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Method for synthesizing cyclohexanone oxime under catalytic action of molecular sieve

A technology of cyclohexanone oxime and molecular sieve, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high hydroxylamine salt dosage and low selectivity, and achieve high selectivity of cyclohexanone oxime , high conversion rate, simple post-processing effect

Inactive Publication Date: 2016-06-22
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process has two main disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts at the same time
In order to solve the above problems, develop an environmentally friendly synthetic process for cyclohexanone oxime, US4,745,221 discloses a method for synthesizing cyclohexanone oxime with a mixture of titanium-silicon molecular sieve or silicon dioxide and titanium-silicon molecular sieve as a catalyst, but the selection of oxime Sex is lower, only 79.45%

Method used

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  • Method for synthesizing cyclohexanone oxime under catalytic action of molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0024] The first step is according to weight ratio cyclohexanone: catalyst is 1:0.1, cyclohexanone: solvent is 1:5, cyclohexanone: the mol ratio of ammonia is 1:1.7, and ammonia is liquid ammonia, and concentration is 25%, solvent It is a mixture of 25% by weight of water and 75% of tert-butanol, and the catalyst is a molecular sieve with an MFI topology, a Si / Ti molar ratio of 60, a Si / B molar ratio of 100, and a Si / Al molar ratio of 100;

[0025] The second step reaction temperature is 75 DEG C, and the mol ratio of cyclohexanone: hydrogen peroxide is 1:1.1, and the concentration of hydrogen peroxide is 30%, and the dropping time is 1 hour, continues to react for 0.5 hour after dropping, and reacts The pressure of the system is 1 atm.

[0026] The analysis results showed that the conversion rate of cyclohexanone was 99.6%, and the selectivity of cyclohexanone oxime was 99.7%.

Embodiment 2

[0032] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0033] In the first step, according to the weight ratio cyclohexanone: catalyst is 1:0.05, cyclohexanone: solvent is 1:10, the catalyst has MFI topological structure, composition Si / Ti molar ratio is 40, Si / B molar ratio Be 120, the molecular sieve that Si / Al mol ratio is 200; In the second step, cyclohexanone: the mol ratio of hydrogen peroxide is 1:1.05.

[0034] The analysis results showed that the conversion rate of cyclohexanone was 99.5%, and the selectivity of cyclohexanone oxime was 99.7%.

Embodiment 3

[0036] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0037]In the first step, according to the weight ratio cyclohexanone: catalyst is 1:0.35, cyclohexanone: solvent is 1:3, cyclohexanone: the molar ratio of ammonia is 1:1.1, and the catalyst has MFI topological structure, composition Molecular sieves with a Si / Ti molar ratio of 60, a Si / B molar ratio of 60, and a Si / Al molar ratio of 80; in the second step, the reaction temperature is 85°C and the cyclohexanone:hydrogen peroxide molar ratio is 1 : 1.3, the dropping time was 2 hours, and continued to react for 1 hour after the dropwise addition was completed.

[0038] The analysis results showed that the conversion rate of cyclohexanone was 99.0%, and the selectivity of cyclohexanone oxime was 99.8%.

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Abstract

The invention discloses a method for synthesizing cyclohexanone oxime catalyzed by molecular sieves. The catalyst has an MFI topological structure, and the molar ratio of Si / Ti is 20-200, the molar ratio of Si / B is 50-200, and the molar ratio of Si / Al is It is a molecular sieve of 50~300, and catalyzes cyclohexanone, ammonia and hydrogen peroxide liquid phase method to prepare cyclohexanone oxime. It is characterized in that, compared with the TS-1 molecular sieve with the same MFI topology, the catalyst of the present invention simultaneously introduces heteroatoms B and Al atoms into the MFI molecular sieve framework through crystallization synthesis, which is effective in catalyzing the ammoximation reaction of ketone compounds Among them, on the basis of maintaining a considerable level of activity and selectivity of the traditional TS-1 molecular sieve, it shows the effect of significantly improving the catalyst life. The further mechanism of action shows that due to the introduction of heteroatoms B and Al atoms into the framework of TS-1 molecular sieve, the obtained catalyst has the effect of significantly reducing the residual hydrogen peroxide in the system and obviously inhibiting the loss of Ti in the active center framework, resulting in a longer catalyst life. Significantly increased.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a method for synthesizing cyclohexanone oxime by molecular sieve catalysis. The molecular sieve with the molar ratio of 50-200 and the Si / Al molar ratio of 50-300 catalyzes the method for preparing cyclohexanone oxime by the liquid phase method of cyclohexanone, ammonia and hydrogen peroxide. Background technique [0002] Cyclohexanone oxime is a key intermediate product in the production process of caprolactam, which is mainly prepared by the reaction of hydroxylamine salt and cyclohexanone. This technique has two main disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts simultaneously. This process is an environmentally unfriendly process. In order to solve the above problems, develop an environmentally friendly synthetic process for cyclohexanone oxime, US4,745,221 discloses a method for synthesizi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/04B01J29/89
CPCC07C249/04B01J29/89B01J2229/183
Inventor 刘月明王磊尹寒梅唐智谋姚旭婷余云开吴立志王健豪
Owner EAST CHINA NORMAL UNIV
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