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Rapid preparation methods of graphene oxide and graphene

A graphene and graphene dispersion technology, applied in the field of graphene, can solve problems such as hindering the commercial application of graphene oxide and graphene, unfavorable industrial production, long production cycle, etc., to avoid heating and cooling operations, and to achieve complete lamellae. High degree and complete lattice effect

Inactive Publication Date: 2017-02-22
SHANDONG OBO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, this method usually needs to go through low temperature, medium temperature and high temperature reaction process, frequent temperature rise and fall, multiple feeding, cumbersome operation, long production cycle, low intercalation efficiency, incomplete sheets, which is not conducive to industrial production, and serious obstacles commercial applications of graphene oxide and graphene

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  • Rapid preparation methods of graphene oxide and graphene
  • Rapid preparation methods of graphene oxide and graphene
  • Rapid preparation methods of graphene oxide and graphene

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preparation example Construction

[0054] The invention provides a kind of preparation method of graphene oxide, comprises the following steps:

[0055] A) under airtight conditions, react after graphite, intercalation agent and oxidizing agent are mixed, obtain reaction mixture;

[0056] B) after the reaction mixture obtained in the above steps is separated, a reaction product is obtained;

[0057] C) Exfoliating the reaction product obtained in the above steps in a dispersant to obtain a graphene oxide dispersion.

[0058] In the present invention, graphite, intercalation agent and oxidant are mixed and then reacted under airtight conditions to obtain a reaction mixture.

[0059] The present invention does not have special limitation to described graphite, gets final product with the graphite that is well known to those skilled in the art and is used for preparing graphene, and those skilled in the art can select and adjust according to actual production situation, product requirement and quality requirement...

Embodiment 1

[0091] Mix 1.0 g of 1000-mesh natural flake graphite with 3.5 g of potassium permanganate, add it into a 100 mL polytetrafluoroethylene pressure vessel, add a magnetic rotor, and add 30 mL of concentrated sulfuric acid (98%) at 0°C. Put the autoclave into the autoclave, seal the autoclave under normal pressure, and install a magnetic stirrer under the autoclave. Stirring was started for 5 min to allow the reactants to be fully mixed. Then the reaction vessel was heated to 60° C. for 1 h, then cooled to room temperature, and the pressure vessel was released to obtain a reaction mixture.

[0092] The obtained reaction mixture was centrifuged at 5000rmp for 5min, the clarified intercalation agent in the upper layer was recovered for use, the muddy product in the lower layer was poured into 50mL deionized water for dilution, and 5mL of 30% hydrogen peroxide was added to remove high-valent oxides, and the clear liquid was removed by centrifugation. Deionized water was centrifuged ...

Embodiment 2

[0100] Mix 1.0g of 5000-mesh natural flake graphite with 4.0g of potassium manganate and 1.0g of phosphorus pentoxide, add it to a 100mL polytetrafluoroethylene pressure vessel, add a magnetic rotor, and add 30mL of concentrated sulfuric acid (98%) at 0°C . Put the autoclave into the autoclave, seal the autoclave under normal pressure, and install a magnetic stirrer under the autoclave. Stirring was started for 5 min to allow the reactants to be fully mixed. Then the reaction vessel was heated to 50° C. for 1.5 h, and then cooled to room temperature. After the pressure was released, the pressure vessel was opened to obtain a reaction mixture.

[0101] The obtained reaction mixture was centrifuged at 5000rmp for 5min, the clarified intercalation agent in the upper layer was recovered for use, the muddy product in the lower layer was poured into 50mL deionized water for dilution, and 5mL of 30% hydrogen peroxide was added to remove high-valent oxides, and the clear liquid was r...

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Abstract

The invention provides a preparation method of graphene oxide. The method comprises the following steps: firstly, mixing graphite, an intercalator and an oxidizing agent under an airtight condition and then carrying out a reaction to obtain a reaction mixture; separating the reaction mixture obtained in the previous step to obtain a reaction product; finally, stripping the reaction product, obtained in the previous step, in a dispersing agent to obtain graphene oxide dispersion liquid. According to the preparation method, the intercalator is inserted into the parts among graphene sheet layers under the action of pressure and under the airtight condition, so that the acting force among layers is reduced, and the distances among the layers are increased; then, the oxidizing agent enters the parts among the graphene sheet layers and has an oxidation reaction, so that the graphene oxide is formed; due to the action of the pressure, the intercalator and the oxidizing agent are enabled to enter the parts among graphene layers more rapidly, and the reaction is promoted to be completed within a short time, so that first-order intercalating for the graphite is realized; furthermore, the preparation method is less in energy consumption in a reaction process, environmentally-friendly, convenient and fast to operate as well as safe and controllable, thus being more suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a rapid preparation method of graphene oxide and graphene. 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 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 properties, and can maintain good structural stability under high operating voltage and high current ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198C01B32/184C01B32/196
CPCC01B2204/02C01B2204/22C01P2004/03C01P2004/04
Inventor 程金杰张在忠钱路明胡兴华
Owner SHANDONG OBO NEW MATERIAL CO LTD
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