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A kind of preparation method of graphene oxide

A graphene and graphite technology, applied in the field of graphene oxide preparation, can solve problems such as difficulty in dispersion, difficulty in large-scale production, and restricting the development and application of graphene

Active Publication Date: 2019-02-12
SHANDONG OBO NEW MATERIAL CO LTD
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Problems solved by technology

[0003] Graphene oxide is a derivative of graphene. Although graphene has excellent properties, its surface is inert, its reactivity is low, and it is difficult to disperse in solvents such as water. The force is easy to gather together, this shortcoming limits the development and application of graphene
Compared with pure graphene, the surface of graphene oxide has oxygen-containing functional groups. Although the conductivity is much lower than that of graphene, its surface activity is easier to react with other substances.
[0004] The traditional synthesis of graphene oxide needs to be exfoliated from graphite oxide into graphene oxide by ultrasonic treatment, but it takes a long time to exfoliate graphite oxide into graphene oxide by ultrasonic alone, and it is difficult for large-scale production
At the same time, the single-layer rate of graphene oxide in the traditional method is low, and the washing step mostly adopts the sedimentation method, which brings difficulties to large-scale production

Method used

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preparation example Construction

[0028] The invention provides a kind of preparation method of graphene oxide, comprises the following steps:

[0029] A) Mix and react concentrated sulfuric acid, graphite and fuming nitric acid, then lower the temperature, add potassium permanganate, add water to quench the reaction after the mixed reaction, and finally add hydrogen peroxide to obtain graphene oxide.

[0030] Wherein, the graphite is preferably natural flake graphite; the particle size of the natural flake graphite is preferably 5-20 μm, more preferably 5-15 μm, more preferably 8-12 μm, most preferably 10 μm; the graphite and concentrated sulfuric acid The mass ratio of graphite is preferably 1:(60-80), more preferably 1:(65-75); in some embodiments provided by the present invention, the mass ratio of graphite to concentrated sulfuric acid is preferably 1:73.44; In other embodiments provided by the present invention, the mass ratio of graphite to concentrated sulfuric acid is preferably 1:68.85; the mass rati...

Embodiment 1

[0041] Disperse 20g (1.667mol) of natural flake graphite with a particle size of 10μm in 800ml of 98% concentrated sulfuric acid at room temperature, add 10ml of fuming nitric acid after stirring for 1 hour, and add 80g of permanganic acid to control the reaction temperature below 10°C after reacting for 14 hours Potassium, react at a constant temperature of 30°C for 72 hours. Use a constant pressure dropping funnel to control the temperature below 60°C and add 1.2L of high-purity water dropwise. Raise the temperature to 90°C to react for 2.5h, cool down to below 60°C, and add 40ml of hydrogen peroxide. After natural cooling, clean with ceramic membrane cleaning equipment, and obtain a single-layer graphene oxide solution after 20KHz ultrasound for 3 hours.

[0042] figure 1 It is a photo of the appearance of the graphene oxide solution obtained in Example 1.

[0043] Utilize scanning electron microscope to analyze the graphene oxide obtained in embodiment 1, obtain its scann...

Embodiment 2

[0046] Disperse 60g (5mol) of natural flake graphite with a particle size of 10μm in 2.25L of 98% concentrated sulfuric acid at room temperature, add 30ml of fuming nitric acid after stirring for 1 hour, and add 240g of high manganese after 14 hours of reaction to control the reaction temperature below 10°C Potassium acid, react at a constant temperature of 30°C for 72 hours. Use a constant pressure dropping funnel to control the temperature below 60°C and add 2.25L of high-purity water dropwise. Raise the temperature to 90°C and react for 2.5 hours, then lower the temperature to below 60°C, and add 125ml of hydrogen peroxide. After natural cooling, clean with ceramic membrane cleaning equipment, and obtain a single-layer graphene oxide solution after 20KHz ultrasound for 3 hours.

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Abstract

The invention provides a method for preparing graphene oxide, comprising the following steps: A) mixing concentrated sulfuric acid, graphite and fuming nitric acid, then cooling the temperature, adding potassium permanganate, adding water after the mixing reaction to quench the reaction, and finally adding Hydrogen peroxide to obtain graphene oxide. Compared with the prior art, the present invention adopts fuming nitric acid as the intercalating agent, so that the obtained graphene oxide monolayer rate is higher.

Description

technical field [0001] The invention belongs to the technical field of graphene oxide, in particular to a preparation method of graphene oxide. Background technique [0002] Graphene is the thinnest and toughest material that people have discovered so far. It also has high electrical and thermal conductivity, making it play a huge role in many fields such as electrochemistry and biomedicine. [0003] Graphene oxide is a derivative of graphene. Although graphene has excellent properties, its surface is inert, its reactivity is low, and it is difficult to disperse in solvents such as water. The force is easy to gather together, which limits the development and application of graphene. Compared with pure graphene, the surface of graphene oxide has oxygen-containing functional groups. Although the conductivity is much lower than that of graphene, its surface activity is easier to react with other substances. [0004] The traditional synthesis of graphene oxide needs to exfolia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/198
CPCC01B2204/02C01P2002/72C01P2004/03
Inventor 程金杰张在忠吴开付
Owner SHANDONG OBO NEW MATERIAL CO LTD
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