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Graphene oxide supported Schiff base palladium catalyst as well as preparation method and application thereof

A technology of Schiff base palladium and graphene, applied in the direction of physical/chemical process catalysts, organic chemical methods, chemical instruments and methods, etc., can solve the loss of palladium nanoparticles, reduce industrial applications, reduce catalytic activity and reusable performance, etc. problems, achieve good reusability, improve dispersion performance, and excellent reusability

Inactive Publication Date: 2013-12-18
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it must be pointed out that the aggregation and loss of palladium nanoparticles often occur during the catalytic C-C coupling reaction of most of the supported Schiff base palladium catalysts, which makes the catalytic activity and repeated use of the fixed Schiff base palladium catalyst The performance is reduced, which greatly reduces its large-scale industrial application in C-C coupling reaction

Method used

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  • Graphene oxide supported Schiff base palladium catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Cool 250 ml of concentrated sulfuric acid to about 0 °C, add 12 g of graphite powder and 8 g of sodium nitrate, slowly add 45 g of potassium permanganate under vigorous stirring, keep the temperature of the system not exceeding 20 °C, stir well and put Put it in a water bath at 35°C for 2 h, then add 800 ml of deionized water so that the temperature of the system does not exceed 98°C, and continue to stir for 20 min; add 700 ml of deionized water and 60 ml of 30% (w) H 2 o 2 , filtered while hot, with 1 mol·L -1 Wash the filter cake sufficiently with HCl until SO4 cannot be detected in the filtrate 2- , and then washed with deionized water to become neutral, and the sample obtained after centrifugation was freeze-dried to obtain black graphene oxide powder.

[0032] The preparation method of graphene oxide supported Schiff base palladium catalyst:

Embodiment 2

[0034] Put 0.2 parts of graphene oxide into 200 parts of nitrogen containing ethylenediamine, nitrogen dimethylformamide solution, the nitrogen of ethylenediamine, the mass fraction of nitrogen dimethylformamide is 5.0%, ultrasonic vibration 2 h, add 2.5 parts of dicyclohexyl carboximide and 2.5 parts of N-hydroxysuccinimide, and continue to sonicate for 1 h. Stir the reaction at a temperature of 80 °C for 12 h, cool to room temperature, and centrifuge the product, wash it with ethanol and distilled water in turn, and freeze-dry to obtain a black solid that is amidated graphene oxide; 0.2 parts of The amidated graphene oxide is added to 150 parts of ethanol solution containing 2-pyridineformaldehyde, the mass fraction of ethanol solution containing 2-pyridineformaldehyde is 5.0%, ultrasonic oscillation 2h, stirring reaction at reflux temperature for 12h, cooling to After the product is centrifuged at room temperature, it is washed with ethanol and distilled water in sequence, ...

Embodiment 3

[0036] Put 0.2 parts of graphene oxide into 200 parts of nitrogen containing ethylenediamine, nitrogen dimethylformamide solution, the nitrogen of ethylenediamine, the mass fraction of nitrogen dimethylformamide is 5.0%, ultrasonic vibration 2 h, add 2.5 parts of dicyclohexyl carboximide and 2.5 parts of N-hydroxysuccinimide, and continue to sonicate for 1 h. Stir the reaction at a temperature of 80 °C for 12 h, cool to room temperature, and centrifuge the product, wash it with ethanol and distilled water in turn, and freeze-dry to obtain a black solid that is amidated graphene oxide; 0.2 parts of The amidated graphene oxide was added to 150 parts of ethanol solution containing 2,6-diacetylpyridine, the mass fraction of the ethanol solution containing 2,6-diacetylpyridine was 5.0%, ultrasonic vibration was performed for 2h, and at reflux Stir and react at high temperature for 12 hours, after cooling to room temperature, the product is centrifuged, washed with ethanol and disti...

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Abstract

The invention relates to a graphene oxide supported Schiff base palladium catalyst as well as a preparation method and application thereof. A catalyst carrier is a graphene oxide prepared by an improved Hummers process, ligand is Schiff base and an active ingredient is palladium salt; the capacity of the palladium in the active ingredient palladium salt is 5.0%-10.0% of the total mass of the catalyst, the diameter of the graphene oxide is 1 mu m-5 mu m, the thickness of the graphene oxide is 0.8 nm-1.2 nm, and the particle diameter of a palladium nano particle is 3 nm-8 nm. The graphene oxide-supported Schiff base palladium catalyst can be used for preventing the palladium from losing in a catalysis process, meanwhile, the graphene oxide has a unique two-dimensional planar structure and can also be used for improving dispersing performance of the palladium nano particle on the surface of the graphene oxide to prevent the palladium from gathering in the catalysis process, so that the catalytic activity of the supported type catalyst is improved. Therefore, the graphene oxide-supported Schiff base palladium catalyst disclosed by the invention can be used for preventing the palladium from gathering and losing better in a catalytic C-C (Carbon-Carbon) coupling reaction process, and has higher catalytic activity and better recycling performance.

Description

field of invention [0001] The invention relates to a graphene oxide supported Schiff base palladium catalyst, a preparation method and an application. Background technique [0002] In the fields of fine chemical industry and pharmaceutical synthetic chemistry, palladium-catalyzed C-C coupling reaction is one of the most effective tools for constructing C-C bonds. In the palladium-catalyzed C-C coupling reaction system, the choice of palladium ligand has a crucial impact on the yield and selectivity of the reaction product. The most commonly used ligands for traditional C-C coupling reactions are monodentate, high-steric hindrance and strong electron-donating ability triarylphosphine. However, most of the commonly used phosphine-containing ligands are sensitive to water and air, which makes the reaction conditions harsh; and in the reaction, the phosphine-containing ligands are very easy to decompose and generate phosphate during the heating process, and recovery is difficul...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07B37/00C07C51/353C07C57/44
Inventor 袁定重钱勇黄斌陈碧波
Owner EAST CHINA UNIV OF TECH
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