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A kind of preparation method of graphene

A graphene and graphene technology, applied in the field of graphene preparation, can solve the problems of graphene with many defects, low strength, poor electrical conductivity and thermal conductivity of graphene, etc., to improve economic efficiency, high electrical conductivity, oxygen-containing low volume effect

Active Publication Date: 2015-09-02
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used reducing agents mainly include hydrazine hydrate, sodium borohydride, etc., but hydrazine hydrate is highly toxic and harmful to the environment. In the production process, it increases the hazard to workers' health; when sodium borohydride is used as a reducing agent, As a result, the reduction of graphene oxide is not complete, and the oxygen content in graphene prepared by the existing oxidation-reduction method is generally 10%.
At present, graphene has also been prepared by microwave reduction method, but the graphene obtained by this method has many defects, resulting in relatively poor electrical and thermal conductivity and low strength of graphene.

Method used

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preparation example Construction

[0014] The embodiment of the present invention provides a safe, environmentally friendly, and thoroughly reduced graphene preparation method. The process flow of the graphene preparation method is as follows figure 1 As shown, it specifically includes the following steps:

[0015] S1: Obtain an organic solution of graphene oxide;

[0016] S2: Under oxygen-free and anhydrous conditions, after adding the alkyl derivative of tungsten hexachloride and lithium to an organic solvent for reaction, then adding the organic solution of graphene oxide for reduction reaction to obtain crude graphene product;

[0017] S3: heat-treating the crude graphene product with microwaves to obtain graphene.

[0018] The above-mentioned preparation method of graphene uses the alkyl derivative of tungsten hexachloride-lithium as the reaction system, and the product produced by the reaction system-low-valent tungsten has good reducing performance for graphene oxide and can effectively remove the graphite oxid...

Embodiment 1

[0029] A method for preparing graphene includes the following process steps:

[0030] S11: Preparation of graphite oxide: add 0.5 g of natural flake graphite powder with a particle size of 100 mesh to 11.5 mL of concentrated sulfuric acid at 0°C, then add 1.5 g of potassium permanganate, keep the temperature of the mixture below 10°C, and stir 2h, then stirred in a water bath at room temperature for 24h, slowly add 46mL of deionized water under ice bath conditions, and then add 140mL of deionized water (containing 2.5mL of 30% hydrogen peroxide) after 15min, wait until the color of the mixture turns bright After the yellow color, perform suction filtration, and finally wash with 250 ml of 10% hydrochloric acid, suction filtration, and vacuum dry at 60° C. for 48 hours to obtain graphite oxide.

[0031] S12: Preparation of graphene oxide solution: adding the graphite oxide powder in step S11 to tetrahydrofuran, and ultrasonically dispersing for 30 minutes to obtain a graphene oxide ...

Embodiment 2

[0038] A method for preparing graphene includes the following process steps:

[0039] S21: Preparation of graphite oxide: add 0.5 g of natural flake graphite powder with a particle size of 500 mesh to 11.5 mL of concentrated sulfuric acid at 0°C, then add 1.5 g of potassium permanganate, keep the temperature of the mixture below 10°C, and stir 2h, then stirred in a water bath at room temperature for 24h, slowly add 46mL of deionized water under ice bath conditions, and then add 140mL of deionized water (containing 2.5mL of 30% hydrogen peroxide) after 15min, wait until the color of the mixture turns bright After the yellow color, perform suction filtration, and finally wash with 250 ml of 10% hydrochloric acid, suction filtration, and vacuum dry at 60° C. for 48 hours to obtain graphite oxide.

[0040] S22: Preparation of graphene oxide solution: adding the graphite oxide powder in step S21 to n-hexane, and ultrasonically dispersing for 60 minutes to obtain a graphene oxide solutio...

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Abstract

The invention provides a preparation method of graphene, which comprises the steps of: obtaining an organic solution of graphene oxide; under the conditions of no oxygen and no water, adding an alkyl derivative of tungsten hexachloride and lithium into an organic solvent for reacting, then adding the organic solution of the graphene oxide for carrying out reduction reaction to obtain a graphene crude product; and thermally treating the graphene crude product by using microwaves to obtain the graphene. A low valent tungsten chemical reduction method and a microwave reduction method are combined, thus the preparation method of the graphene has the advantages of safety, environmental friendliness, thorough reduction, short time and high efficiency; and an SP2 hybridized structure of the graphene is repaired, so that the prepared graphene is low in oxygen content and high in conductivity.

Description

Technical field [0001] The invention belongs to the technical field of graphene, and specifically is a method for preparing graphene. Background technique [0002] Since Andre K. Geim of the University of Manchester in the United Kingdom prepared graphene materials in 2004, they have received extensive attention due to their unique structure and photoelectric properties. Single-layer graphene is considered an ideal material due to its large specific surface area, excellent electrical and thermal conductivity, and low thermal expansion coefficient. Such as: ①high strength, Young's molar weight, (1,100GPa), breaking strength: (125GPa); ②high thermal conductivity, (5,000W / mK); ③high conductivity, carrier transmission rate, (200,000cm 2 / V·s); ④High specific surface area, (theoretical calculation value: 2,630m 2 / g). In particular, its high conductivity, large specific surface properties and its monolayer two-dimensional nano-scale structural properties can be used as electrode mate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04B82Y40/00C01B32/184
Inventor 周明杰吴凤王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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