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Method for preparing oxidized graphene

A technology of graphene and graphite, which is applied in the field of improving the preparation method of graphene oxide, can solve problems such as easy damage to graphene oxide sheet structure, temperature rise of graphite oxide solution, uneven size of graphene oxide, etc., to achieve favorable Environmental protection, easy mass production, complete stripping effect

Active Publication Date: 2014-04-09
北京石墨烯技术研究院有限公司
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Problems solved by technology

[0005] Generally speaking, the ultrasonic methods currently used all require a long processing time; and the size of the exfoliated graphene oxide is not uniform due to the inhomogeneity of the ultrasonic wave; it is easy to cause the temperature of the graphite oxide solution to rise rapidly during ultrasonic treatment; high power Ultrasound is also easy to destroy the sheet structure of graphene oxide; the use of organic solvents is easy to cause environmental pollution

Method used

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  • Method for preparing oxidized graphene
  • Method for preparing oxidized graphene

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preparation example Construction

[0016] The present invention will be described in further detail below. A kind of preparation method of graphene oxide is characterized in that, the step of preparation is:

[0017] 1. Preparation of graphite oxide: oxidized intercalation of flake graphite or highly oriented pyrolytic graphite by Hummers method or Staudenmaier method to obtain graphite oxide; the layer spacing of graphite oxide sheets is 0.6nm-1.0nm;

[0018] 2. Preparation of graphite oxide aqueous solution: dissolve dry graphite oxide powder in deionized water, stir for 20-60 minutes to prepare graphite oxide aqueous solution, the concentration is 0.1mg / mL-10mg / mL;

[0019] 3. Freezing: Put not less than 10ml of graphite oxide aqueous solution in a cold storage not higher than 0°C for not less than 60 minutes to make it completely freeze, and use the hydrogen bond formed when water freezes to cause the volume to increase. Expansion principle exfoliates graphite oxide;

[0020] 4. Thawing: After taking out ...

Embodiment 1

[0025] Using the Hummers method, add 100mL of 98% concentrated sulfuric acid into a dry single-necked flask, cool it to 0°C with a low-temperature coolant circulation pump, add 4g of natural flake graphite, 2g of NaNO 3 and 12g KMnO 4 , control the temperature of the reaction solution at 10-15°C, stir and react for 2 hours; then place the beaker in a constant temperature water bath at about 35°C, and continue stirring for 30 minutes when the temperature of the reaction solution rises to about 35°C; finally add 200mL deionized water, control the temperature of the reaction solution within 100°C, and continue to stir for 2h. Dilute the reaction solution to 800-1000mL with deionized water, then add 100mL of 5% H2O2, filter while hot, wash fully with 5% HCI and deionized water until there is no sulfate ion in the filtrate (detected with BaCl solution), and The filter cake was dried in a vacuum oven at 80°C for 12 hours to obtain dry graphite oxide flakes. The interlayer distance ...

Embodiment 2

[0028] Using the Staudenmaier method, add natural flake graphite to the mixture of 98% concentrated sulfuric acid and 65% concentrated nitric acid, wherein the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 3:1, add sodium nitrate under magnetic stirring, and react at room temperature for 24h to obtain oxidized Graphite, dilute the reactant, wash with 5% dilute hydrochloric acid and deionized water until there is no SO in the filtrate 4 2- And it is neutral, and the graphite oxide powder is obtained after drying and grinding, and the interlayer distance of graphite oxide is 1.0nm.

[0029] Take 0.2g of graphite oxide and dissolve it in 50mL of deionized water (the concentration of graphite oxide is 4mg / mL), and magnetically stir for 40min to obtain a uniformly dispersed aqueous solution of graphite oxide. Then place it in a freezer at -5°C for 3 hours to completely freeze it, then melt it at room temperature, dry it in a vacuum oven at 80°C for 8 h...

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Abstract

The invention belongs to a graphene preparation technology and relates to an improvement on an oxidized graphene preparation method. Preparation steps are as follows: preparing oxidized graphite; preparing an oxidized graphite aqueous solution; freezing; unfreezing; and drying. The invention provides a method for preparing the oxidized graphene through cold expansion stripping, which avoids environment pollution, is beneficial to environmental protection, has a simple process, is complete in oxidized graphite stripping, cause less damage on graphite sheets and is convenient for mass production.

Description

technical field [0001] The invention belongs to graphene preparation technology and relates to the improvement of graphene oxide preparation method. 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 novel physical and chemical properties. Studies have shown that the specific surface area of ​​graphene can be as high as 2600m 2 / g, the Young's modulus is about 1100GPa, the breaking strength is 125GPa, the mechanical strength is 1060GPa, and the thermal conductivity is 5000W / m·K. Graphene also has excellent electron transport capabilities, and its electron mobility is as high as 15000 cm at room temperature. 2 / V·S. Since graphene was first discovered in 2004 (Novoselov, K.S. et al Science, 2004, 306, 606), it has immediately aroused...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/198
Inventor 杨程宋洪松
Owner 北京石墨烯技术研究院有限公司
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