Preparation method of graphene oxide dispersion liquid

A technology of graphene dispersion liquid and graphite, which is applied in the direction of chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of long time, low yield, difficulty of exfoliating into single-layer graphene, etc., to reduce production Cost and energy consumption, good dispersion and good stability

Active Publication Date: 2014-05-14
江苏超电新能源科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, it takes a long time for the obtained graphite oxide to be stripped into graphene oxide simply by ultrasonic treatment, generally 2-5h, and it is more difficult to realize stri

Method used

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  • Preparation method of graphene oxide dispersion liquid
  • Preparation method of graphene oxide dispersion liquid
  • Preparation method of graphene oxide dispersion liquid

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Experimental program
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Embodiment 1

[0043] A preparation method for a graphene oxide dispersion, specifically comprising the following steps:

[0044] (1) Preparation of sulfate intercalated graphite / sulfuric acid mixture

[0045] At normal temperature, 1.5g of graphite and 30ml of concentrated sulfuric acid with a concentration of 98% were mixed in a ratio of 1g:20mL, and ultrasonicated for 1h to obtain a sulfate-intercalated graphite / sulfuric acid mixture;

[0046] Described graphite is natural graphite powder;

[0047] (2), the preparation of preliminary graphite oxide:

[0048] Add 6g of potassium permanganate at one time to the sulfate intercalated graphite / sulfuric acid mixture obtained in step (1) at normal temperature, and ultrasonicate for 10s to obtain the sulfate intercalated graphite / sulfuric acid / potassium permanganate mixture;

[0049] The amount of potassium permanganate added is calculated according to the mass ratio, that is, graphite: potassium permanganate is 1:4;

[0050] Then the graphite...

Embodiment 2

[0063] A preparation method for a graphene oxide dispersion, specifically comprising the following steps:

[0064] (1) Preparation of sulfate intercalated graphite / sulfuric acid mixture

[0065] At normal temperature, 1.5g of graphite and 30ml of concentrated sulfuric acid with a concentration of 98% were mixed in a ratio of 1g:20mL, and ultrasonicated for 1h to obtain a sulfate-intercalated graphite / sulfuric acid mixture;

[0066] Described graphite is natural flake graphite;

[0067] (2), the preparation of preliminary graphite oxide:

[0068] Add 6g of potassium permanganate at one time to the sulfate intercalated graphite / sulfuric acid mixture obtained in step (1) at normal temperature, and ultrasonicate for 10s to obtain the sulfate intercalated graphite / sulfuric acid / potassium permanganate mixture;

[0069] The amount of potassium permanganate added is calculated according to the mass ratio, that is, graphite: potassium permanganate is 1:4;

[0070] The obtained graph...

Embodiment 3

[0089] A preparation method for a graphene oxide dispersion, specifically comprising the following steps:

[0090] (1) Preparation of sulfate intercalated graphite / sulfuric acid mixture

[0091] At normal temperature, 1.5g of graphite and 30ml of mass percent concentration of 98% concentrated sulfuric acid were mixed in the ratio of 1g:20mL, ultrasonic 1h, prepared graphite / sulfuric acid mixture for sulfate radical intercalation;

[0092] Described graphite is microcrystalline graphite;

[0093] (2), the preparation of preliminary graphite oxide:

[0094] Add 6g of potassium permanganate at one time to the sulfate intercalated graphite / sulfuric acid mixture obtained in step (1) at normal temperature, and ultrasonicate for 10s to obtain the sulfate intercalated graphite / sulfuric acid / potassium permanganate mixture;

[0095] The amount of potassium permanganate added is calculated according to the mass ratio, that is, graphite: potassium permanganate is 1:4;

[0096] Then the...

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Abstract

The invention discloses a preparation method of a graphene oxide dispersion liquid, and the preparation method comprises the following steps: performing ultrasonic treatment so as to obtain a sulfate-intercalated graphite/sulfuric acid mixture; adding potassium permanganate into the obtained sulfate-intercalated graphite/sulfuric acid mixture for a medium-temperature oxidation reaction to obtain a preliminary graphite oxide; performing a high-temperature hydrolysis reaction to obtain a graphite oxide with a hydrophilic group; adding hydrogen peroxide and continuously performing an oxidation reaction to obtain luminous yellow graphite oxide turbid liquid; centrifuging or filtering to obtain claybank mud-like or cake-like object, and treating with a mixed solution of hydrogen peroxide and concentrated sulfuric acid to obtain graphite oxide with a great quantity of hydrophilic groups; washing and vacuum-drying to obtain pure graphite oxide, adding into a solvent and performing ultrasonic treatment to obtain graphene oxide dispersion liquid. The graphene oxide in the graphene oxide dispersion liquid has good dispersity, good stability and relatively large slice. By adopting the preparation method, the process steps are simplified, and the production cost and energy consumption are reduced; the emission of NO2/N2O4 toxic gas is avoided in the reaction process, thereby being environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of graphene oxide preparation, in particular to a method for preparing a graphene oxide dispersion liquid. Background technique [0002] It is generally believed that graphite oxide is a quasi-two-dimensional layered structure. During the oxidation process, graphene sheets are bonded with a large number of oxygen-containing functional groups such as hydroxyl, carboxyl, and epoxy groups. Due to the support of these functional groups and the water between the sheets, the lattice parameters of pristine graphite expand from 0.335 nm to 0.6-1.1 nm of graphite oxide (Lerf, A. et al. Physical Chemistry of Solids 67, 1106 (2006)), It is more conducive to the realization of single-sheet exfoliation and continuous preparation of graphene oxide; at the same time, the functional group also endows the graphene oxide sheet with excellent chemical activity and wetting properties, and makes its surface negatively charged, w...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/198
Inventor 张全生党国举王淼李细方闵凡奇王昭勍李硕李海燕尹佳佳
Owner 江苏超电新能源科技发展有限公司
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