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Chemical-additive-free and safe preparation method of graphene oxide

A chemical and graphene technology, applied in the field of electrochemical preparation of graphene oxide, can solve problems such as safety risks and complex preparation processes, and achieve the effects of easy regulation, high purity and simple operation.

Pending Publication Date: 2021-01-01
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production process of graphene oxide requires two acid pools, which contain strong acid with significant concentration, complicating the production process
Although residual acid can be recycled, it inevitably poses safety risks to people, working conditions and the natural environment

Method used

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  • Chemical-additive-free and safe preparation method of graphene oxide
  • Chemical-additive-free and safe preparation method of graphene oxide
  • Chemical-additive-free and safe preparation method of graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]Under normal temperature and pressure conditions, the solution in the electrolytic cell is pure water with a conductivity of 24.8μs / cm, a flexible graphite paper material with a carbon content of 99.8% by weight is used as the anode, platinum sheets are used as the cathode, and the distance between the two electrodes is 0.170mm. A cellulose porous membrane is blocked by 0.159mm, and the bias voltage is +5V; when the applied voltage is about 60s, it can be observed that graphite oxide particles are attached to the anode. After 20s ultrasonic peeling, a yellow graphene oxide solution (figure 2 a) The carbon to oxygen ratio reaches 2:1. The solution is then freeze-dried to directly obtain graphene oxide powder.

[0029]Under a scanning transmission electron microscope (Hitachi STEM SU9000, acceleration voltage 20KV), the secondary electron morphology of graphene oxide obtained by the above process (image 3a), transmission electron micrograph (image 3b), the atomic force micrograph (...

Embodiment 2

[0031]This embodiment has the same process as the first embodiment. The difference is that the electrode spacing is 10mm, the diaphragm thickness is 0mm, and the bias voltage is +60V. When the voltage is applied for about 120 hours, a large amount of graphite oxide particles can be found in the solution. The solution was peeled off ultrasonically for 20 seconds to obtain a darker color graphene oxide solution (figure 2 b). STEM electron microscopy characterization was performed under the same conditions, and the results were consistent with Example 1.

Embodiment 3

[0033]This embodiment has the same process as the first embodiment. The difference is that the electrode spacing is increased to 10mm, the diaphragm thickness is 0mm, and the voltage application time is increased to 180 hours.

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Abstract

The invention discloses a chemical-additive-free and safe preparation method of graphene oxide, and belongs to the field of graphene preparation. Graphite processed products such as graphite coiled materials, strips and blocks are used as a raw material, andundergo two processes of liquid-phase electrochemical treatment and mechanical treatment, oxidation and stripping to prepare thethe graphene oxide. The electrochemical process is characterized in that in a water system without addition of any acid, alkali, salt or other electrolytes, a graphite material is taken as an anode, is electrifiedwith direct current under a soaking condition, and participates in oxidation and intercalation of graphite under the driving of an electric field to form a graphite oxide intermediate material; and inthe mechanical treatment, graphite oxide is subjected to low-intensity mechanical stripping, such as ultrasonic treatment to obtain the graphene oxide. According to the method, post-treatment processes such as washing are not needed, and energy consumption is greatly reduced; the obtained product does not contain any impurity such as metal ions, and has the advantages of controllable graphene oxidation degree, safe process, no pollution and the like.

Description

Technical field[0001]The invention belongs to the field of carbon material preparation, and specifically relates to an electrochemical preparation method of graphene oxide.Background technique[0002]Graphene oxide is an important precursor for the large-scale production and application of graphene. From the mid-nineteenth century to the present, there are four main methods for preparing graphene oxide core proposed by domestic and foreign scholars: Brodie (KClO3-HNO3) Method, Staudenmaier (KClO3-HNO3-H2SO4) Method, Hummers (KMnO4-H2SO4-NaNO3) Method and electrochemical method. Based on the previous three wet chemical oxidation methods, this field has derived a large number of improved methods suitable for raw materials with different sizes and texture structures (see the review article Analysis Sun L. Structure and Synthesis of Graphene Oxide. "Chinese Journal of Chemical Engineering", 2019, pages 2251-2260). These methods have a common principle, that is, in order to overcome the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198
CPCC01B32/198
Inventor 孙凌
Owner BEIJING UNIV OF TECH
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