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Preparation method of graphene powder

A graphene powder, graphene solution technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of high degree of agglomeration, poor order, many defects, etc., and achieve excellent electrical conductivity and structure. Fewer defects and the effect of repairing surface defects

Active Publication Date: 2017-05-31
BEIJING SINEVA MATERIAL TECH CO LTD +2
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Problems solved by technology

[0006] The invention provides a preparation method of graphene powder, which is used to solve the problems of high degree of agglomeration, many defects and poor order degree in the graphene powder prepared by the prior art

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preparation example Construction

[0028] A kind of preparation method of graphene powder according to the present invention may further comprise the steps:

[0029] (1) prepare graphene oxide solution:

[0030] Firstly, the improved Hummers method is used to prepare graphite oxide colloid. The following method can be used: add concentrated sulfuric acid and potassium permanganate to the reactor in sequence, mix well, then slowly add graphite raw materials, and stir and react at 40°C for 1.5h. After the reaction is completed, add water to dilute, and then add a certain amount of hydrogen peroxide to obtain a golden yellow graphite oxide coarse slurry. The graphite oxide coarse slurry is centrifuged and washed with deionized water for several times until the pH of the supernatant is 5-6, and the graphite oxide colloid is obtained.

[0031] Then, dilute a certain amount of graphite oxide colloid with deionized water to 0.1-20 mg / mL, and ultrasonically disperse to obtain a graphene oxide solution. The preparatio...

Embodiment 1

[0042] (1) Dilute 1500mL concentrated H 2 SO 4 Pour into the reaction kettle, stir in the ice bath for 10min, slowly add 150gKMnO 4 , stirred for about 15 minutes, then slowly added 50 g of graphite powder with a particle size of 300 mesh, and then stirred and reacted at 40 ° C for 1.5 hours. After the reaction is completed, add water to the reactor to dilute, then add 100ml of 30% hydrogen peroxide to obtain a golden yellow graphite oxide coarse slurry, and the graphite oxide coarse slurry is centrifugally washed with deionized water for many times until the pH of the supernatant is 5 to 6 to obtain graphite oxide Colloid, the concentration is about 30mg / mL.

[0043] (2) Take 10ml of graphite oxide colloid and dilute it to 0.5mg / mL with deionized water, and ultrasonically disperse to obtain a graphene oxide solution. 0.3 g of benzoic acid monomer was added to the graphene oxide solution, stirred for 30 min, and the solution was freeze-dried at -60° C. for 30 h. The mass ra...

Embodiment 2

[0052] (1) Dilute 1500mL concentrated H 2 SO 4 Pour into the reaction kettle, stir in the ice bath for 10min, slowly add 150gKMnO 4 , Stir for about 15 minutes, then slowly add 50g of expanded graphite, and then stir and react at 40°C for 1.5h. After the reaction is completed, add water to the reactor to dilute, then add 100ml of 30% hydrogen peroxide to obtain a golden yellow graphite oxide coarse slurry, and the graphite oxide coarse slurry is centrifugally washed with deionized water for many times until the pH of the supernatant is 5 to 6 to obtain graphite oxide Colloid, the concentration is about 30mg / mL.

[0053] (2) Dilute 100ml of graphite oxide colloid with deionized water to 10mg / mL, and ultrasonically disperse to obtain a graphene oxide solution. Add 0.3 g of salicylic acid monomer to the graphene oxide solution, stir for 1 h, and dry the solution in a vacuum oven at 50° C. for 24 h. The mass ratio of salicylic acid to graphite oxide in the dried product is 1:10...

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Abstract

The invention relates to the technical field of preparation of nanophase materials, and in particular relates to a preparation method of graphene powder. The preparation method comprises the following steps: (1) preparing a graphene oxide solution; (2) adding organic small molecules to the graphene oxide solution, stirring and drying to obtain graphite oxide containing the organic small molecules; and (3) carrying out heat reduction treatment on the dried graphite oxide containing the organic small molecules to obtain graphene powder. The graphene powder prepared by the method provided by the invention has the characteristics of high degree of peeling, thin sheets, few structural defects, good degree of order and excellent electric conductivity, and has great application prospects in the fields of lithium-ion batteries, supercapacitors and the like.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing graphene powder. Background technique [0002] As an emerging two-dimensional nanomaterial, graphene has a perfect crystal structure and many excellent physical and chemical properties. The unique electrical, optical, thermal and mechanical properties of graphene make it have broad application prospects in the fields of electronic devices, field emission materials, composite materials, gas sensors, energy storage and environmental science. Because of its potential value and wide application prospects, the research on graphene materials has become one of the most concerned research fields. In 2004, Geim and Novoselov obtained graphene by mechanically exfoliating highly oriented pyrolytic graphite, which broke the traditional understanding and won the 2010 Nobel Prize in Physics. [0003] At present, the preparation methods of graphene main...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192
Inventor 岳爽段红云韩耀华常珊
Owner BEIJING SINEVA MATERIAL TECH CO LTD
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