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A kind of method of cyclohexane oxidation

A technology of cyclohexane and hydrogen peroxide, applied in the field of cyclohexane oxidation, to achieve the effects of improving effective utilization, activity stability, and selectivity

Active Publication Date: 2015-09-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature (such as J Natural Gas Chem 2001, 10: 295~307 and Applied Catal A: Gen 2001, 211: 1~17) also studied the oxidation of cyclohexane catalyzed by titanium silicon molecular sieves, but the conversion rate of cyclohexane and cyclohexane There is still room for further improvement in the selectivity of hexanol

Method used

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  • A kind of method of cyclohexane oxidation
  • A kind of method of cyclohexane oxidation
  • A kind of method of cyclohexane oxidation

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0033] This preparation example illustrates the preparation of the silicon-coated hollow titanium-silicon molecular sieve catalyst used in the present invention.

[0034]Under normal pressure and 30°C, firstly add ethyl silicate to organic alkali tetrapropylammonium hydroxide aqueous solution and mix, stir and hydrolyze for 8 hours to obtain a colloidal solution, then add titanium silicon molecular sieves into it and mix evenly, and titanium The mass ratio of silicon molecular sieve, organic silicon ester, organic base and water is 100:10:2:200. Finally, transfer the above slurry to a high-pressure reactor for hydrothermal treatment at 170°C and autogenous pressure for 12 hours, take it out and filter, dry and roast Catalyst A can be obtained after conventional treatment.

preparation example 2

[0036] This preparation example illustrates the preparation of the silicon-coated hollow titanium-silicon molecular sieve catalyst used in the present invention.

[0037] Under the condition of normal pressure and 60°C, first add ethyl silicate to the organic alkali tetrapropyl ammonium hydroxide aqueous solution and mix, stir and hydrolyze for 3 hours to obtain a colloidal solution, then add titanium silicon molecular sieve into it and mix evenly, and titanium The mass ratio of silicon molecular sieve, organic silicon ester, organic base and water is 100:45:8:500. Finally, transfer the above slurry to a high-pressure reactor for hydrothermal treatment at 140°C and autogenous pressure for 16 hours, take it out and filter, dry and roast Catalyst B can be obtained after conventional treatment.

preparation example 3

[0039] This preparation example illustrates the preparation of the silicon-coated hollow titanium-silicon molecular sieve catalyst used in the present invention.

[0040] Under normal pressure and 80°C, firstly add ethyl silicate to organic alkali tetrapropylammonium hydroxide aqueous solution and mix, stir and hydrolyze for 1 hour to obtain a colloidal solution, then add titanium silicon molecular sieve into it and mix evenly, and titanium The mass ratio of silicon molecular sieve, organic silicon ester, organic base and water is 100:5:1:100. Finally, transfer the above slurry to a high-pressure reactor for hydrothermal treatment at 160°C and autogenous pressure for 6 hours, take it out and filter, dry and roast Catalyst C can be obtained after conventional treatment.

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Abstract

The invention discloses a method for oxidizing cyclohexane. Cyclohexane and hydrogen peroxide contact and react with a catalyst to prepare cyclohexanone and cyclohexanol under the condition of oxidation reaction. The method is characterized in that the catalyst is a mobile five instructure (MFI) titanium silicalite molecular sieve of which the surface is coated by silicon. By adopting the method, the keto-alcohol selectivity of the product is improved; the effective utilization rate of the hydrogen peroxide also can be greatly improved; more unexpectedly, the cyclohexane conversion rate and the catalytic activity stability are also improved.

Description

technical field [0001] The invention relates to a method for oxidizing cyclohexane, and more particularly relates to a method for oxidizing cyclohexane using silicon-coated titanium-silicon molecular sieve as a catalyst. Background technique [0002] Cyclohexanone is an important chemical raw material, widely used in fiber, synthetic rubber, industrial coating, medicine, pesticide, organic solvent industry. Cyclohexanol is also an important chemical raw material, used to make adipic acid, plasticizers and detergents, as well as solvents and emulsifiers. Especially due to the rapid development of the polyamide industry, the demand for cyclohexanone (alcohol) as an intermediate for the preparation of nylon-6 and nylon-66 is more than 1 million tons per year all over the world. [0003] Today, there are three main production process routes for cyclohexanone: cyclohexane liquid-phase oxidation, phenol hydrogenation and benzene partial hydrogenation, and cyclohexane oxidation is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/16C07C49/403C07C45/28C07C35/08C07C29/48
CPCB01J29/89B01J2229/32C07C29/48C07C45/28C07C49/403C07C35/08
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP