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Catalyst taking graphene nano-sheet as framework as well as preparation method and application of catalyst

A graphene nanosheet and catalyst technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effects of simple and practical preparation method, mild reaction conditions, and excellent catalytic activity

Active Publication Date: 2014-03-19
INST OF HIGH ENERGY PHYSICS CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Similar graphene-ligand-metal catalysts prepared by chemical reactions have not been reported yet

Method used

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  • Catalyst taking graphene nano-sheet as framework as well as preparation method and application of catalyst
  • Catalyst taking graphene nano-sheet as framework as well as preparation method and application of catalyst

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Experimental program
Comparison scheme
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Embodiment 1

[0035] The preparation of embodiment 1 graphene-pyridine-copper bromide catalyst

[0036] 1. Preparation of brominated graphene: 1.0g graphene nanosheet (multilayer), 0.5g N-bromosuccinimide and 0.032g zirconium tetrachloride were added in 20mL dichloromethane, under argon protection Stir overnight at room temperature, filter, wash with water, and dry after the reaction;

[0037]2. the preparation of pyridine graphene: add described brominated graphene 0.5g and 0.074g3-pyridine boronic acid into 4mL1, in the 2-dimethoxyethane, then add sodium carbonate aqueous solution (0.38g NaCO 3 Dissolved in 1.6mL water), and 0.046g tetrakis (triphenylphosphine) palladium catalyst, the reaction was stirred overnight at 84°C, filtered, washed with water and dichloromethane, and dried;

[0038] 3. Preparation of a catalyst with graphene nanosheets as a skeleton: the pyridine graphene (0.02mmol by pyridine content) and copper bromide (0.01mmol) were added to 3mL of toluene, stirred and react...

Embodiment 2

[0039] The preparation of embodiment 2 graphene-pyridine-palladium acetate catalyst

[0040] 1. Preparation of brominated graphene: 2.0g graphene nanosheets (multilayer), 1.0g N-bromosuccinimide and 0.052g zirconium tetrachloride were added in 30mL dichloromethane, under argon protection Stir overnight at room temperature, filter, wash with water, and dry after the reaction;

[0041] 2. the preparation of pyridine graphene: add described brominated graphene 0.8g and 0.16g3-pyridine boronic acid into 7mL1, in the 2-dimethoxyethane, then add sodium carbonate aqueous solution (0.38g NaCO 3 Dissolved in 1.6mL water), and 0.046g tetrakis (triphenylphosphine) palladium catalyst, the reaction was stirred overnight at 84°C, filtered, washed with water and dichloromethane, and dried;

[0042] 3. the preparation of the catalyst with graphene nanosheets as the skeleton: the pyridine graphene (0.03mmol by pyridine content) and palladium acetate (0.018mmol) were added to 5mL toluene, and ...

Embodiment 3

[0043] The preparation of embodiment 3 graphene-pyridine-palladium acetate catalyst

[0044] 1. Preparation of brominated graphene: 2.0g graphene nanosheets (multilayer), 1.0g N-bromosuccinimide and 0.052g zirconium tetrachloride were added in 30mL dichloromethane, under argon protection Stir overnight at room temperature, filter, wash with water, and dry after the reaction;

[0045] 2. the preparation of pyridine graphene: the brominated graphene 0.8g and 0.20g3-pyridine boronic acid are added in 7mL1,2-dimethoxyethane, then add sodium carbonate aqueous solution (0.38g NaCO 3 dissolved in 1.6 mL of water), and 0.046 g of tetrakis(triphenylphosphine)palladium catalyst, and the reaction was stirred overnight at 84°C. Filtered, washed with water and dichloromethane, and dried;

[0046] 3. the preparation of the catalyst with graphene nanosheet as skeleton: the pyridine graphene (by pyridine content is 0.03mmol) and palladium acetate (0.022mmol) is added 5mL toluene, reaction i...

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Abstract

The invention relates to a catalyst taking a graphene nano-sheet as a framework as well as a preparation method and application of the catalyst, belonging to the technical field of chemical catalysts. The graphene nano-sheet is taken as a framework, the framework is connected to a pyridine group through a catalyzed bromination reaction and a Suzuki coupled reaction to generate an organic ligand, and the organic ligand is coordinated with transition metal ions to obtain the catalyst which has high catalytic activity and takes the graphene nano-sheet as the framework. The preparation method is simple, convenient and practical, and the reaction conditions are mild. In an oxidation reaction between 1-phenylethanol and air, the catalyst shows good catalytic activity, the oxidation yield is high, the reaction conditions are simplified, and the catalyst can be recycled. Therefore, the catalyst taking the graphene nano-sheet as the framework is expected to be applied to more metal-catalyzed organic reactions.

Description

technical field [0001] The invention relates to an organic catalyst and its preparation method and application, in particular to an organic catalyst with graphene nanosheets as the skeleton, its preparation method and application, and belongs to the technical field of chemical catalysts. Background technique [0002] Graphene, as a two-dimensional crystal with a single-atom thickness bonded by sp2 carbon atoms, exhibits excellent chemical, physical, and mechanical properties, and has a huge application background and value. So far, graphene has been widely used in condensed matter physics, electronics, materials science, etc. Modification methods such as surface modification, chemical doping, surface functionalization, and generation of derivatives on graphene can effectively control its structure and properties, and realize more abundant functions and applications. [0003] The monoatomic layer structure of graphene is a regular hexagonal grid composed of carbon atoms. Its...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C45/39C07C49/78
CPCY02P20/584
Inventor 张延华刘宇薛井泉汪建军杨文江魏乐
Owner INST OF HIGH ENERGY PHYSICS CHINESE ACADEMY OF SCI