Preparation methods of graphene and graphene-oxide compound

A graphene and oxide technology, applied in the field of new functional carbon materials, can solve the problems of easy aggregation of metal oxide particles, uneven particle size, easy aggregation of graphene, etc., and achieve uniform size, low cost, and sufficient reduction reaction Effect

Active Publication Date: 2013-10-02
SHANGHAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Another object of the present invention is to provide a kind of preparation method that adopts water system, mild reaction, uniformly dispersed graphene-oxide composite, solves the easy agglomer

Method used

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  • Preparation methods of graphene and graphene-oxide compound
  • Preparation methods of graphene and graphene-oxide compound

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Embodiment 1

[0034] See figure 1 , the invention provides a kind of preparation method of graphene, comprises the following steps: (1) prepares graphene:

[0035]Weigh a certain amount of catechol or catechol derivatives, dissolve in a solvent to obtain a solution of catechol or its derivatives with a mass concentration of 0.05g / ml, grind graphene oxide into powder, and weigh a certain amount Graphene oxide powder is added to the solution of catechol or its derivatives, and after magnetic stirring to disperse evenly, ultrasonically disperse for 0.5-4 hours, transfer the dispersion liquid into a high-pressure reactor, and place the high-pressure reactor in a water bath at 80-200°C After hydrothermal reaction for 12-48 hours, the sample was filtered, washed with water, and dried in vacuum to obtain graphene.

[0036] The catechol derivative described in the step (2) is one of dopamine, α-methyldopamine, dihydroxyphenylalanine; the described solvent is water, methanol, ethanol, isopropanol, ...

Embodiment 2

[0047] The preparation method for preparing graphene and graphene-oxide composite that present embodiment provides is basically the same as embodiment 1, and its difference is:

[0048] The preparation method of described graphene is realized through the following steps:

[0049] (1) Graphite oxidation:

[0050] In an ice-water bath at -4°C, add 3g of graphite and 1.5g of sodium nitrate into a 500ml three-necked flask, slowly add 120mL of concentrated sulfuric acid with a mass fraction of 98% and 18g of potassium permanganate under stirring, and then raise the temperature to a constant temperature water bath of 35°C Stir for 0.5h, then slowly add 140mL of deionized water to dilute, stir for 10 minutes, add 120ml of hot water at 60°C, continue stirring for 10 minutes, add 30mL of 30% H 2 o 2 , filtered after standing still, fully washed the filter cake until neutral, then dispersed the filter cake in water, ultrasonicated for 6 hours, and vacuum-dried at 45°C to obtain graphe...

Embodiment 3

[0054] The preparation method for the preparation of graphene and graphene-oxide compound that present embodiment provides is basically the same as embodiment 1, 2, and its difference is:

[0055] A kind of preparation method of graphene, realizes by following steps:

[0056] (1) Graphite oxidation:

[0057] Add 4g of graphite and 2g of sodium nitrate into a 500ml three-necked flask in an ice-water bath at -4~0°C, slowly add 150mL of concentrated sulfuric acid with a mass fraction of 98% and 12g of potassium permanganate under stirring, and then raise the temperature to 35°C to keep the temperature Stir in a water bath for 1 hour, then slowly add 160 mL of deionized water to dilute, stir for 10 minutes, add 160 mL of hot water at 60°C, continue stirring for 10 minutes, add 22.75 mL of 30% H 2 o 2 , filtered after standing still, fully washed the filter cake until neutral, then dispersed the filter cake in water, ultrasonicated for 6 hours, and vacuum-dried at 45°C to obtain ...

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Abstract

The invention relates to the technical field of carbon material preparation and provides a preparation method of graphene. The preparation method comprises the following step that graphene oxide is dispersed in a solution of catechol or its derivatives and the mixed solution undergoes a hydrothermal reaction to produce the graphene having particle length and width of 10-200 microns. The invention also discloses a preparation method of a graphene-oxide compound comprising uniform-size and uniformly-dispersed oxide particles. The preparation method comprises that the graphene and an oxide precursor solution are dispersed in an aqueous solution and the mixed solution undergoes a hydrothermal reaction to produce the graphene-oxide compound. The preparation methods adopt a hydrothermal method and a water system, do not produce toxins and are environmentally friendly. The graphene has good transparency and small thickness. The graphene-oxide compound comprises the uniform-size oxide particles uniformly dispersed in the graphene, solves the problems of easy aggregation of the graphene and the oxide particles, uneven dispersion of the graphene and the oxide particles, complex preparation processes and high equipment requirements, and can be widely used in fields of supercapacitors, lithium ion batteries and electrochemical sensing.

Description

technical field [0001] The invention relates to the technical field of novel functional carbon materials, in particular to a method for preparing graphene and a method for preparing a graphene-oxide compound prepared by using the graphene. Background technique [0002] Graphene (Graphene) is a new type of carbon material, as a new type of two-dimensional carbon material, was first discovered in 2004 by Novoselov et al. (Novoselov, K.S.; Geim, A.K.; Morozov, S.V.; Jiang, D .; Zhang, Y.; Dubonos, S.V.; Grigorieva, I.V.; Firsov, A.A. Science 2004, 306, 666-9). As a new type of two-dimensional honeycomb structure carbon material, graphene has good electrical conductivity (7200S / m), large theoretical specific surface area (2600m 2 / g), high mechanical stability and other superior properties, it has attracted widespread attention. [0003] Graphene (Graphene) refers to a kind of flakes arranged in a hexagonal ring between carbon atoms. It is composed of a layer of carbon atoms a...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01G25/02C01G23/053C01B33/12C01G19/02C01G45/02C01G51/04C01G53/04C01B32/184C01B32/194
Inventor 施利毅王竹仪徐海平袁帅赵尹张美红
Owner SHANGHAI UNIV
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