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Preparation method of graphene and graphene-oxide composite

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

Active Publication Date: 2016-03-23
SHANGHAI UNIV
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  • Summary
  • 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 agglomeration of graphene in the graphene-oxide composite obtained in the prior art, The metal oxide particles are easy to agglomerate, the dispersion of the two is uneven, and the particle size is not uniform

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  • Preparation method of graphene and graphene-oxide composite
  • Preparation method of graphene and graphene-oxide composite

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Embodiment 1

[0034] See figure 1 , The present invention provides a method for preparing graphene, including the following steps: (1) preparing graphene:

[0035] Weigh a certain amount of catechol or catechol derivative, dissolve it in a solvent to obtain a solution of catechol or its derivative 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 the magnetic stirring is uniformly dispersed, the dispersion is ultrasonically dispersed for 0.5 to 4 hours, and the dispersion is transferred to an autoclave, and the autoclave is placed in a water bath at 80-200℃ Under hydrothermal reaction for 12 to 48 hours, the sample is filtered, washed with water, and dried under vacuum to obtain graphene.

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

Embodiment 2

[0047] The method for preparing graphene and graphene-oxide composites provided in this embodiment is basically the same as that of Embodiment 1, and the difference lies in:

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

[0049] (1) Graphite oxidation:

[0050] Add 3g graphite and 1.5g sodium nitrate into a 500ml three-necked flask at -4℃ in an ice water bath, slowly add 120mL 98% concentrated sulfuric acid and 18g potassium permanganate under stirring, and then heat to 35℃ constant temperature water bath Stir for 0.5h, then slowly add 140mL deionized water to dilute, stir for 10 minutes, add 120ml of hot water at 60℃, continue to stir for 10 minutes, add 30mL of 30% H 2 O 2 , After standing, filter, fully wash the filter cake, wash to neutral, then disperse the filter cake in water, ultrasonic 6h, vacuum drying at 45 ℃ to obtain graphene oxide.

[0051] (2) Preparation of graphene:

[0052] Weigh a certain amount of catechol to dissolve in formic ...

Embodiment 3

[0054] The method for preparing graphene and graphene-oxide composites provided in this embodiment is basically the same as that of Embodiments 1 and 2, and the difference lies in:

[0055] A method for preparing graphene is achieved through the following steps:

[0056] (1) Graphite oxidation:

[0057] In an ice-water bath -4~0℃, add 4g graphite and 2g sodium nitrate into a 500ml three-necked flask, slowly add 150mL 98% concentrated sulfuric acid and 12g potassium permanganate under stirring, and then heat to 35℃ constant temperature Stir in a water bath for 1 hour, then slowly add 160mL deionized water to dilute, stir for 10 minutes, add 160ml of hot water at 60℃, continue to stir for 10 minutes, add 22.75mL of 30% H 2 O 2 , After standing, filter, fully wash the filter cake, wash to neutral, then disperse the filter cake in water, ultrasonic 6h, vacuum drying at 45 ℃ to obtain graphene oxide.

[0058] (2) Preparation of graphene:

[0059] Weigh a certain amount of dopamine dissolved...

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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 composite prepared by using the graphene. Background technique [0002] Graphene is a new type of carbon material. As a new type of two-dimensional structure of carbon material, it was first discovered by Novoselov et al. in 2004 (Novoselov, KS; Geim, AK; Morozov, SV; Jiang, D .; Zhang, Y.; Dubonos, SV; Grigorieva, IV; Firsov, AAScience 2004, 306, 666-9). Graphene is a new type of carbon material with a two-dimensional honeycomb structure. It has good conductivity (7200S / m) and a large theoretical specific surface area (2600m 2 / g), high mechanical stability and other superior performance, so it has attracted widespread attention. [0003] Graphene refers to a sheet-like body arranged in a hexagonal ring between carbon atoms. It is composed of a layer of carbon atoms and can extend inf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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