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Method for preparing cyclohexanol and cyclohexanone by selective oxidation of cyclohexane

A technology of cyclohexanol and cyclohexane, which is applied in the field of selective oxidation of cyclohexane to cyclohexanol and cyclohexanone, which can solve the problems of high cost and limited industrial application prospects, and achieve high conversion rate and high selectivity

Active Publication Date: 2013-11-20
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although noble metal catalysts have good cyclohexane oxidation activity, the high cost of such catalysts will greatly limit their industrial application prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of MCM-48 mesoporous molecular sieve catalysts supported by Ce and 3-aminopropyltrimethoxysilane surface functionalization.

[0026] Mix 1.2 grams of NaOH and 70 grams of deionized water to obtain a sodium hydroxide solution, add 10.5 grams of cetyltrimethylammonium bromide at 50 ° C, stir for 1 hour, and form a transparent gel A; 0.52 grams of Ce ( NO 3 ) 3 ·nH 2 O was mixed with 10 grams of deionized water, stirred and dissolved to obtain a cerium solution, and then added dropwise to the transparent gel A under stirring. After stirring for 0.5 hours, 12.5 grams of ethyl orthosilicate was added dropwise to the mixed solution, and stirred for 3 Hours later, transfer to an autoclave for crystallization. Place the autoclave at 100°C for 3 days, cool, filter, and wash to obtain a solid, dry at 100°C for 2 hours, and roast at 550°C for 6 hours to obtain cerium-supported MCM-48 molecular sieve.

[0027] Then the surface of the Ce-loaded MCM-48 mesoporous mole...

Embodiment 2

[0030] The Ce(NO) added in Example 1 3 ) 3 ·nH 2 O was increased to 0.78 g, and other preparation conditions of the catalyst were the same as in Example 1 to obtain a surface-functionalized MCM-48 mesoporous molecular sieve catalyst loaded with Ce and 3-aminopropyltrimethoxysilane. The reaction conditions were the same as in Example 1, the conversion rate of cyclohexane obtained was 14.6%, and the selectivity of cyclohexanol and cyclohexanone was 86%.

Embodiment 3

[0032] The cerium source that adopts among the embodiment 1 is made of Ce(NO 3 ) 3 ·nH 2 O to Ce(SO 4 ) 2 4H2 O, Ce(SO 4 ) 2 4H 2 The amount of O added was 0.78 g, and other preparation conditions of the catalyst were the same as in Example 1 to obtain a surface-functionalized MCM-48 mesoporous molecular sieve catalyst loaded with Ce and 3-aminopropyltrimethoxysilane. The reaction conditions were the same as in Example 1, and the conversion rate of cyclohexane obtained was 7.1%, and the selectivity of cyclohexanol and cyclohexanone was 99.5%.

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PUM

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Abstract

The invention discloses a method for preparing cyclohexanol and cyclohexanone by selective oxidation of cyclohexane. The method comprises the step of carrying out catalytic oxidation on cyclohexane under the condition that no solvent is added in the presence of a cerium-supported and surface-functionalized MCM-48 mesoporous molecular sieve used as a catalyst and oxygen used as an antioxidant. The method is characterized in that hydrophobic treatment is carried out on the surface of the mesoporous material through organic group functionalization while an oxidation active component is supported in the mesoporous molecular sieve, thereby reducing the polarity of the surface of the catalyst so as to improve the selectivity of the catalyst to cyclohexanol and cyclohexanone.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanol and cyclohexanone through the selective oxidation of cyclohexane. Specifically, the MCM-48 mesoporous molecular sieve loaded with cerium and surface functionalized is used as a catalyst, and oxygen is used as an oxidant. Under the condition of solvent, cyclohexane is catalyzed to oxidize cyclohexanol and cyclohexanone. Background technique [0002] Cyclohexanol and cyclohexanone are important intermediates in the production of nylon, and they are also widely used in the fields of industrial coatings, medicine and pesticides, so the selective oxidation of cyclohexane is very important in industry. At present, more than 90% of cyclohexanol and cyclohexanone at home and abroad are produced by the cyclohexane oxidation method (DSM / HPO) developed by the Dutch mining company. This technology is currently the most mature industrial technology, but the single-pass conversion rate of cyclohexane is o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/12C07C35/08C07C29/50C07C49/403C07C45/33B01J29/70
Inventor 詹望成张欣烨郭杨龙郭耘张志刚王筠松王艳芹卢冠忠
Owner EAST CHINA UNIV OF SCI & TECH