Method for preparing graphene oxide

A technology of graphene and graphite, which is applied in the field of graphene oxide preparation, can solve the problems of many defects, decreased comprehensive performance, and unsuitability for large-scale production, and achieve the goals of reducing energy consumption, increasing yield, and reducing by-products and impurities Introduced effects

Active Publication Date: 2013-10-02
CHONGQING JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thermal expansion method and reduction method of graphite oxide in the above method can prepare graphene oxide and graphene in large quantities, but due to the action of a strong oxidant, there are many defects in the structure and the overall performance decreases; methods such as crystal epitaxial growth and chemical vapor deposition are suitable for preparation Large-area graphene is not suitable for the preparation of large-volume, small-area (less than 1mm2 per sheet) graphene or graphene oxide required in many fields

Method used

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preparation example Construction

[0016] In the preparation method of graphene oxide in this embodiment, graphene oxide is prepared by combining mechanical action and oxidation reaction from graphite raw materials.

[0017] In this embodiment, graphene oxide is prepared by mechanical action after mixing the oxidizing agent and graphite raw material; first chemical reaction and then mechanical action, let the graphite raw material react partly first, and then perform mechanical action, step by step to make the reaction more thorough, graphite When the carbon sheets are staggered and slipped under mechanical action, the molecular bonds are broken, and the oxidant molecules are more easily inserted between the carbon sheets, and the distance between the carbon sheets is increased due to chemical oxidation and then peeled off. The thermal effect in this process can also promote the reaction rate. And strengthen the mass transfer, so that the yield of graphene oxide is better.

[0018] In this embodiment, graphite ...

Embodiment 1

[0027] Graphene oxide is prepared by mechanical action after mixing oxidant and graphite raw materials, first oxidation reaction and then mechanical action: mix graphite and oxidant with a mass ratio of graphite: oxidant: grinding aid = 1:1:0.2, and mix at a certain temperature , Under pressure, conditions such as stirring, light, and radiation can be applied to react for a certain period of time and then put into a ball mill for 40 minutes to obtain a graphene oxide mixture, which is put into water, stirred, left to stand, and separated; a little stirring can be observed. Graphene oxide solution or suspension in golden yellow, light brown-dark brown-black, cyan-dark green and other colors, unreacted graphite or grinding aid is deposited at the bottom. The obtained graphene oxide solution or suspension can be stably suspended in a centrifuge at 16000 rpm.

[0028] In this embodiment, the graphite raw material is flake graphite, and the flake graphite can be replaced by one of ...

Embodiment 2

[0035] Graphene oxide is prepared by mechanical action after mixing oxidant and graphite raw materials: mix graphite and oxidant with a mass ratio of graphite: oxidant = 1:0.5, and react under conditions such as stirring, light, and radiation at a certain temperature and pressure After a certain period of time, put it into a ball mill and mill it for 100 minutes to obtain a graphene oxide mixture, put it into water, stir, let it stand, and separate it; after a little stirring, it can be observed that it is golden, light brown-dark brown-black, cyan ——Graphene oxide solution or suspension with dark green and other colors, unreacted graphite or medium deposited at the bottom. The obtained graphene oxide solution or suspension can be stably suspended in a centrifuge at 16000 rpm.

[0036] In this embodiment, the graphite raw material is expanded graphite. In this embodiment, the expanded graphite is replaced by one of flake graphite, unexpanded graphite, and graphite powder in th...

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Abstract

The invention discloses a method for preparing a graphene oxide. The graphene oxide is prepared from a graphite raw material in a mode that mechanical action and oxidation reaction are combined. The method comprises the following steps of: mixing an oxidant with the graphite raw material, subsequently preparing the graphene oxide by employing mechanical action, adding the oxidant after the graphite raw material is subjected to mechanical action so as to prepare the graphene oxide, and adding the oxidant after the graphite raw material is subjected to mechanical action so as to carry out oxidation reaction and prepare the graphene oxide. According to the method, strong acids and strong oxidants required in a chemical oxidation method are abandoned, so that the introduction of byproducts and impurities is greatly reduced, the separation and the purification are convenient, the process procedures are reduced, the treatment time of a mechanical milling method is shortened, the energy consumption is reduced, and the yield is greatly increased. With the combination of the two methods, the graphene oxide can be prepared at one step within the shortest time, the yield is greater than 20%, the graphite oxide can be stably suspended under a centrifugal condition of 16,000rpm without ultrasound, and the method has the characteristics of rapidness, simplicity, convenience, environmental-protection and efficiency.

Description

technical field [0001] The invention relates to graphene, in particular to a preparation method of graphene oxide. Background technique [0002] Graphene oxide is the oxide of graphene. Graphene oxide is a new type of carbon material with excellent performance, which has a high specific surface area and abundant functional groups on the surface. Graphene oxide is generally obtained by oxidation of graphite with strong acid. There are mainly three methods for preparing graphite oxide: Brodie method, Staudenmaier method and Hummers method. Among them, the timeliness of the preparation process of the Hummers method is relatively good and the preparation process is also relatively safe, which is currently the most commonly used one. It uses potassium permanganate in concentrated sulfuric acid and graphite powder to undergo oxidation reaction to obtain brown graphite flakes with derivatized carboxylic acid groups on the edges and mainly phenolic hydroxyl groups and epoxy groups...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C01B32/198
Inventor 周超李力袁小亚何丽红何钊
Owner CHONGQING JIAOTONG UNIVERSITY
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