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Preparation method of graphene oxide and preparation method of graphene

A technology of graphene and graphite, which is applied in the field of graphene, can solve the problems of complex process, cumbersome operation, and difficulty in preparing large particle size graphene oxide, and achieve the effects of simple process, expanded application, and sufficient oxidation peeling

Active Publication Date: 2011-10-26
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process requires step-by-step precise control of reaction temperature and reaction time. Not only is the process complicated and the operation is cumbersome, but it is also difficult to prepare large-grained graphene oxide that is fully oxidized and exfoliated.

Method used

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  • Preparation method of graphene oxide and preparation method of graphene
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  • Preparation method of graphene oxide and preparation method of graphene

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[0029] The invention provides a kind of preparation method of graphene oxide, comprises the following steps:

[0030] Mix graphite, concentrated acid and strong oxidant evenly, and react in a closed environment at 80°C to 130°C to obtain graphene oxide.

[0031] The invention uses graphite as a raw material, oxidizes it with a strong oxidant under the conditions of concentrated acid, high temperature and airtightness, and exfoliates the graphite into a single-sheet structure to obtain graphene oxide.

[0032] The present invention has no special restrictions on the graphite, which can be natural flake graphite or pure graphite powder; when the graphite is natural flake graphite, the present invention has no special restrictions on the particle size of the natural flake graphite, preferably 20 mesh- 800 mesh, more preferably 30-200 mesh; when the graphite is pure graphite powder, it is preferably analytically pure graphite powder or spectrally pure graphite powder.

[0033] Ac...

Embodiment 1

[0058] Cool 20g of 50-mesh natural flake graphite, 50g of sodium nitrate, 100g of potassium permanganate and 800g of concentrated sulfuric acid with a mass concentration of 98% at 2°C to 4°C for 1 hour, and then add them to the polytetrafluoroethylene In the ethylene reaction kettle, stir slowly for 1min, cover the lid tightly, let it stand at 2°C to 4°C for 1h, then react in an oven at 100°C for 1h; Take out, slowly pour the reaction mixture into 6L of deionized water, stir evenly, add 90mL of hydrogen peroxide aqueous solution with a mass concentration of 20%, stir until the suspension is bright yellow, suction filter and wash the suspension Graphene oxide is obtained after the pH value is 7;

[0059] The graphene oxide was added to 5L of deionized water, 25g of hydrazine hydrate with a mass concentration of 85% was added under stirring conditions, the temperature was raised to 95°C for 15h, and the obtained reaction mixture was cooled, settled, suction filtered, and used to...

Embodiment 2

[0067] Cool 2g of 200-mesh natural flake graphite, 16g of potassium chlorate and 40g of concentrated nitric acid at 1°C to 3°C for 1 hour respectively, then add them into a polytetrafluoroethylene reaction kettle placed in a stainless steel kettle shell, stir slowly for 0.5min, and cover the kettle tightly Cover, let stand at 1°C to 3°C for 0.5h, then react in an oven at 90°C for 1h; after fully cooling, take the polytetrafluoroethylene reactor out of the stainless steel shell, and slowly pour the reaction mixture into 3L In deionized water, stir evenly, suction filter, and wash until the pH value is 7 to obtain graphene oxide;

[0068] The graphene oxide was added to 0.4L deionized water, 2.4g of hydrazine hydrate with a mass concentration of 85% was added under stirring conditions, the temperature was raised to 95°C for 15h, and the obtained reaction mixture was cooled, settled, suction filtered, Graphene was obtained after washing with deionized water until the pH value was...

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Abstract

The invention provides a preparation method of graphene oxide, which comprises the following steps of: uniformly mixing graphite, a concentrated acid and a strong oxidant; and carrying out reaction in a sealed environment at 80-130 DEG C to obtain grapheme oxide. The invention also provides a preparation method of graphene, which comprises the following steps of: uniformly mixing graphite, a concentrated acid and a strong oxidant; carrying out reaction in a sealed environment at 80-130 DEG C to obtain grapheme oxide; adding hydrazine hydrate to the grapheme oxide; and carrying out reduction reaction to obtain graphene. The methods provided by the invention do not need step-by-step precise control of reaction temperature and reaction time, and the process is simple and easy to operate. Graphene oxide prepared by the preparation method provided by the invention has multiple oxygen-containing functional groups, facilitates surface modification, and widens the application of graphene oxide.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a method for preparing graphene oxide and a method for preparing graphene. Background technique [0002] Since Andre K. Geim produced graphene for the first time in 2004, as a new type of two-dimensional nano-carbon material, graphene has attracted widespread attention and in-depth research in the scientific community. . Graphene is a new type of carbonaceous material with the thickness of a single layer of carbon atoms, which is arranged in a two-dimensional honeycomb lattice structure. It is considered to be the basic unit of all other dimensional carbonaceous materials. Zero-dimensional fullerenes, curled into one-dimensional carbon nanotubes, stacked into three-dimensional graphite, etc. Graphene is made of carbon atoms with sp 2 The monoatomic carbon layer formed by hybridization has a very stable structure and has excellent mechanical properties, peculiar electrical pro...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B31/04
Inventor 胡源包晨露宋磊郭玉强
Owner UNIV OF SCI & TECH OF CHINA
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