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Method for preparing high-quality graphene through catalytic oxidation multiple-intercalation

A catalytic oxidation, graphene technology, applied in graphene, chemical industry, sustainable manufacturing/processing, etc., to achieve high operating efficiency, improve production efficiency, and protect integrity.

Inactive Publication Date: 2015-02-18
上海二工大资产经营有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method with controllable reaction, high production efficiency, simple and easy process, green environmental protection, low energy consumption and high quality graphene for the current situation of graphene preparation technology

Method used

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  • Method for preparing high-quality graphene through catalytic oxidation multiple-intercalation
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  • Method for preparing high-quality graphene through catalytic oxidation multiple-intercalation

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Pretreatment step: put 5g graphite in 25ml Fe 2+ with H 2 o 2 In the mixed aqueous solution, where Fe 2+ with H 2 o 2 The molar ratio is 1:40, the pH value of the solution is 3, the mechanical stirring rate is 500rpm and supplemented by ultraviolet light irradiation with a wavelength of 254nm for 3h, and then the graphite pretreatment product is filtered and washed;

[0033] (2) Intercalation and exfoliation step: place 4.5g of the graphite pretreated product obtained in step (2) in 20ml of cetyltrimethylammonium bromide aqueous solution for intercalation and exfoliation, the mechanical stirring rate is 300rpm, and the ultrasonic power is 1000W , the treatment time is 60min, and multi-layer graphene is obtained through filtration and washing;

[0034] (3) Repeat the pretreatment and intercalation stripping process of the multilayer graphene twice, and finally place the washed, filtered and dried product in a high-temperature reducing atmosphere (the volume rati...

Embodiment 2

[0037] (1) Pretreatment step: put 5g graphite in 25ml Fe 2+ with H 2 o 2 In the mixed aqueous solution, where Fe 2+ with H 2 o 2 The molar ratio is 1:30, the pH value of the solution is 4, the mechanical stirring rate is 400rpm and supplemented by ultraviolet light irradiation with a wavelength of 254nm for 2h, and then the graphite pretreatment product is filtered and washed;

[0038] (2) Intercalation and stripping step: put 4.3g of the graphite pretreated product obtained in step (2) into 20ml of tetrabutylammonium bromide aqueous solution for intercalation and stripping, the mechanical stirring rate is 400rpm, the ultrasonic power is 1200W, and the treatment time is 60min , obtain multilayer graphene through filtering and washing;

[0039] (3) Repeat the pretreatment and intercalation stripping process of the multilayer graphene three times, and finally place the washed, filtered and dried product in a high-temperature reducing atmosphere (the volume ratio of hydrogen...

Embodiment 3

[0042] (1) Pretreatment step: put 5g graphite in 25ml Fe 2+ with H 2 o 2 In the mixed aqueous solution, where Fe 2+ with H 2 o 2 The molar ratio is 1:50, the pH value of the solution is 2, the ultrasonic power is 800W, and the treatment time is 3h. Then the graphite pretreatment product is filtered and washed;

[0043](2) Intercalation and stripping step: put 4.6g of the graphite pretreated product obtained in step (2) into 20ml of tetraethylammonium bromide aqueous solution for intercalation and stripping, the mechanical stirring rate is 200rpm, the ultrasonic power is 800W, and the treatment time is 120min , obtain multilayer graphene through filtering and washing;

[0044] (3) Repeat the pretreatment and intercalation stripping process of the multilayer graphene twice, and finally place the washed, filtered and dried product in a high-temperature reducing atmosphere (the volume ratio of hydrogen to argon is 4:96; reduction The flow rate of the protective atmosphere i...

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Abstract

The invention relates to a method for preparing high-quality graphene through catalytic oxidation multiple-intercalation. The method comprises the following steps of: (1) pretreating; (2) carrying out intercalation peeling; (3) repeatedly carrying out the pretreating of the step (1) and the intercalation peeling of the step (2) on a product obtained in the step (2) to obtain a graphene product; and (4) washing the graphene product obtained in the step (3) and carrying out integrated filtration and drying on the graphene product obtained in the step (3); and (5) placing the dried product in a reduction protective atmosphere for deoxidation, thus obtaining the high-performance graphene. The method has the advantages of controlled reaction, high production efficiency, environmental friendliness, low energy consumption, high yield of single-layer graphene and few structure faults of graphene, and is simple and practicable in technology.

Description

technical field [0001] The invention relates to a method for preparing high-quality graphene by catalytic oxidation and multiple intercalation, and belongs to the field of graphene preparation. Background technique [0002] Since graphene was discovered in 2004, it has immediately attracted great attention from the scientific community as a new type of carbon material. Graphene has a unique two-dimensional nanostructure. It has high electron transmission rate, excellent electrical conductivity, and high thermal conductivity. It is the material with the highest mechanical strength known and has the advantages of stable chemical properties and good light transmission. Graphene has a very broad application prospect in the fields of lithium-ion batteries, supercapacitors, functional composite materials, sensors, biomedicine, transparent conductive films, and microelectronic devices. [0003] So far, the known preparation methods of graphene are: 1) micromechanical exfoliation m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/19
CPCY02P20/10
Inventor 于伟谢华清陈立飞黎阳
Owner 上海二工大资产经营有限公司
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