Method for preparing cyclohexanol by catalyzing by base metal catalyst

A catalytic preparation and catalyst technology, applied in the direction of heterogeneous catalyst chemical elements, metal/metal oxide/metal hydroxide catalyst, hydrogenation preparation, etc., can solve the catalyst surface carbon activity, improve the production cost and life of cyclohexanone Shortening and other issues, to achieve good chemical stability, reduce synthesis costs, and easy separation

Inactive Publication Date: 2015-03-25
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The one-step synthesis of cyclohexanone requires high catalyst active components and supports. For example, the catalyst active components involved in this process are limited to nano-noble metals (Pd, Ru, etc.),

Method used

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  • Method for preparing cyclohexanol by catalyzing by base metal catalyst
  • Method for preparing cyclohexanol by catalyzing by base metal catalyst

Examples

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Embodiment 1

[0020] The preparation method of porous carbon material loaded base metal: with 1g glucosamine hydrochloride, 40g melamine and 0.85gCo(NO 3 ) 2 ·6H 2 O was dissolved in 300 mL of water, heated in an oil bath at 80°C, stirred by magnetic force, and evaporated to dryness completely. Then the obtained solid is fully ground and evenly calcined at a high temperature of 800°C to obtain a porous carbon material with a Co loading of about 25% and a nitrogen content of about 1.5%, namely 25CoCN 1.5 .

[0021] Phenol hydrogenation reaction: 100mg phenol, 10mL water, 100mg Co loaded porous carbon material 25CoCN 1.5 Add it into a 25mL autoclave, replace the atmosphere in the autoclave with hydrogen three times, fill the hydrogen pressure to 3MPa, seal the autoclave and raise the temperature to 150°C, stir it magnetically, and react for 20 hours. The catalyst is separated from the reaction liquid by means of filtration, the reaction liquid is detected by gas chromatography, and toluen...

Embodiment 2

[0023] The preparation method of porous carbon material loaded base metal: with 1g glucosamine hydrochloride, 40g melamine and 0.85gCo(NO 3 ) 2 ·6H 2 O was dissolved in 300 mL of water, heated in an oil bath at 80°C, stirred by magnetic force, and evaporated to dryness completely. Then the obtained solid is fully ground and evenly calcined at a high temperature of 900°C to obtain a porous carbon material with a Co loading of about 25% and a nitrogen content of about 2%, namely 25CoCN 2 .

[0024] Phenol hydrogenation reaction: 100mg phenol, 10mL water, 100mg Co loaded porous carbon material 25CoCN 2 Add it into a 25mL autoclave, replace the atmosphere in the autoclave with hydrogen three times, fill the hydrogen pressure to 3MPa, seal the autoclave and raise the temperature to 150°C, stir it magnetically, and react for 24 hours. The catalyst is separated from the reaction liquid by means of filtration, the reaction liquid is detected by gas chromatography, and toluene is u...

Embodiment 3

[0026] The preparation method of porous carbon material loaded base metal: with 1g glucosamine hydrochloride, 40g melamine and 0.85gCo(NO 3 ) 2 ·6H 2 O was dissolved in 300 mL of water, heated in an oil bath at 80°C, stirred by magnetic force, and evaporated to dryness completely. Then the obtained solid is fully ground and evenly calcined at a high temperature of 1000°C to obtain a porous carbon material with a Co loading of about 30% and a nitrogen content of about 1.5%, that is, 30CoCN 1.5 .

[0027] Phenol hydrogenation reaction: 100mg phenol, 10mL water, 100mg Co loaded porous carbon material 30CoCN 1.5 Add it into a 25mL autoclave, replace the atmosphere in the autoclave with hydrogen three times, fill the hydrogen pressure to 3MPa, seal the autoclave and raise the temperature to 150°C, stir it magnetically, and react for 30 hours. The catalyst is separated from the reaction liquid by means of filtration, the reaction liquid is detected by gas chromatography, and tol...

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Abstract

The invention discloses a method for preparing cyclohexanol by catalyzing phenol hydrogenation by taking a porous carbon material loaded base metal as a catalyst. The synthetic route of the traditional two-step method comprises phenol hydrogenation and cyclohexanol dehydrogenation, and the catalysis of phenol hydrogenation in preparing cyclohexanol is mainly completed through metals, namely nanometer noble metal Pd, Ni radical and the like which have higher activated cracked hydrogen molecules. The method is characterized in that cyclohexanol is prepared in the presence of a solvent by using the porous carbon material loaded base metal as the catalyst, taking phenol or a phenol derivative as a raw material and catalyzing hydrogenation; a general formula of the catalyst is aM@CXy, wherein a indicates the weight percentage content of the metals contained in the catalyst, M indicates the base metal, C indicates carbon, X indicates a doped mixed element, and y indicates the weight percentage content of the mixed element. The method disclosed by the invention can be used for reducing the usage cost of the catalyst by recovering the catalyst by adopting a simple filtering method, and can obtain cyclohexanol by directly concentrating filter liquor obtained through filtration.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanol by catalyzing the hydrogenation of phenol by using a porous carbon material loaded with base metal as a catalyst. Background technique [0002] Cyclohexanone is an important organic chemical raw material with multiple uses, mainly used to manufacture caprolactam, adipic acid, etc., and caprolactam and adipic acid are monomers of synthetic fibers nylon 6 and nylon 66. At present, the processes for preparing cyclohexanone mainly include cyclohexane oxidation and phenol hydrogenation reduction. Patent US3957876 introduces a cyclohexane air oxidation method using boric acid compounds as catalysts. This method can improve the conversion rate of cyclohexane and the selectivity of alcohols and ketones, but the reaction process is relatively complicated. Literature (Angew.Chem.Int.Ed.2010, 49, 3356-3359.) introduces a method for preparing cyclohexanone by catalytic oxidation of cyclohexane with boro...

Claims

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Application Information

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IPC IPC(8): C07C35/08C07C29/20B01J27/24B01J23/75B01J23/755B01J23/745B01J35/10
CPCY02P20/52C07C29/20B01J23/75B01J27/24B01J2523/845C07C2601/14C07C35/08
Inventor 王勇李浩然陈志荣李翼李建清吕养心彭俊华
Owner ZHEJIANG UNIV
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