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Microporous graphene aerogel and preparation method thereof

A technology of graphene airgel and graphene hydrogel, which is applied in the direction of graphene, chemical instruments and methods, nano-carbon, etc., can solve the problem that the pore size of graphene airgel is difficult to control, and achieve the goal of optimizing electrochemical performance Effect

Inactive Publication Date: 2018-08-28
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the pore size of existing graphene airgel is difficult to control, the present invention provides a preparation method of microporous graphene airgel

Method used

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  • Microporous graphene aerogel and preparation method thereof
  • Microporous graphene aerogel and preparation method thereof
  • Microporous graphene aerogel and preparation method thereof

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Effect test

Embodiment 1

[0037]Graphene oxide was prepared by modified Hummers method using flake graphite as raw material. After the prepared graphene oxide dispersion was centrifuged at a speed of 10,000 rpm for 1 h with a centrifuge, the clear solution in the upper layer was monodisperse few-layer graphene oxide, and diluted to 1 mg / ml with deionized water. Take 50ml of 1mg / ml graphene oxide dispersion, add 1ml of Nafion film solution with a concentration of 5%wt, ultrasonically disperse for 30 minutes, and then magnetically stir in a water bath environment at 60°C for 2h. Subsequently, 0.5 ml of ethylenediamine was added, sealed and kept in an oven at 90° C. for 12 hours to form a graphene hydrogel. The obtained hydrogel was soaked in deionized water, and the water was changed every 6 hours for a total of 5 days before being taken out. Afterwards, the airgel obtained by freeze-drying the hydrogel at -60° C. was annealed in a nitrogen atmosphere at 800° C. for 30 minutes to obtain the product grap...

Embodiment 2

[0039] Graphene oxide was prepared by modified Hummers method using flake graphite as raw material. After the prepared graphene oxide dispersion was centrifuged at a speed of 10,000 rpm for 1 h with a centrifuge, the clear solution in the upper layer was monodisperse few-layer graphene oxide, and diluted to 1 mg / ml with deionized water. Take 50ml of 1mg / ml graphene oxide dispersion, add 2ml of Nafion membrane solution with a concentration of 5%wt, ultrasonically disperse for 30 minutes, and then magnetically stir in a water bath environment at 60°C for 2h. Subsequently, 100 mg of p-phenylenediamine was added, stirred at 60° C. for 10 minutes, sealed, and kept in an oven at 90° C. for 12 hours to form a graphene hydrogel. The obtained hydrogel was soaked in deionized water, and the water was changed every 6 hours for a total of 5 days before being taken out. Afterwards, the airgel obtained by freeze-drying the hydrogel at -60° C. was annealed in a nitrogen atmosphere at 800° C...

Embodiment 3

[0041] Graphene oxide was prepared by modified Hummers method using flake graphite as raw material. After the prepared graphene oxide dispersion was centrifuged at a speed of 10,000 rpm for 1 h with a centrifuge, the clear solution in the upper layer was monodisperse few-layer graphene oxide, and diluted to 1 mg / ml with deionized water. Take 50ml of 1mg / ml graphene oxide dispersion, add 2ml of Nafion membrane solution with a concentration of 5%wt, ultrasonically disperse for 30 minutes, and then magnetically stir in a water bath environment at 80°C for 2h. Subsequently, 1 ml of hydrazine hydrate solution was added, stirred, sealed, and kept in an oven at 90° C. for 12 hours to form a graphene hydrogel. The obtained hydrogel was soaked in deionized water, and the water was changed every 6 hours for a total of 5 days before being taken out. Afterwards, the airgel obtained by freeze-drying the hydrogel at -50° C. was annealed in a nitrogen atmosphere at 800° C. for 30 minutes to...

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Abstract

The invention relates to a microporous graphene aerogel and a preparation method thereof. The preparation method comprises: (1) adding a Nafion material to a graphene oxide dispersion liquid, fully dispersing, and carrying out thermal insulation for 0.5-12 h at a temperature of 25-95 DEG C; (2) adding a diamine-based substance to the product obtained in the step (1), and carrying out thermal insulation treatment or hydrothermal treatment to form a graphene hydrogel; and (3) soaking the graphene hydrogel obtained in the step (2) in water or carrying out dialysis washing, carrying out freeze drying, and annealing to obtain the microporous graphene aerogel. According to the present invention, the graphene oxide is modified by adding a certain amount of the perfluorinated sulfonic acid resin Nafion< > material (Dupont Company) to the graphene oxide dispersion liquid (such as the Graphene oxide aqueous solution) so as to regulate the dispersion of the graphene oxide.

Description

technical field [0001] The invention relates to the field of airgel preparation, in particular to a method for preparing nano-diameter graphene airgel. Background technique [0002] Graphene is a two-dimensional material composed of a layer of carbon atoms. Its special structure reflects unique physical and chemical properties, and has been widely used in many scientific fields. The main limitation in the application of graphene materials is the agglomeration of graphene caused by the van der Waals force between the layers. One of the main methods to overcome the above-mentioned agglomeration phenomenon is to prepare two-dimensional graphene into three-dimensional graphene airgel, which not only makes full use of the excellent properties of graphene, but also overcomes the agglomeration between its sheets. Graphene airgel has high porosity and specific surface area, excellent thermal conductivity and electrical conductivity, and has been widely used in catalysis, energy sto...

Claims

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Application Information

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IPC IPC(8): C01B32/184
CPCC01B2204/22C01B2204/32C01P2004/03C01P2006/16
Inventor 于云王勇冯爱虎江峰于洋米乐宋力昕
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI