered filter at 85° C., and backwash once every 20 seconds.

[0091] Cyclohexanone conversion rate: 98.5%

[0092] Conversion rate of hydrogen peroxide: 100%

[0093] Reaction selectivity based on cyclohexanone: 97.6%

[0094] Effective utilization rate of hydrogen peroxide: 87.4%

[0095] Yield of cyclohexanone oxime: 96.1%

[0096] Tita...

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Abstract

The invention relates to a method for preparing cyclohexanone-oxime from cyclohexanone ammoximation. The method comprises the following steps of: contacting reaction materials comprising hydrogen peroxide, cyclohexanone, a solvent and ammonia with titanium silicalite molecular sieves with a concentration of 1-10 wt% for 60-100 minutes at a temperature of 60-90 DEG C and under a pressure ranging from a normal pressure to 0.6 MPa, wherein in the reaction materials, the molar ratio of hydrogen peroxide to cyclohexanone is (1.01 to 1.20): 1, and the molar ratio of ammonia to cyclohexanone is (1.2 to 2.5): 1, and a catalyst is titanium silicalite molecular sieves with an average grain diameter of 10-50 microns; and separating the catalyst, namely, the titanium silicalite molecular sieves from reaction products in an external sintering filter, and then conveying the titanium silicalite molecular sieves into a reactor and recycling. Under a catalyst separation condition provided by the method disclosed by the invention, the reaction products are greatly separated from the molecular sieves, thus solving a separation problem for the catalyst and the reaction products, and avoiding the inconvenience brought to installation, maintenance and replacement caused by arranging a separation component in the reactor.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanone oxime by ammoximation of cyclohexanone, and furthermore relates to a method for ammoximation of cyclohexanone using titanium silicon molecular sieve as a catalyst and using a sintered filter to separate reactants and catalysts Process for producing cyclohexanone oxime. Background technique [0002] Caprolactam is a monomer for the production of nylon 6, and it is also an important chemical raw material, and the preparation step of cyclohexanone oxime by cyclohexanone oximation is a key step in the production of caprolactam. [0003] At present, there are three process routes for industrial production of caprolactam: one is the production route of cyclohexanone-hydroxylamine, including traditional Raschig process, DSM / HPO process, BASF-NO reduction process, Inventa-NO reduction process, Allied cumene / phenol process and caprolactam process; the second is the cyclohexane photonitrosation proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/04
CPCY02P20/582Y02P20/584
Inventor 蒋遥明尹华清刘国强李文辉罗光辉肖勇
Owner WUHAN YOULIKE NEW MATERIAL TECH
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