Method for preparing graphene through reduction of oxidized graphene

A graphene and graphene suspension technology, which is applied in the field of preparing graphene materials by using graphene oxide, can solve the problems of reducing the electrical properties of graphene, the toxic price of a reducing agent, and a long reduction reaction period, and achieves large-scale production, The reduction effect is good, and the effect of accelerating the reduction reaction

Active Publication Date: 2014-10-01
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The reducing agent of chemical reduction preparation graphene reported in literature at present mainly contains hydrazine hydrate, dimethyl hydrazine, sodium borohydride, p-diphenol, metal hydride, hydroiodic acid etc. On the one hand, the amount of reducing agent is large and the reduction is insufficient, the reduction reaction cycle is longer (reaction time is greater than 18h), graphene is easy to reunite during the reduction process, etc.; on the other hand, the reducing agent itself is toxic or expensive, and additional functional groups, thereby reducing the electrical properties of graphene

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Embodiment 1

[0035] A method for preparing graphene by reducing graphene oxide according to the present invention, which uses an alkali metal as a reducing agent and iodine as an initiator, and under ultrasonic-assisted stirring, graphene oxide is reduced, and then separated and purified to obtain Graphene specifically comprises the following steps:

[0036] 1. Preparation of graphene oxide: Assemble a three-neck reaction bottle in an ice-water bath, add 48ml of concentrated sulfuric acid and stir, and keep the temperature at (0±1)°C, add 2g of natural flake graphite and 1g of sodium nitrate in sequence, and then add slowly in batches 6g strong oxidant potassium permanganate, react at (10±1)°C for 2h, then react for 2h under stirring in a constant temperature water bath at (35±3)°C, slowly add deionized water to raise the temperature to (98±1) ℃, keep it for 1h, then add hydrogen peroxide to oxidize the unreacted strong oxidant, turn the solution into bright yellow, stop the reaction, let ...

Embodiment 2

[0042] A method for preparing graphene by reducing graphene oxide according to the present invention, which uses an alkali metal as a reducing agent and iodine as an initiator, and under ultrasonic-assisted stirring, graphene oxide is reduced, and then separated and purified to obtain Graphene specifically comprises the following steps:

[0043] 1. Preparation of graphene oxide: Assemble a three-neck reaction bottle in an ice-water bath, add 48ml of concentrated sulfuric acid and stir, and keep the temperature at (0±1)°C, add 2g of natural flake graphite and 1g of sodium nitrate in sequence, and then add slowly in batches 6g strong oxidant potassium permanganate, react at (10±1)°C for 2h, then react for 2h under stirring in a constant temperature water bath at (35±3)°C, slowly add deionized water to raise the temperature to (98±1) ℃, keep it for 1h, then add hydrogen peroxide to oxidize the unreacted strong oxidant, turn the solution into bright yellow, stop the reaction, let ...

Embodiment 3

[0048] A method for preparing graphene by reducing graphene oxide according to the present invention, which uses an alkali metal as a reducing agent and iodine as an initiator, and under ultrasonic-assisted stirring, graphene oxide is reduced, and then separated and purified to obtain Graphene specifically comprises the following steps:

[0049] 1. Preparation of graphene oxide: Assemble a three-neck reaction bottle in an ice-water bath, add 48ml of concentrated sulfuric acid and stir, and keep the temperature at (0±1)°C, add 2g of natural flake graphite and 1g of sodium nitrate in sequence, and then add slowly in batches 6g strong oxidant potassium permanganate, react at (10±1)°C for 2h, then react in a constant temperature water bath at (35±3)°C for 2h with stirring, slowly add 96ml of deionized water to raise the temperature to (98±1) )°C, keep it for 1 hour, add 10ml of 30% hydrogen peroxide to oxidize the unreacted oxidizing agent, turn the solution into bright yellow, st...

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Abstract

The invention discloses a method for preparing graphene through reduction of oxidized graphene. The method comprises the steps of under ultrasonic-assisted stirring, reducing the oxidized graphene with alkali metal or alkaline earth metal as a reducing agent and iodine as an initiator, and separating and purifying to obtain the graphene. The method has the advantages of short reaction cycle, simple operation, high efficiency, no pollution, low cost, good product quality and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanometer materials, and in particular relates to a method for preparing graphene materials by using graphene oxide. Background technique [0002] Graphene is SP 2 Hybridized carbon atoms are arranged in a honeycomb-like hexagonal planar crystal with a thickness of only a single layer of atoms. It is a new type of carbon nanomaterial and is the basic unit of graphite, carbon nanotubes and fullerenes. It has special physical and chemical properties. Since its first discovery in 2004, graphene has immediately aroused great interest in the scientific community and has become one of the most popular materials in chemistry, materials science and physics research in recent years. [0003] The current methods for preparing graphene mainly include mechanical exfoliation, high temperature CVD growth, epitaxial growth, chemical ultrasonic dispersion exfoliation, graphene oxide reduction, etc. The p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 邓凌峰
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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