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Method for preparing large-sized graphene by highly-efficiently exfoliating graphite powder

A technology for exfoliating graphite and graphene, applied in the field of graphene

Active Publication Date: 2017-07-25
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above technical problems, the present invention provides a method for efficiently exfoliating graphite powder to prepare large-size graphene, which uses a micro-fluidizer to exfoliate graphite powder, combined with the use of a water-soluble intercalation agent, on the one hand avoids the use of ultrasonic On the other hand, the water-soluble intercalation agent is easy to remove; the final graphene has few defects and the size is 3-15 μm

Method used

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  • Method for preparing large-sized graphene by highly-efficiently exfoliating graphite powder
  • Method for preparing large-sized graphene by highly-efficiently exfoliating graphite powder
  • Method for preparing large-sized graphene by highly-efficiently exfoliating graphite powder

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Experimental program
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Effect test

Embodiment 1

[0036] 1) Prepare polyoxyethylene-b-polyoxypropylene-b-polyoxyethylene and deionized water into a 200 mg / mL intercalant solution;

[0037]2) Homogeneously disperse 4000 meshes of pyrolytic graphite in the intercalation agent solution obtained in step 1), mechanically stir for 1.5h, and the stirring speed is 1000r / min, to obtain a graphite powder suspension with a mass concentration of 15%;

[0038] 3) Inhale the graphite suspension obtained in step 2) through a high-pressure pump, add it into the micro-fluidizer (Y-shaped cavity), and the slit width is 10mm, and the graphite powder suspension enters the pump cavity at a speed of 300mL / min. Collect the graphite suspension; utilize the micro-fluidizer again to carry out 19 cycles of treatment on the graphite suspension to obtain the suspension I;

[0039] 4) The suspension I was centrifuged at 10000rpm for 30min, filtered, washed 3 times with deionized water, then centrifuged at 10000rpm for 30min, filtered, and vacuum-dried to ...

Embodiment 2

[0042] 1) Polyoxypropylene-b-polyoxyethylene copolymer and deionized water are prepared into a 400 mg / mL intercalant solution;

[0043] 2) Disperse the 800-mesh flake graphite powder homogeneously in the intercalation agent solution obtained in step 1), mechanically stir for 1 h, and the stirring speed is 1000 r / min, to obtain a graphite powder suspension with a mass concentration of 10%;

[0044] 3) the graphite suspension obtained in step 2) is inhaled by a high-pressure pump, added in the micro-jet machine (Y-shaped cavity), the slit width is 14mm, and the graphite powder suspension enters the pump cavity at a speed of 450mL / min. Collect graphite suspension; Utilize this micro-jet machine again to carry out 25 times circulation processing to this graphite suspension, obtain suspension I;

[0045] 4) The suspension I was centrifuged at 10,000 rpm for 30 min, filtered, washed 3 times with deionized water, then centrifuged, and vacuum-dried to obtain powdered graphene.

[004...

Embodiment 3

[0048] 1) Polyvinylpyrrolidone and deionized water are prepared into a 50 mg / mL intercalant solution;

[0049] 2) Homogeneously disperse the 300-mesh expanded graphite powder in the intercalation agent solution obtained in step 1), mechanically stir for 2 hours, and the stirring speed is 800r / min, to obtain a graphite powder suspension with a mass concentration of 15%;

[0050] 3) the graphite suspension obtained in step 2) is inhaled by a high-pressure pump, added in the micro-fluidizer (Z-shaped cavity), the slit width is 12mm, and the graphite powder suspension enters the pump cavity at a speed of 100mL / min. Collect graphite suspension; Utilize this microjet machine again to carry out 49 cycles to this graphite suspension, obtain suspension I;

[0051] 4) The suspension I was centrifuged at 10000rpm for 30min, filtered, washed twice with deionized water, then centrifuged at 10000rpm for 30min, filtered to obtain a graphene wet cake.

[0052] Show through shape analysis and...

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Abstract

The invention discloses a method for preparing large-sized graphene by highly-efficiently exfoliating graphite powder. The method comprises the following steps: 1) dissolving an intercalating agent in deionized water to prepare an intercalating agent solution, wherein the intercalating agent is a water-soluble polymer; 2) adding graphite powder to the intercalating agent solution, and uniformly mixing the graphite powder and the intercalating agent solution to obtain a graphite powder suspension; 3) allowing the graphite powder suspension to go through a microfluidizer at a rate of 50-450 mL / min, and carrying out circulating treatment multiple times to obtain a suspension I; and 4) filtering the suspension I, repeatedly washing the filtered suspension I with deionized water, carrying out filtration drying to obtain a graphene filter cake, and using the graphene filter cake directly or carrying out spray drying and vacuum drying to remove water in order to obtain dry graphene powder. The method utilizes the microfluidizer to exfoliate the graphite powder, and the water-soluble intercalating agent is combined, so abuses which can not be avoided by ultrasonic separation are avoided, and the water-soluble intercalation agent is easy to remove; and the finally prepared graphene has few defects, and the size is 3-15 [mu]m.

Description

technical field [0001] The invention relates to the technical field of graphene, in particular to a method for efficiently exfoliating graphite powder to prepare large-size graphene. Background technique [0002] Graphene is a sp 2 A two-dimensional material with a honeycomb hexagonal planar structure formed by hybridized carbon atoms. Graphene has good electrical, optical, mechanical, thermal properties and many other properties that ordinary materials do not have, and has potential application prospects in many fields such as energy, electronic materials, composite materials and environmental protection. With the increasing potential use of graphene, the macro-preparation method of graphene has become a research hotspot. Known graphene preparation methods include mechanical exfoliation, electrochemical methods, graphite oxide reduction methods, epitaxial growth methods, chemical vapor deposition methods, and the like. In recent years, the mechanical exfoliation of graph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B2204/02C01B2204/04C01P2002/82C01P2004/04C01P2004/61
Inventor 张兴祥王玉周刘焕炳陈甜刘海辉
Owner TIANJIN POLYTECHNIC UNIV
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