Method for preparing graphene powder

A technology of graphene powder and graphene solution, which is applied in the production of bulk chemicals, can solve the problems of low efficiency, environmental pollution, and small output, and achieve the effects of increasing effective volume, less environmental pollution, and increasing output

Inactive Publication Date: 2011-02-09
HARBIN INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problems of low efficiency, low output, and environme

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  • Method for preparing graphene powder
  • Method for preparing graphene powder
  • Method for preparing graphene powder

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specific Embodiment approach 1

[0008] Specific embodiment one: the preparation method of graphene powder in the present embodiment is carried out according to the following steps: one, the preparation of graphite oxide: 10g graphite is added in the mixture of strong oxidizing acid and nitrate, nitrate and graphite mass The ratio is 0.2-1:1, the mass ratio of strong oxidizing acid to graphite is 2-30:1, then cool to 0°C-5°C, stir for 30-40min, continue stirring while slowly adding potassium-containing strong oxidant (takes 30min) , the mass ratio of the potassium-containing strong oxidant to graphite is 0.4-6:1, then the temperature is raised to 10-15°C, and the stirring is continued for more than 12h, and then the liquid is introduced into a water bath with a temperature of 30-40°C, and the reaction is continued for 20-20°C. 40min, slowly add 200ml of water (takes 30min), heat up to 90-100°C and keep it for 35min, then add hydrogen peroxide and 100ml of water, the mass ratio of hydrogen peroxide and graphite...

specific Embodiment approach 2

[0010] Embodiment 2: This embodiment is different from Embodiment 1 in that: the graphite described in Step 1 is flake graphite. Other steps and parameters are the same as in the first embodiment.

specific Embodiment approach 3

[0011] Embodiment 3: This embodiment is different from Embodiment 1 or 2 in that: the strong oxidizing acid described in Step 1 is concentrated sulfuric acid or perchloric acid. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention discloses a method for preparing graphene powder, which belongs to the field of graphene preparation and aims to solve the technical problems of low efficiency, low yield and environmental protection in the conventional graphene preparation methods. The method of the invention comprises the following steps of: 1, preparing graphite oxide; 2, stripping the graphite oxide; 3, performing purification, namely, performing centrifugation treatment and collecting upper-layer solution; and 4, controlling the reaction temperature to be above the supercritical temperature of a solvent in the step 2 to perform reaction for 1 to 24 hours under the conditions of the protection of an inert gas and the pressure of 20 to 100 MPa, naturally cooling or quenching with water a reaction kettle, and slowly exhausting the gas from the kettle to obtain the graphene powder. The graphene powder prepared by the method is goose feather-like black fluffy powder. The method of the invention has the advantages of the high efficiency of 100 percent, high yield and less environmental pollution.

Description

technical field [0001] The invention belongs to the field of graphene preparation. Background technique [0002] At present, the production methods of graphene mainly include mechanical exfoliation method, thermal expansion graphite method and chemical vapor deposition method. The mechanical exfoliation method and the thermal expansion graphite method have low efficiency and small output, and can only be limited to small-scale experiments in the laboratory. The chemical vapor deposition method is still very immature. Recently, scientists have prepared graphene oxide solution with controllable structure on a large scale by using potassium permanganate to oxidize graphite in concentrated sulfuric acid, and then reduced it with reducing agents such as hydrazine to obtain graphene aqueous solution. However, this method uses hydrazine, which is relatively toxic, and it is difficult to obtain graphene powder. [0003] In summary, the existing methods for preparing graphene have...

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Application Information

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IPC IPC(8): C01B31/04
CPCY02P20/54
Inventor 姜再兴黄玉东刘丽
Owner HARBIN INST OF TECH
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