Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite

A technology of microcrystalline graphite and solvothermal, which is applied in the field of graphene material preparation, can solve problems such as lack of scientific research investment, and achieve the effects of long cycle time, high yield and high grade

Active Publication Date: 2015-08-19
BEIJING INSTITUTE OF TECHNOLOGYGY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

my country's microcrystalline graphite ore has high grade and large reserves, but there are few reports on the method of preparing graphene from microcrystalline graphite, and the investment in scientific research is relatively lacking.

Method used

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  • Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite
  • Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite
  • Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite

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Embodiment 1

[0036] A method for preparing microcrystalline graphene by solvent thermal exfoliation of microcrystalline graphite, the method steps are as follows:

[0037] (1) Take by weighing 35mg microcrystalline graphite powder, add in 35mL solvent 1, described solvent 1 is formed by mixing N-methylpyrrolidone and o-dichlorobenzene at a volume ratio of 1:1, stir for 30min, then ultrasonically treat for 30min, The ultrasonic power is 80W, so that the microcrystalline graphite and the solvent 1 are evenly mixed to obtain a black suspension 1, such as figure 1 Shown, wherein, the concentration of microcrystalline graphite is 1mg mL -1 ;

[0038] (2) The suspension 1 obtained in step (1) is packed into a 50mL reactor whose bottom surface diameter is 5cm. The lining material of the reactor is polytetrafluoroethylene. Seal the reactor, heat it in an oven to 180°C and keep the temperature, stir and react for 24 hours to obtain a black suspension 2;

[0039] (3) After the suspension 2 obtain...

Embodiment 2

[0049] A method for preparing microcrystalline graphene by solvent thermal exfoliation of microcrystalline graphite, the method steps are as follows:

[0050] (1) Weigh 9g microcrystalline graphite powder, add in 1500mL solvent 1, described solvent 1 is formed by mixing N,N-dimethylformamide and o-dichlorobenzene with a volume ratio of 1:3, stir for 30min, and then Ultrasonic treatment for 30min, the ultrasonic power is 100W, so that microcrystalline graphite and solvent 1 are mixed uniformly to obtain black suspension 1, wherein the concentration of microcrystalline graphite is 6mg mL -1 ;

[0051] (2) the suspension 1 that step (1) obtains is packed into the reactor that 2000mL bottom surface diameter is 15cm, and the liner material of described reactor is polytetrafluoroethylene, puts into the reactor that diameter is 3cm Magneto, seal the reaction vessel, heat it in an oven to 210°C and maintain the temperature, stir and react for 72 hours, and obtain a black suspension 2...

Embodiment 3

[0062] A method for preparing microcrystalline graphene by solvent thermal exfoliation of microcrystalline graphite, the method steps are as follows:

[0063] (1) Weigh 22.5g microcrystalline graphite powder, add in 750mL solvent 1, described solvent 1 is formed by mixing N,N-dimethylacetamide and o-dichlorobenzene at a volume ratio of 1:2, stir for 30min, Then ultrasonic treatment 30min, ultrasonic power is 100W, makes microcrystalline graphite and solvent 1 mix homogeneously, obtains black suspension 1, wherein, the concentration of microcrystalline graphite is 30mg mL -1 ;

[0064] (2) The suspension 1 obtained in step (1) is packed into a 1000mL reactor whose bottom surface diameter is 10cm. Seal the reaction kettle, heat it in an oven to 210°C and keep the temperature, stir and react for 72h, and obtain a black suspension 2;

[0065] (3) After the suspension 2 obtained in step (2) in the reactor is cooled to room temperature, transfer it to a beaker, and perform ultraso...

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PUM

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Abstract

The invention relates to a method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite, and belongs to the technical field of graphene material preparation. The method comprises the following steps: uniformly mixing microcrystalline graphite powder with a mixed solution of o-dichlorobenzene and one or more of N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethyl acetamide and butanolide to the microcrystalline graphite concentration of 1-30mg.mL<-1>; adding the obtained solution into a closed container, heating to 180-210DEG C, and stirring for 24h or more; carrying out continuous ultrasonic treatment at 0-5DEG C under 80-100W for 10min or above; centrifuging, and collecting the obtained precipitate; dispersing the precipitate in methanol or ethanol or isopropanol or n-propanol, centrifuging, and collecting the obtained new precipitate; dispersing the new precipitate in water, centrifuging, and collecting the finally obtained precipitate; and dispersing the finally obtained precipitate, freezing within 10min to form a solid, and carrying out vacuum drying to obtain the microcrystalline graphene. The method has the advantages of low cost, high grade and large reserve of the above raw material, simple preparation, low cost, and realization of amplified production.

Description

technical field [0001] The invention relates to a method for preparing microcrystalline graphene by solvent thermal exfoliation of microcrystalline graphite, and belongs to the technical field of graphene material preparation. Background technique [0002] Graphene is a single-layer sheet structure composed of carbon atoms, which are connected to each other to form a hexagonal grid. Graphene has a theoretical value of 2630m 2 g -1 Large specific surface area, 200000cm 2 V -1 the s -1 The high electron mobility, excellent light transmittance and mechanical strength make graphene widely used in electronic devices (such as: field effect transistors, transparent electrodes, solar cells, etc.), energy storage devices (such as: supercapacitors, lithium-ion batteries, etc.) , Energy conversion devices (such as hydrogen storage, photoelectric conversion, fuel cells, etc.) and other fields have been widely used, which has attracted extensive attention of researchers around the w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 曲良体郑观培胡传刚胡仔健何新元王勇
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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