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A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method

A weak oxidation and reduction technology, which is applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of complex preparation process, harsh conditions, and high energy consumption, so as to improve preparation efficiency, improve dispersibility, and good compatibility sexual effect

Active Publication Date: 2020-04-03
明德润和机械制造(天津)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical exfoliation method is too limited and not suitable for large-scale industrial production of graphene; the complex preparation process, harsh conditions and low yield of chemical vapor deposition and epitaxial growth methods also limit the large-scale production and application of graphene
The redox method is currently recognized as a method for the industrial production of graphene, but there are many problems such as environmental pollution, high energy consumption, and defects in the structure of the produced graphene, which limit its further application.

Method used

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  • A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method
  • A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method
  • A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method

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Embodiment 1

[0038] A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method, the steps are as follows:

[0039] 1) After ball milling 10 g of flake graphite for 4 hours, put it into a mixed solution of 50 g of 10% acetic acid solution and 50 g of 30% hydrogen peroxide solution, and soak in airtight at room temperature for 12 hours;

[0040] 2) Add a mixture of 1 g of ammonium nitrate and ammonium persulfate to the solution obtained after airtight immersion in step 1), the mass ratio of ammonium nitrate and ammonium persulfate is 10:1, stir evenly and put it into a high-pressure closed hydrothermal kettle , 150°C for 6 hours;

[0041] 3) Cool the mixed solution after the intercalation treatment in step 2) to room temperature, add deionized water, and use a pressure of 15 MPa to subject the mixed solution to high-pressure treatment, and then perform ultrasonic stripping treatment for 3 hours, and the ultrasonic power is 800W;

[0042] 4) The mixed so...

Embodiment 2

[0053] A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method, the steps are as follows:

[0054] 1) After ball milling 5g of flake graphite for 3 hours, put it into a mixed solution of 10g of 8% acetic acid solution and 30g of 25% hydrogen peroxide solution, and soak for 8 hours at room temperature;

[0055] 2) Add a mixture of 0.5 g of ammonium nitrate and ammonium persulfate to the solution obtained after airtight soaking in step 1), the mass ratio of ammonium nitrate and ammonium persulfate is 8:1, stir well and put it into a high-pressure airtight hydrothermal kettle medium, 120°C for 4 hours;

[0056] 3) Cool the mixed solution after the intercalation treatment in step 2) to room temperature, add deionized water, and use a pressure of 12 MPa to perform high-pressure treatment on the mixed solution, and then perform ultrasonic stripping treatment for 1 hour, and the ultrasonic power is 1000W;

[0057] 4) The mixed solution after ...

Embodiment 3

[0062] A method for preparing high-performance graphene by a multi-step weak oxidation-reduction method, the steps are as follows:

[0063] 1) After ball milling 20g of flake graphite for 4 hours, put it into a mixed solution of 50g of 15% acetic acid solution and 150g of 20% hydrogen peroxide solution, and soak for 14 hours at room temperature;

[0064] 2) Add a mixture of 1 g of ammonium nitrate and ammonium persulfate to the solution obtained after airtight soaking in step 1), the mass ratio of ammonium nitrate and ammonium persulfate is 9:1, stir evenly and put it into a high-pressure closed hydrothermal kettle , 140°C for 5 hours;

[0065] 3) Cool the mixed solution after the intercalation treatment in step 2) to room temperature, add deionized water, and use a pressure of 14MPa to subject the mixed solution to high-pressure treatment, and then perform ultrasonic stripping treatment for 4 hours, and the ultrasonic power is 1200W;

[0066] 4) The mixed solution after the ...

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Abstract

The invention discloses a method for preparing high-performance graphene by a multi-step weak oxidation-reduction method. The method comprises the following steps: 1) closedly immersing flake graphitein a mixed solution of an organic carboxylic acid solution and a weak oxidant solution for weak oxidation treatment; 2) adding an intercalation agent into the solution obtained after the closed immersion in the step 1), and conducting intercalation treatment; 3) cooling the mixed solution obtained after intercalation treatment in the step 2), adding deionized water, conducting high-pressure treatment and conducting ultrasonic stripping; 4) centrifugally washing the mixed solution obtained after ultrasonic stripping in the step 3), and collecting a slurry with the solid content of 5-10%; 5) drying the collected slurry, and conducting ball-milling to obtain a graphene powder precursor; and 6) conducting high-temperature sintering and thermal reduction on the graphene powder precursor to obtain the graphene. The graphene prepared by the method has excellent performance, high preparation efficiency, and less environmental pollution and industrialization is easy to realize.

Description

technical field [0001] The invention belongs to the field of large-scale preparation of new material graphene, and in particular relates to a method for preparing high-performance graphene by a multi-step weak oxidation-reduction method. Background technique [0002] As a carbon nanomaterial, graphene has attracted extensive attention and research in the scientific community due to its special crystal structure and excellent performance in the frontier of technological innovation. From scientists determining the structure of graphite and diamond, to zero-dimensional fullerene and one-dimensional carbon nanotubes, and then to the University of Manchester research team successfully obtaining graphene for the first time, carbon materials have formed from zero-dimensional fullerene to one-dimensional carbon Complete systems from nanotubes, 2D graphene to 3D diamond and graphite. Graphene is made of carbon atoms with sp 2 A new type of two-dimensional atomic crystal composed of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/04C01B2204/22C01B2204/24C01B2204/30C01B2204/32
Inventor 周磊秦晓娟吴钦文周佳林昭宁
Owner 明德润和机械制造(天津)有限公司
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