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Preparation method of graphene

A technology of graphene and graphene, which is applied in the field of graphene preparation, can solve the problems of graphene agglomeration, hard-to-wash separation products, etc.

Active Publication Date: 2013-08-14
SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In these polar solvents, graphite oxide is easy to exfoliate and disperse in aqueous solution to form a colloidal solution, but it is easy to agglomerate and agglomerate during reduction to prepare graphene, and it is difficult to wash and separate the product

Method used

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preparation example Construction

[0027] Such as figure 1 Shown, the preparation method of the graphene of one embodiment, comprises the steps:

[0028] Step S10, preparing a colloidal solution of graphene oxide:

[0029] First prepare graphite oxide, the following method can be adopted: mix concentrated sulfuric acid and graphite powder in the reactor evenly, heat to 70-80°C for oxidation for 4 hours, after cooling, sonicate for 2 hours, then dilute with deionized water, wash and dry , to obtain pretreated graphite powder; according to the Hummer oxidation method, it is oxidized with concentrated sulfuric acid, sodium nitrate and potassium permanganate to prepare fully oxidized graphite oxide. The preparation method of graphite oxide is not limited thereto.

[0030] Then mix the obtained graphite oxide with a solvent in a mortar and grind to obtain a jelly.

[0031] Finally, the obtained jelly is added to a solvent for ultrasonic stripping for 0.5-4 hours to obtain a colloidal solution of graphene oxide. ...

Embodiment 1

[0042] Weigh 5g of solid graphite powder and 30mL of concentrated sulfuric acid in a 500mL three-neck flask, mix evenly, heat the oil bath to 80°C for oxidation, take it out after 4 hours of reaction, and cool it down, sonicate it at 500W for 2 hours, and then use deionized water Dilute to 500mL, transfer to 1L container, dilute to 1L with deionized water, filter through 0.22μm filter, wash with deionized water to 1M BaCl 2 No white precipitate was detected, and then dried at 70° C. for 24 hours to obtain pretreated graphite powder.

[0043] Add the above-mentioned pretreated graphite powder into a 500mL three-necked flask, add 2.5g NaNO 3 and 120mL concentrated sulfuric acid, the three-necked flask was fixed in an ice-water bath and stirred for 30min, the temperature was controlled below 20°C; then 15g KMnO 4 After stirring for 2 hours, add 75mL of deionized water, heat up to 35±3°C and stir for 30min, add 75mL of deionized water, heat up to 98°C and stir for 15min, then add...

Embodiment 2-11

[0047] The reaction conditions such as the type of neutral salt and the type of reducing agent were changed to obtain Examples 2-11, and the results are shown in Table 1 and Table 2.

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Abstract

The invention relates to a preparation method of graphene, comprising the following steps: preparing a colloidal solution of oxidized graphene; adding neutral salt into the colloidal solution and uniformly mixing to obtain an oxidized graphene neutral salting liquid; adding a reducing agent into the oxidized graphene neutral salting liquid and carrying out hot reduction to obtain the graphene. By adding neutral salt into the colloidal solution of oxidized graphene and carrying out reduction, the graphene which has good dispersibility and is caking resistant can be obtained. The specific surface area of the prepared graphene is more than or equal to 600m<2> / g.

Description

【Technical field】 [0001] The invention relates to a preparation method of graphene. 【Background technique】 [0002] Graphene is a hexagonal two-dimensional crystal structure with sp 2 - A carbon material with a single-layer atomic thickness of the skeleton. Compared with fullerene and carbon nanotubes, graphene is considered to be the most promising carbon material. Its raw material graphite is rich in sources, and it has excellent properties in electricity, mechanics, heat and optics. It is used in supercapacitors, lithium There are many potential applications in the fields of ion batteries, liquid crystal devices, transistors and sensors. However, high-quality, large-scale preparation of graphene flakes is currently the biggest bottleneck in the application of graphene. The traditional publicly reported methods for preparing graphene mainly include: chemical vapor deposition, epitaxial vapor deposition growth, micromechanical exfoliation, and preparation of colloidal di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 于淑会孙蓉陈日雄
Owner SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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