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Method for preparing cyclohexanone

A technology of cyclohexanone and cyclohexane, which is applied in the field of preparation of cyclohexanone, can solve the problems of low efficiency and low efficiency, and achieve the effects of environmental friendliness, good stability and high conversion rate of cyclohexane

Active Publication Date: 2013-01-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, no matter which method is used, the cyclohexane oxidation production process has the disadvantage of low efficiency, and the cyclohexane oxidation process is even considered to be the least efficient of all chemical industry processes
The low efficiency of cyclohexane oxidation synthesis cyclohexanone has become one of the bottlenecks restricting the production of polyamide industry using caprolactam and adipic acid

Method used

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  • Method for preparing cyclohexanone
  • Method for preparing cyclohexanone
  • Method for preparing cyclohexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] This example is used to illustrate the method for preparing cyclohexanone according to the present invention.

[0074] 10 grams of TS-1 titanium-silicon molecular sieve (in terms of oxides, the titanium content in the titanium-silicon molecular sieve is 2.5% by weight), 4.8 grams of concentration is 28% by weight of tetraethylammonium hydroxide aqueous solution placed in the lining In the autoclave of polytetrafluoroethylene, and add 2mL of deionized water to the above autoclave, then close the autoclave, raise the temperature in the autoclave to 145°C, and react at this temperature for 12 hours . The reaction product was dried at 100° C. for 180 minutes, and then the dried product was calcined at 650° C. in an air atmosphere for 3 hours, thereby obtaining Catalyst A.

[0075] Put cyclohexane, hydrogen peroxide, acetone and catalyst A in an autoclave, and react for 12 hours at a temperature of 30° C. and a pressure of 1.5 MPa. Wherein, the molar ratio of cyclohexane, ...

Embodiment 2

[0085] This example is used to illustrate the method for preparing cyclohexanone according to the present invention.

[0086] 12 grams of TS-1 titanium-silicon molecular sieves (calculated as oxides, the titanium content in the titanium-silicon molecular sieves is 1.2% by weight), 1 gram of triethanolamine and 5 grams of tetra-n-propylammonium hydroxide with a concentration of 16.3% by mass The aqueous solution is placed in an autoclave lined with polytetrafluoroethylene, and 3 mL of deionized water is added to the autoclave, then the autoclave is closed, the temperature in the autoclave is raised to 160 ° C, and the The reaction was carried out at this temperature for 56 hours. The reaction product was dried at 150° C. for 120 minutes, and then the dried product was calcined at 540° C. in an air atmosphere for 6 hours, thereby obtaining Catalyst B.

[0087] Put cyclohexane, hydrogen peroxide, tert-butanol and catalyst B in an autoclave, and react for 12 hours at a temperatur...

Embodiment 3

[0089] This example is used to illustrate the method for preparing cyclohexanone according to the present invention.

[0090] 12 grams of TS-1 titanium-silicon molecular sieve (in terms of oxides, the titanium content in the titanium-silicon molecular sieve is 3.2% by weight), 0.5 gram of n-propylamine and 7.5 grams of tetra-n-propylammonium hydroxide with a concentration of 16.3% by mass The aqueous solution was placed in an autoclave lined with polytetrafluoroethylene, then the autoclave was closed, the temperature in the autoclave was raised to 175° C., and the reaction was carried out at this temperature for 48 hours. The reaction product was dried at 90° C. for 240 minutes, and then the dried product was calcined at 700° C. in an air atmosphere for 2 hours, thereby obtaining Catalyst C.

[0091] Put cyclohexane, hydrogen peroxide, methanol and catalyst C in an autoclave, and react for 12 hours at a temperature of 50° C. and a pressure of 0.5 MPa. Wherein, the molar ratio...

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Abstract

The invention relates to a method for preparing cyclohexanone. The method includes, under oxidation reaction condition, allowing contact of cyclohexane and hydrogen peroxide in the presence of catalyst, wherein the catalyst is obtained by allowing contact of Ti-Si molecular sieve and modification liquid at 80-200 DEG C., drying contact product, and roasting, the modification liquid is a water solution containing organic base, and the mass ratio of the Ti-Si molecular sieve to the modification liquid is of 100:(10-150), and the ratio of the Ti-Si molecular sieve accounted by gram to the organic base accounted by mole is 100:(0.005-0.2). The inventive method has high cyclohexane conversion rate and cyclohexanone selectivity. Furthermore, the catalyst used in the method has good stability, and high catalytic activity even if it is used for long time. In addition, the inventive method is simple, easy and environment friendly.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanone. Background technique [0002] Cyclohexanone is widely used in fiber, synthetic rubber, industrial coatings, medicine and pesticide industries, and can be used as a chemical raw material. Used in the preparation of plasticizers and detergents, etc., can also be used as solvents and emulsifiers in chemical operations. With the rapid development of the polyamide industry, the demand for cyclohexanone also increases. At present, the world's annual consumption of cyclohexanone is more than 1 million tons. [0003] There are three main production process routes of cyclohexanone: cyclohexane liquid-phase oxidation method, phenol hydrogenation method and benzene partial hydrogenation method, among which cyclohexane oxidation method is the main process used to produce cyclohexanone in industry, accounting for more than 90 percent. According to whether a catalyst is used and the type of catalyst ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/403C07C45/28
Inventor 史春风龙立华林民朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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