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Preparation method for oxidized grapheme in large sheet

A natural flake graphite and fossil technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of high energy consumption, environmental pollution of sulfide or nitride, poor oxidation efficiency, and poor peelability of graphite oxide. Achieve the effect of large specific surface area, improved oxidation efficiency and no environmental pollution

Active Publication Date: 2015-04-15
HEILONGJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there have been patent reports on the preparation of graphene oxide by using graphite micropowder or expanded graphite as raw material by the improved Hummers method. However, when using small particle size graphite micropowder as raw material, the oxidation efficiency is higher. When using large flake graphite as raw material, Its oxidation efficiency and the exfoliation degree of graphite oxide are poor; when expanded graphite is used as raw material, although the expanded worm-like graphite provides more contact area for strong acid and strong oxidant, which improves the oxidation efficiency, however, the huge The expansion volume makes the oxidation reaction require more acid. In addition, in the process of preparing expanded graphite by high temperature expansion, the energy consumption is high, and the released sulfide or nitride will cause serious pollution to the environment.

Method used

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  • Preparation method for oxidized grapheme in large sheet
  • Preparation method for oxidized grapheme in large sheet
  • Preparation method for oxidized grapheme in large sheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Mix 10g of natural flake graphite with a purity of 99% and a particle size of 150μm with 30mL of concentrated nitric acid, add 5mL of hydrogen peroxide with a concentration of 60% from the bottom of the reactor, stir and react for 20min, wash with water, and dry to obtain delaminated graphite; weigh 2g Mix layered graphite with 80mL of concentrated sulfuric acid, slowly add 6g of potassium permanganate, mix evenly, and conduct an ultrasonic-assisted oxidation reaction in an ice-water bath for 30min with an ultrasonic power of 40kHz; raise the temperature of the mixture to 50°C and keep stirring for 10h, then add 200mL to Stirring and reacting for 20 minutes under the assistance of ionized water ultrasound, the obtained product was first centrifuged with a mixed solution of 10% (mass percentage) dilute hydrochloric acid and 1% (mass percentage) hydrogen peroxide at a volume ratio of 1:1, and then washed with deionized water and centrifuged. Separated to obtain graphene ox...

Embodiment 2

[0034] Mix 10g of natural flake graphite with a purity of 99% and a particle size of 180μm with 40mL of concentrated nitric acid, add 7mL of hydrogen peroxide from the bottom of the reactor, stir and react for 30min, wash with water, and dry to obtain delaminated graphite; weigh 2g of delaminated graphite and 100mL Mix concentrated sulfuric acid, slowly add 8g of potassium permanganate, mix well, and conduct ultrasonic-assisted oxidation reaction in an ice-water bath for 30min, with an ultrasonic power of 50kHz; heat the mixture to 60°C and continue stirring for 12h, then add deionized water for ultrasonic-assisted stirring After reacting for 40 minutes, the obtained product was first centrifugally cleaned with a 1:1 mixed solution of 10% dilute hydrochloric acid and 1% hydrogen peroxide, then washed with deionized water, and centrifuged to prepare graphene oxide.

[0035] The TEM characterization photo of the graphene oxide sample obtained by the present embodiment refers to t...

Embodiment 3

[0037] Mix 10g of natural flake graphite with a purity of 90% and a particle size of 270μm with 50mL of concentrated nitric acid, add 10mL of hydrogen peroxide from the bottom of the reactor, stir and react for 60min, wash with water, and dry to obtain delaminated graphite; weigh 2g of delaminated graphite and 90mL Mix concentrated sulfuric acid, slowly add 8g of potassium permanganate, mix well, and then conduct ultrasonic-assisted oxidation reaction in an ice-water bath for 30min, with an ultrasonic power of 40kHz; heat the mixture to 60°C and continue stirring for 12h, then add deionized water and stir under ultrasonic assistance After reacting for 30 minutes, the obtained product was first centrifugally cleaned with a 1:1 mixed solution of 10% dilute hydrochloric acid and 1% hydrogen peroxide, then washed with deionized water, and centrifuged to prepare graphene oxide.

[0038] The TEM characterization photo of the graphene sample that obtains by example refers to attached ...

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Abstract

The invention relates to a preparation method for oxidized graphene in a large sheet. The method comprises the following steps: uniformly mixing natural scale graphite with the mixed acid of concentrated nitric acid or nitric acid and sulfuric acid in a reactor; adding hydrogen peroxide from the bottom of the reactor; reacting under mixing for 10-60 min; washing with water and drying to obtain layered graphite; mixing the layered graphite with strong acid; adding strong oxidant slowly; performing ultrasound-assisted oxidation reaction in an ice-water bath for 30-60 min after uniform mixing; heating the reaction mixture to 50-60 DEG C and continuing mixing for 6-12 h; adding deionized water and performing ultrasound-assisted mixing reaction for 10-30 min; cleaning the obtained product first with mixed solution of diluted hydrochloric acid and hydrogen perhydrol, then with deionized water; performing centrifugal separation to obtain oxidized graphene. The method provided by the invention is simple in operation, high in oxidation efficiency and free from environment pollution; the prepared oxidized graphene has a high peeling rate and a high specific surface area.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide, in particular to a method for preparing large sheets of graphene oxide. Background technique [0002] Since the A.K.Geim group of the University of Manchester in the United Kingdom prepared graphene for the first time by mechanically exfoliating graphite in 2004, graphene, as a new type of two-dimensional nano-carbon material, has attracted much attention because of its unique structure and properties. focus on. Graphene is a hexagonal lattice honeycomb two-dimensional structure material composed of carbon atoms with sp2 hybrid orbitals. The thickness of a single layer is 0.35nm, and the C-C bond length is 0.142nm. It is a component of fullerenes, carbon nanotubes and graphite. The basic unit has excellent electrical, thermal, mechanical and electrochemical properties. The theoretical specific surface area of ​​single atomic layer graphene material is as high as 2630m 2 / g, the semicond...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/198
Inventor 刘丽来丁慧贤丁淑芳张鸿波黄耀群邢善超
Owner HEILONGJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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