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Method for preparing graphene by electrochemically stripping graphite

A technology for exfoliating graphite and graphene, applied in the field of electrochemistry, can solve the problems of insufficient utilization of raw materials, loss of raw material mineralization, insufficient exfoliation of graphite raw materials, etc.

Pending Publication Date: 2022-04-29
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Comprehensive analysis of the impact of various electrolytes on graphene products in the whole process of electrochemical stripping, the effect of ionic liquid stripping is good, the product quality is high, but the price is expensive, the post-processing is complicated, and it is difficult to industrialize large-scale application
The biggest problem facing the intercalation and exfoliation of various metal ions or some complex ions in organic systems is the cost and effect of impurity removal, as well as the damage to the obtained graphene during the reaction process.
Water-based electrolytes also face problems such as insufficient stripping of graphite raw materials, insufficient utilization of raw materials, and loss of mineralization of raw materials.
All of these electrolytes have their own inevitable defects, and it has been difficult to realize the large-scale electrochemical preparation of graphene. Therefore, choosing a clean, environmentally friendly, efficient, cheap, and non-strong oxidation electrolyte has become the key to overcome the high electrochemical preparation. The key to quality graphene technology

Method used

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  • Method for preparing graphene by electrochemically stripping graphite
  • Method for preparing graphene by electrochemically stripping graphite
  • Method for preparing graphene by electrochemically stripping graphite

Examples

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Effect test

Embodiment 1

[0031] A method for electrochemically exfoliating graphite to prepare graphene, comprising the steps of:

[0032] 1) A graphite sheet with a weight of 5 g and a thickness of 1 mm was used as the anode, and a thermally cracked high-purity graphite of 4 cm*10 cm*1 mm was used as the cathode. The concentration of acetic acid in the mixed electrolyte was 0.2 M and sulfuric acid was 16 M. The electrolytic reaction was carried out to realize the electrochemical stripping of the anode material, and the molar concentration ratio of acetic acid to sodium sulfate was 1:32; in the electrolytic reaction, the distance between the anode and the cathode was 2 cm, and the voltage was constant at 7 V without stirring, resulting in Bubbles can form natural convection. During the peeling process, the electrolyte is kept at a constant temperature of 25°C through a circulating refrigeration system, and the graphite sheet is electrochemically peeled for 10 minutes to obtain a graphene precursor;

...

Embodiment 2

[0036] A method for electrochemically exfoliating graphite to prepare graphene, comprising the steps of:

[0037] 1) Highly oriented pyrolytic graphite with a weight of 5 g and a thickness of 1mm was used as the anode, a 4cm*10cm*1mm artificial graphite plate was used as the cathode, and a mixed solution of 0.05M malonic acid and 0.2M ammonium sulfate (500 ml) was used as the electrolysis Liquid, that is, the molar concentration ratio of malonic acid and ammonium sulfate is 1:4, and the electrolytic reaction is carried out to realize the electrochemical stripping of the anode material; in the electrolytic reaction, the distance between the anode and the cathode is 3cm, and the voltage is constant at 8V, without stirring , is still natural convection formed by electrolysis. During the stripping process, the temperature of the electrolyte is kept constant at 30°C through a circulating refrigeration system, and the highly oriented pyrolytic graphite is electrochemically stripped f...

Embodiment 3

[0041] A method for electrochemically exfoliating graphite to prepare graphene, comprising the steps of:

[0042] 1) Use flake graphite with a weight of 5 g and a thickness of 1mm as the anode, a high-purity graphite plate of 4cm*10cm*1mm as the cathode, and a mixed solution of 0.1M formic acid and 1M nitric acid (500 ml) as the electrolyte, namely formic acid The molar concentration ratio with nitric acid is 1:10, and the electrolytic reaction is carried out to realize the electrochemical stripping of the anode material. In the electrolysis reaction, the distance between the anode and the cathode is 1cm, the voltage is constant at 5V, no stirring, natural convection in the electrolytic cell, and the temperature of the electrolyte is kept constant at 20°C through a circulating refrigeration system, and the flake graphite is electrochemically stripped for 2h to obtain Graphene precursor;

[0043] 2) Filter the electrolyte reacted in step 1) with a filter bucket to quickly reco...

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Abstract

The invention discloses a method for preparing graphene by electrochemically stripping graphite, which comprises the following steps: 1) taking a graphite material as an anode material, taking a mixed solution of micromolecular organic acid and inorganic acid or soluble sulfate as an electrolyte, and applying voltage to an anode in an electrolytic tank to realize electrochemical stripping of the graphite material; and 2) carrying out solid-liquid separation on a solid-liquid mixture obtained by electrolysis, washing to remove residual electrolyte so as to extract a graphene precursor dispersed in the electrolyte, drying the extracted graphene precursor, and carrying out fragmentation separation to obtain a graphene sample. According to the method, the graphite stripping effect can be improved, the raw material loss is reduced, the mass ratio of graphene is high, and the method is environment-friendly, energy-saving and low in cost.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a method for electrochemically exfoliating graphite to prepare graphene. Background technique [0002] Graphene is composed of single layer sp 2 Honeycomb-like hexagonal planar two-dimensional crystals formed by the arrangement of hybridized carbon atoms. On the two-dimensional plane, sp 2 The hybridized carbon atoms are connected to the adjacent three carbon atoms through strong σ bonds, and the remaining P electron orbitals are perpendicular to the graphene plane, forming large π bonds with the surrounding atoms, so that graphene has good electrical and thermal conductivity and mechanical properties. performance, electron mobility up to 200,000 cm 2 / (V·s), the electrical conductivity can reach 106 S / m, the thermal conductivity can reach 5000 W / (m·K), and the strength can reach 130 GPa. These excellent properties of graphene make it have great potential application ...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/04
Inventor 蒋卷涛丘志安李庆余黄如冰缪剑文王红强黄有国郑锋华
Owner GUANGXI NORMAL UNIV
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