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Preparation method of graphene

A graphene and expanded graphite technology, which is applied in the field of graphene preparation, can solve the problems of graphene sheet thickness, direct exhaust emission, and inability to recycle, and achieves the effects of uniform thickness, environmental protection in the production process, and sufficient peeling.

Inactive Publication Date: 2019-02-12
青岛岩海碳材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have problems such as high toxicity of the reducing agent and cannot be recycled, direct emission of exhaust gas, incomplete exfoliation, thick graphene sheets, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1-3

[0043] Phosphoric acid, glacial acetic acid, and potassium permanganate in Preparation Examples 1-3 were all analytically pure, and the flake graphite was selected from ZX-S flake graphite sold by Zhengxu Mineral Products Processing Factory in Lingshou County.

preparation example 1

[0044]Preparation Example 1: According to the ratio in Table 1, 1 kg of potassium permanganate was added to 5 kg of flake graphite with a particle size of 150 μm and a carbon content of 95%, and 1 kg of phosphoric acid with a mass fraction of 80% and 5 kg of The glacial acetic acid with a mass fraction of 70% is mixed evenly, heated in a water bath at 30°C, stirred continuously, taken out after reacting for 50 minutes, washed with distilled water until neutral, and dried at 60°C after suction filtration. Put it into a muffle furnace for high-temperature expansion at 900°C to obtain expanded graphite.

[0045] The raw material ratio of expanded graphite in table 1 preparation example 1-3

[0046]

preparation example 2

[0047] Preparation Example 2: According to the proportioning in Table 1, 2 kg of potassium permanganate was added to 8 kg of flake graphite with a particle size of 165 μm and a carbon content of 97%, and 3 kg of phosphoric acid with a mass fraction of 83% and 15 kg of The glacial acetic acid with a mass fraction of 73% was mixed evenly, heated in a water bath at 33°C, stirred continuously, taken out after 55 minutes of reaction, washed with distilled water until neutral, and dried at 65°C after suction filtration. Put it into a muffle furnace for high-temperature expansion at 940°C to obtain expanded graphite.

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Abstract

The invention discloses a preparation method of graphene. The preparation method comprises the following steps that S1, hydrogen peroxide with the mass fraction being 35-40% is added into a reaction kettle, and the amount of the added hydrogen peroxide accounts for 55-60% of the volume of the reaction kettle; S2, expanded graphite is added into the reaction kettle, the mass ratio of the expanded graphite to the hydrogen peroxide is 1:(0.01-0.02), the temperature is raised to 200-280 DEG C under the normal pressure, and a reaction is conducted at the temperature of 200-280 DEG C for 10-20 minutes; S3, supercritical carbon dioxide is introduced into the reaction kettle for pressurizing, thus the pressure is increased to 8-15 MPa, and the pressure is maintained for 5-8 hours; S4, objects obtained in the reaction kettle is discharged and put into a homogenizer to be homogenized; and S5, the homogenized objects are dried, and then the graphene is prepared after drying. The preparation method has the advantages that stripping of graphene sheet layers is more thorough, the stripping layer number is less and more even, and environmental protection is achieved.

Description

technical field [0001] The invention relates to the technical field of graphene materials, more specifically, it relates to a method for preparing graphene. Background technique [0002] Graphene is a two-dimensional crystal composed of closely packed carbon atoms. It has special optical, electrical, thermal, and mechanical properties. It has half-integer quantum Hall effect at room temperature, quantum tunneling effect, and high-speed electron mobility. 20000m 2 V-1s-1, high thermal conductivity 3000Wm-1K-1 and excellent mechanical properties (high modulus 1060GPa, high strength 130GPa). With these characteristics, graphene can not only produce nanoelectronics and spintronics components with special properties, but also use its planar structure to design large-scale integrated nanoelectronic circuits using standard semiconductor photolithography processes. Functional composite materials, energy storage materials, catalyst supports, etc. have broad application prospects. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/04C01B2204/22C01B2204/32Y02P20/54
Inventor 张勇
Owner 青岛岩海碳材料有限公司
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