Method for preparing graphene by inorganic membrane reactor

A technology of inorganic membrane and reactor, applied in the field of graphene prepared by inorganic membrane reactor, can solve the problems of unsatisfactory graphene structure, high production cost, harsh experimental conditions, etc., and achieve easy mass production, simple production process, high The effect of utilization

Active Publication Date: 2012-08-22
NANJING UNIV OF TECH
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Problems solved by technology

The following methods are mainly used in the existing patents about graphene preparation: (1) chemical vapor deposition method: for example, using chemical vapor deposition method to crack methane or other Carbon source gas is deposited to obtain graphene film, but most of this method needs high temperature and high pressure, harsh experimental conditions, complicated operation, and high production cost; (2) the method of heating SiC: for example, by thermally splitting SiC polycrystalline powder to make Si sublimates rapidly, and the obtained carbon species self-assembles to form graphene, but the structure of graphene obtained by this method is often not ideal; (3) microphysical method or mechanical separation method: for example, under vacuum, microwaves are used to treat graphite oxide Radiation, thermal dissociation of graphite oxide to obtain graphene, or wet ball milling of graphite powder in an organic solvent, the graphene obtained by this method has high purity and good conductivity, but the area is small and the reproducibility is poor

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  • Method for preparing graphene by inorganic membrane reactor
  • Method for preparing graphene by inorganic membrane reactor

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Experimental program
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Effect test

Embodiment 1

[0027] as attached figure 1 As shown, add 2.5kg mass concentration successively in reaction kettle 1 and be the concentrated sulfuric acid of 98%, 100g graphite powder, 100g potassium permanganate and stir evenly, pass circulating cooling water in the jacket of reaction kettle, make reaction kettle in Cool to 0°C in an ice-water bath, and cool for 0.5h. The reaction temperature was controlled at 70° C. by a water bath, and the mixture was continuously stirred and reacted for 1 h under the condition of a constant temperature water bath at 70° C. to obtain a graphite oxide suspension. Add 200g mass concentration of 20% hydrogen peroxide aqueous solution to wash the graphite oxide suspension. The material is transported to the membrane module 6 through the circulation pump 5 for membrane filtration and separation. After washing and concentration, graphite oxide with a solid content of 25% is obtained in the reaction kettle. suspension. Raise the temperature to 85°C, add 50g of ...

Embodiment 2

[0029] as attached figure 2Shown, add 5kg mass concentration successively in reaction kettle 1 and be the concentrated nitric acid of 95%, 100g graphite powder, 400g potassium perchlorate and stir evenly, pass circulating cooling water in the jacket of reaction kettle, make the reaction kettle in the ice-water bath Cool to 2°C in medium temperature, cold treatment for 1h. The reaction temperature was controlled at 90° C. by a water bath, stirring was continued and reacted for 4 hours under the condition of a constant temperature water bath at 90° C. to obtain a graphite oxide suspension. Adding 1 kg of mass concentration of 30% hydrogen peroxide solution to wash the graphite oxide suspension, start the circulation pump 5, and use the membrane module 6 to perform membrane filtration on the material in the reactor. After washing and concentration, the reactor with a solid content of 30% graphite oxide suspension. Raise the temperature to 100°C, add 600g of hydrazine hydrate t...

Embodiment 3

[0031] as attached figure 1 As shown, add 8.5kg of perchloric acid, 100g of graphite powder, 250g of sodium perchlorate, 250g of potassium permanganate, and 250g of potassium perchlorate successively in reactor 1 with a mass concentration of 97% and stir evenly. Cooling water was circulated through the jacket, so that the reactor was cooled to 5°C in an ice-water bath, and cold treated for 1.5 hours. The reaction temperature was controlled at 130° C. by a water bath, and the mixture was continuously stirred and reacted for 6 h under the condition of a constant temperature water bath at 110° C. to obtain a graphite oxide suspension. Add 1.8 kg of mass concentration of 40% hydrogen peroxide aqueous solution to wash the graphite oxide suspension, and the material is transported to the membrane module 6 through the circulation pump 5 for membrane filtration. After washing and concentration, the graphite oxide suspension with a solid content of 35% is obtained in the reactor. grap...

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Abstract

The invention relates to a method for preparing graphene by an inorganic membrane reactor. The method comprises the following concrete steps of: in a reaction kettle of the inorganic membrane reactor, carrying out water-bath heating for oxidation reaction after cold treatment on graphite powder, strong acid and strong oxidizer serving as raw materials; adding a hydrogen peroxide water solution; conveying the mixture by a pump to a membrane component for membrane filtration; washing the mixture with deionized water; carrying out concentration to obtain graphite oxide suspension; adding a reducing agent for reduction, thus obtaining graphene suspension; conveying the graphene suspension into the membrane component for continuous membrane filtration by the membrane component; carrying out washing by deionized water; carrying out concentration to obtain graphene suspension in the reaction kettle; and drying the graphene suspension to obtain graphene. By use of the method, the integration of preparation and separation of graphene is effectively realized, the waste rate of a product is lowered, the utilization rate of the raw material is improved, the production processes are simple and production in large batches is easy.

Description

technical field [0001] The invention relates to a method for preparing graphene with an inorganic membrane reactor, belonging to the field of new material preparation. Background technique [0002] Graphene is a one-atom-thick two-dimensional crystal of carbon atoms. Due to its unique electrical properties, mechanical properties, thermal properties, and high specific surface area, graphene has received great attention in the fields of chemistry, physics, materials, energy, and the environment in recent years. At present, there are four main methods for preparing graphene: chemical vapor deposition, mechanical exfoliation, epitaxial growth, and colloidal suspension formation. The micromechanical exfoliation method is only suitable for the production of small batches of single-layer or multi-layer graphene for basic research, while the mass production of sheet-layer graphene is mainly through chemical vapor deposition on metal surfaces and the formation of graphene glue by ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 邢卫红徐南平仲兆祥
Owner NANJING UNIV OF TECH
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