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Method for preparing graphene oxide

A technology of graphene and graphite, which is applied in the field of graphene oxide preparation, can solve problems such as low electrical conductivity and damage to the lattice structure of graphene oxide, and achieve the effect of improving electrical conductivity, simple and easy preparation steps, and mild conditions

Active Publication Date: 2017-12-01
SHANDONG OBO NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the existing preparation methods of graphene oxide, the lattice structure of graphene oxide has been destroyed during the oxidation process, and many excellent characteristics of graphene have been lost, and then reduction means are usually used to obtain graphene, so often leading to the reduction of the resulting graphene
The surface is prone to defects, forming a pentagonal or heptagonal lattice, and the electrical conductivity is usually very low

Method used

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preparation example Construction

[0052] The invention provides a kind of preparation method of graphene oxide, comprises the following steps:

[0053] A) after graphite, intercalation agent and auxiliary intercalation agent are mixed, carry out reaction, obtain reaction mixture;

[0054] B) After cooling down, react the reaction mixture obtained in the above steps with the oxidizing agent again, add water, and then heat up the reaction to obtain the intermediate system;

[0055] The mass ratio of the graphite to the oxidant is 1: (1.5-2.0);

[0056] C) after the intermediate system obtained in the above steps is continued to react with the reducing agent, graphene oxide is obtained;

[0057] In the graphene oxide, the molar ratio of carbon element to oxygen element is (1.6-2):1.

[0058] In the invention, graphite, intercalation agent and auxiliary intercalation agent are firstly mixed and then reacted to obtain a reaction mixture.

[0059] The present invention does not have special limitation to describe...

Embodiment 1

[0098] Disperse 20g of natural flake graphite with a particle size of 20μm in 700ml of 98% concentrated sulfuric acid at room temperature, add 10ml of fuming nitric acid after stirring for 1 hour, and control the reaction temperature below 10°C after 12 hours of reaction. °C for 50 hours. Use a constant pressure dropping funnel to control the temperature below 50°C and add 0.65L of high-purity water dropwise. Raise the temperature to 90°C for 2 hours, then lower the temperature to about 50°C, and add 20ml of hydrogen peroxide. Naturally lower the temperature and perform ultrasonic cleaning to obtain a single-layer graphene oxide solution.

[0099] The graphene oxide prepared in Example 1 of the present invention was analyzed for organic elements, see Table 1, Table 1 is the elemental analysis table of the graphene oxide prepared in Example 1 of the present invention.

[0100] Table 1

[0101]

[0102] It can be seen from Table 1 that the carbon-to-oxygen molar ratio prep...

Embodiment 2

[0110] Disperse 60g of natural flake graphite with a particle size of 10μm in 2000ml of 98% concentrated sulfuric acid at room temperature, add 45ml of fuming nitric acid after stirring for 1 hour, and add 108g of potassium permanganate after 12 hours of reaction to control the reaction temperature below 10°C. °C for 50 hours. Use a constant-pressure dropping funnel to control the temperature below 50°C and add 2L of high-purity water dropwise. Raise the temperature to 90°C for 2 hours, then lower the temperature to about 50°C, and add 60ml of hydrogen peroxide. Naturally lower the temperature and perform ultrasonic cleaning to obtain a single-layer graphene oxide solution.

[0111] The graphene oxide prepared in Example 2 of the present invention was analyzed for organic elements, see Table 3, Table 3 is the elemental analysis table of the graphene oxide prepared in Example 2 of the present invention.

[0112] table 3

[0113]

[0114] As can be seen from Table 3, the c...

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Abstract

The invention provides a method for preparing graphene oxide. The method comprises the following steps: firstly, mixing graphite, an intercalator and an auxiliary intercalator, and performing a reaction so as to obtain a reaction mixture; secondly, cooling, performing a secondary reaction on the reaction mixture obtained in the former step and an oxidant, adding water, and performing a heating reaction so as to obtain an intermediate system, wherein the mass ratio of the graphite to the oxidant is 1:(1.5-2.0); and finally further performing a reaction on the intermediate system obtained in the former step with a reducing agent, thereby obtaining the graphene oxide, wherein the mole ratio of a carbon element to an oxygen element in the graphene oxide is (1.6-2):1; and the lamella thickens of the graphene oxide is 5-10nm. The invention proposes a concept of moderate oxidation, with specific preparation steps, the mole ratio of carbon and oxygen elements is controlled within a specific range, the graphene oxide which is high in hardness and complete in surface structure is prepared, and the conductivity of graphene prepared later is improved. The method is simple and feasible and beneficial to industrial production.

Description

technical field [0001] The invention belongs to the technical field of graphene materials, and relates to a method for preparing graphene oxide, in particular to a method for preparing graphene oxide with a controllable oxidation degree. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a planar film composed of carbon atoms with sp2 hybrid orbitals forming a hexagonal honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. As a two-dimensional crystal composed of carbon atoms with only one layer of atomic thickness, it is the thinnest material and the strongest material currently in the application field, and its fracture strength is 200 times higher than that of steel, and it is also very good Excellent elasticity, the stretching range can reach 20% of its own size; at the same time, graphene has a huge theoretical specific surface area, stable physical and chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01P2002/72C01P2002/82C01P2004/02C01P2004/03C01P2004/04C01P2004/64C01P2006/40
Inventor 赵永彬张在忠程金杰吴开付
Owner SHANDONG OBO NEW MATERIAL CO LTD
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