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Preparing method of oxidized graphene and high-conductivity graphene

A graphene and graphene dispersion technology, applied in the field of graphene, can solve problems such as affecting the integrity of products and affecting the electrical conductivity of graphene

Inactive Publication Date: 2017-04-19
SHANDONG OBO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These defects can greatly affect the integrity of the product, which in turn affects properties such as electrical conductivity of graphene

Method used

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  • Preparing method of oxidized graphene and high-conductivity graphene
  • Preparing method of oxidized graphene and high-conductivity graphene
  • Preparing method of oxidized graphene and high-conductivity graphene

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preparation example Construction

[0053] The invention provides a kind of preparation method of graphene oxide, comprises the following steps:

[0054] A) Under the condition of protective gas pressurization, after mixing graphite, intercalation agent and oxidant, carry out low-temperature reaction to obtain a reaction mixture;

[0055] B) after the reaction mixture obtained in the above steps is separated, a reaction product is obtained;

[0056] C) Exfoliating the reaction product obtained in the above steps in a dispersant to obtain a graphene oxide dispersion.

[0057] In the present invention, firstly, under the condition of pressurizing the protective gas, the graphite, the intercalation agent and the oxidant are mixed and reacted at low temperature to obtain the reaction mixture.

[0058] 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 i...

Embodiment 1

[0090] 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, and seal the autoclave. A magnetic stirrer is arranged below the autoclave. Introduce argon gas into the autoclave until the pressure rises to 8MPa and maintain the pressure, start stirring for 5min, so that the reactants are fully mixed. Then react the reactor at 5° C. for 36 h, and then release the pressure and open the autoclave to obtain the reaction product.

[0091] The obtained reaction product 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 cent...

Embodiment 2

[0098] 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, and seal the autoclave. A magnetic stirrer is arranged below the autoclave. Nitrogen gas was introduced into the autoclave until the pressure rose to 15MPa and the pressure was maintained, and the stirring was started for 5 minutes, so that the reactants were fully mixed. Then the reaction kettle was reacted at 0°C for 48h, and the pressure kettle was opened after the pressure was released to obtain the reaction product.

[0099] The obtained reaction product was centrifuged at 10000rmp 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 1mol / L sodium th...

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Abstract

The invention provides a preparing method of oxidized graphene. The preparing method comprises the following steps that at first, on the condition of pressurization of protective gas, graphite, an intercalator and an oxidizing agent are subjected to low-temperature reaction after being mixed, and a reaction mixture is obtained; then the reaction mixture obtained in the above step is separated, and then a reaction product is obtained; finally, the reaction product obtained in the above step is stripped in a dispersing agent, and oxidized graphene dispersing liquid is obtained. By the adoption of the low-temperature condition, the defect rate is reduced obviously, under the effect of pressure, the intercalator is inserted between graphene sheet layers, the acting force between the layers is reduced, and the distance between the layers is increased; then the oxidizing agent enters the portions between the graphene sheet layers, the oxidizing reaction is carried out, and thus oxidized graphene is formed; and due to the effect of the pressure, the intercalator and the oxidizing agent enter the portions between the graphene sheet layers faster, the reaction is promoted to be more complete within a short time, one-step intercalation to graphene is achieved, and then graphene powder with the low defect rate and high quality is obtained and prepared.

Description

technical field [0001] The invention belongs to the technical field of graphene, relates to a preparation method of graphene oxide and graphene, in particular to a preparation method of graphene oxide and high-conductivity graphene. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a 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 mainta...

Claims

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Application Information

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IPC IPC(8): C01B32/198C01B32/184C01B32/196
CPCC01B2204/02C01B2204/22C01B2204/32C01P2004/03C01P2004/04
Inventor 刘海波张在忠张聪胡兴华
Owner SHANDONG OBO NEW MATERIAL CO LTD
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