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Catalyst for converting benzyl alcohol to benzaldehyde, and preparation method thereof

A catalyst, benzyl alcohol technology, applied in catalyst activation/preparation, organic compound preparation, physical/chemical process catalyst, etc., can solve the problems of easy loss and deactivation of active components, low catalyst activity, etc. The effect of excellent reusability

Active Publication Date: 2019-08-16
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical key to be solved in the present invention is to provide a kind of high activity, high selectivity, high stability, and the problem that catalyst activity is low and active component is easy to lose deactivation exists in the benzaldehyde reaction of selective oxidation of benzyl alcohol, and in addition Catalyst for converting benzyl alcohol into benzaldehyde that can be recovered and reused conveniently and quickly under the action of a magnetic field and its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Prepare FeCl 3 ·6H 2 A mixture of O, 2-aminoterephthalic acid, and DMF in a molar ratio of 2:1:200: weigh 2.7g FeCl 3 ·6H 2 O, 0.9g of 2-aminoterephthalic acid was dissolved in 80mL of DMF and put into a polytetrafluoroethylene reactor, and the two were mixed and stirred for 10min to obtain a mixed solution. 0.195g HAuCl 4 ·3H 2 O was added to the mixed solution, and the stirring was continued for 30 min; the above mixed solution was sealed and placed in an oven at 145°C for crystallization for 20 h to obtain a solid. Cool to room temperature, wash the obtained solid with DMF and methanol successively, and suction filter, and dry the obtained solid at 80°C for 12 hours to obtain a precious metal weight of 5% Au@NH 2 -MIL-101(Fe); 2 Under the atmosphere, at a heating rate of 3°C / min, keep at 700°C for 5h, cool to room temperature, and the obtained black powder is Au@γ-Fe 2 o 3 @N-C catalyst, where γ-Fe 2 o 3 The weight ratio of the catalyst to the porous carbon...

Embodiment 2

[0021] Prepare FeCl 3 ·6H 2 A mixture of O, 2-aminoterephthalic acid, and DMF in a molar ratio of 2:1:100: weigh 2.7g FeCl 3 ·6H 2 O, 0.9g of 2-aminoterephthalic acid was dissolved in 40mL of DMF and put into a polytetrafluoroethylene reactor, and the two were mixed and stirred for 10min to obtain a mixed solution. 0.037g HAuCl 4 ·3H 2 O was added to the mixed solution, and the stirring was continued for 30 min; the above mixed solution was sealed and placed in an oven for crystallization at 170° C. for 24 h to obtain a solid. Cool to room temperature, wash the obtained solid with DMF and methanol successively, and suction filter, and dry the obtained solid at 80°C for 12 hours to obtain a precious metal weight of 0.5% Au@NH 2-MIL-101(Fe); 2 Under the atmosphere, at a heating rate of 5°C / min, keep at 900°C for 5h, cool to room temperature, and the obtained black powder is Au@γ-Fe 2 o 3 @N-C catalyst, where γ-Fe 2 o 3 The weight ratio of the catalyst to the porous car...

Embodiment 3

[0024] Prepare FeCl 3 ·6H 2 A mixture of O, 2-aminoterephthalic acid, and DMF in a molar ratio of 2:1:150: weigh 2.7g FeCl 3 ·6H 2 O, 0.9g of 2-aminoterephthalic acid was dissolved in 60mL of DMF and put into a polytetrafluoroethylene reactor, and the two were mixed and stirred for 10min to obtain a mixed solution. 0.076g HAuCl 4 ·3H 2 O was added to the mixed solution, and the stirring was continued for 30 min; the above mixed solution was sealed and placed in an oven at 120° C. for crystallization for 16 h to obtain a solid. Cool to room temperature, wash the obtained solid with DMF and methanol successively, and suction filter, and dry the obtained solid at 80°C for 12 hours to obtain a precious metal weight of 2% Au@NH 2 -MIL-101(Fe); 2 Under the atmosphere, at a heating rate of 1 °C / min, keep at 500 °C for 5 h, cool to room temperature, and the obtained black powder is Au@γ-Fe 2 o 3 @N-C catalyst, where γ-Fe 2 o 3 The weight ratio of the catalyst to the porous c...

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PUM

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Abstract

The invention discloses a catalyst for converting benzyl alcohol into benzaldehyde, and preparation method thereof. The catalyst is composed of gamma-Fe2O3 derived from an amino functionalized metal-organic framework material NH2-MIL-101(Fe), N-doped porous carbon and noble metal Au nanoparticles, wherein a weight ratio of the gamma-Fe2O3 to the porous carbon is 2-5, and the noble metal Au accounts for 0.5-5% of the weight of the catalyst. The preparation method comprises the following steps: adding iron trichloride and 2-aminoterephthalic acid to N,N-dimethylformamide, dropwise adding a HAuCl4 solution to the above obtained mixed solution, heating and stirring the obtained solution, crystallizing the solution, and washing and drying obtained crystals to obtain Au@NH2-MIL-101(Fe); and carrying out high temperature treatment on the obtained solid in an inert atmosphere to obtain the finished catalyst. The catalyst has the advantages of high activity, high selectivity and high stability,can be easily and quickly recovered and reused under the action of an external magnetic field, and can be reused.

Description

technical field [0001] The invention relates to a heterogeneous catalyst and a preparation method thereof, in particular to a catalyst for converting benzyl alcohol into benzaldehyde and a preparation method thereof Background technique [0002] Oxidation of alcohols to corresponding carbonyl compounds is one of the important reactions in organic synthesis, and its products aldehydes and ketones are important intermediates of many medicines, spices and vitamins. At present, industrial alcohol oxidation mainly uses oxygen-containing inorganic substances such as dichromate and permanganate as oxidants, and the heavy metal salts produced will cause serious environmental pollution. From the perspective of green chemistry, the use of oxygen or air to replace traditional inorganic oxidants has become the main trend of current research and development. As an important fine chemical intermediate, benzaldehyde is widely used in the manufacturing industries of medicine, spices, seaso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08C07C45/38C07C47/54
CPCB01J27/24B01J37/086C07C45/38C07C47/54
Inventor 张富民徐琼皓方莉涂高美朱伟东
Owner ZHEJIANG NORMAL UNIVERSITY
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