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Method for preparing supported nano-cobalt catalyst by pyrolysis of deep eutectic solvent and application

A low eutectic solvent, supported technology, used in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc. Good application value and prospect, high activity, high selectivity effect

Inactive Publication Date: 2018-04-24
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The materials or catalysts for catalytic oxidation reported above all have problems such as complicated methods and high prices, and it is difficult to realize large-scale application in terms of economic benefits and operability.

Method used

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  • Method for preparing supported nano-cobalt catalyst by pyrolysis of deep eutectic solvent and application
  • Method for preparing supported nano-cobalt catalyst by pyrolysis of deep eutectic solvent and application
  • Method for preparing supported nano-cobalt catalyst by pyrolysis of deep eutectic solvent and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, in the reactor, add 1-butyl-3-methylimidazolium bromide ([Bmim]Br) 4.38g (2.0mmol) and Co(NO 3 ) 2 ·6H 2 O 1.83g (1.0mmol), stirred and mixed 25 minutes, obtained cobalt-containing deep eutectic solvent; Continue to add 2.0g carbon black and 40g solvent ethanol to reactor, stir and mix 80 minutes and evenly disperse solid-liquid mixture, after removing solvent, obtain A carbon black mixture loaded with a deep eutectic solvent; put the prepared mixture into a tube furnace, and heat up and pyrolyze it under an argon protective atmosphere, starting from an initial temperature of 50°C, with a heating rate of 5°C / min , raised the temperature to 700°C, kept at 700°C for 2 hours, then cooled to room temperature by program, and obtained the residue after pyrolysis. The residue was washed and dried with water to obtain a supported nano-cobalt catalyst, which was named Co-N-C-1.

Embodiment 2

[0025] At room temperature, 2.93 g (2.0 mmol) of 1-ethyl-3-methylimidazolium chloride ([Emim]Cl) and Co(NO 3 ) 2 ·6H 2 O 1.83g (1.0mmol), stirred and mixed 20 minutes, obtained cobalt-containing deep eutectic solvent; Continue to add 2.5g carbon black and 40g solvent ethanol to reactor, stir and mix 90 minutes and evenly disperse solid-liquid mixture, after removing solvent, obtain A carbon black mixture loaded with a deep eutectic solvent; put the prepared mixture into a tube furnace, and heat up and pyrolyze it under a nitrogen protective atmosphere, starting from an initial temperature of 50°C, with a heating rate of 10°C / min, Raise the temperature to 750°C, keep the temperature at 750°C for 2 hours, then cool down to room temperature by program, and obtain the residue after pyrolysis. The residue is washed and dried with water to obtain the supported nano-cobalt catalyst, which is named Co-N-C-2.

Embodiment 3

[0027] At room temperature, in the reactor, add 1-hexyl-3-methylimidazolium bromide ([Hmim]Br) 4.94g (2.0mmol) and Co(NO 3 ) 2 ·6H 2 O 1.83g (1.0mmol), stirred and mixed 30 minutes, obtained cobalt-containing deep eutectic solvent; Continue to add 2.0g carbon black and 40g solvent methanol to reactor, stir and mix 60 minutes and evenly disperse solid-liquid mixture, after removing solvent, obtain A carbon black mixture loaded with a deep eutectic solvent; put the prepared mixture into a tube furnace, and heat up and pyrolyze it under an argon protective atmosphere, starting from an initial temperature of 50°C, with a heating rate of 5°C / min , raised the temperature to 800°C, kept at 800°C for 2 hours, then cooled to room temperature by program, and obtained the residue after pyrolysis. The residue was washed and dried with water to obtain a supported nano-cobalt catalyst, which was named Co-N-C-3.

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Abstract

The invention discloses a method for preparing a supported nano-cobalt catalyst by pyrolysis of a deep eutectic solvent and an application. The method comprises the following steps: firstly, preparinga carbon black mixture supported with the deep eutectic solvent, then pyrolyzing the mixture at high temperature in an inert gas atmosphere to obtain the supported nano-cobalt catalyst, and applyingthe supported nano-cobalt catalyst to an aromatic alcohol liquid phase selective oxidation system with molecular oxygen as an oxygen source. Compared with the prior art, the supported nano-cobalt catalyst prepared with the method has the advantages that a nitrogen-doped carbon skeleton with high specific surface is effectively integrated with the catalytic active center of uniformly dispersed metal cobalt, oxygen can be activated as an oxidant in the absence of alkalinity and aids, aromatic alcohol is catalyzed and oxidized in a green and efficient way, aromatic aldehyde or aromatic ketone isobtained, and the problems about difficulty in recovery, discharge of three wastes and the like caused by extra need of homogeneous organic alkali in the catalytic oxidation process of traditional catalysts are solved. The catalyst prepared with the method has the advantages of high selectivity, high activity, high stability, magnetic recyclability and the like, and has good application value andprospect.

Description

technical field [0001] The invention belongs to the field of composite materials, and relates to a method for preparing a loaded nano-cobalt catalyst by pyrolyzing a deep eutectic solvent and its catalytic oxidation application. Background technique [0002] In the field of chemical industry, the aerobic oxidation of aromatic alcohols to carbonyl compounds is an important class of reactions. The oxidation of benzyl alcohol to prepare benzaldehyde is the most basic reaction in converting hydroxyl functional groups into carbonyl functional groups, and its products are widely used in the preparation of perfume intermediates and pharmaceutical intermediates. Traditional production processes usually use inorganic oxides as oxidants (for example, chromate, permanganate, chlorate, etc.), and need to provide solid bases (for example, sodium hydroxide or potassium carbonate) to accelerate the formation of functional groups. Transformation, so that the reaction can proceed smoothly. ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/75B01J37/08C07C45/38C07C47/54C07C47/575C07C47/544C07C47/565C07C47/55C07C201/12C07C205/44C07C67/313C07C69/76C07C221/00C07C225/22C07D213/48
CPCB01J23/75B01J27/24B01J37/088C07C45/38C07C67/313C07C201/12C07C221/00C07D213/48C07C47/54C07C47/575C07C47/544C07C47/565C07C47/55C07C205/44C07C69/76C07C225/22
Inventor 陶端健赵鑫周言曹志军吴先路
Owner JIANGXI NORMAL UNIV
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