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A method for preparing graphene by continuous exfoliation in a dry powder state using an alternating electric field

An alternating electric field and graphene technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex post-processing process, increased production cost, and low graphene output, so as to retain physical properties and avoid Effect of lattice damage, simple and fast operation

Active Publication Date: 2018-03-13
齐河智谷产业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the graphene prepared by this method cannot completely avoid the surface adsorption of metal powder, which reduces the organic wettability of graphene, which is not conducive to the application of graphene in rubber and plastics.
[0009] In summary, the current electric field exfoliation graphene method faces two major problems: one is the introduction of impurity atoms and ions during the exfoliation process, which affects the product performance of graphene; the other is the low output of periodic alternating electric field exfoliation graphene , only graphite in the direction parallel to the electric field can be peeled off, the production cycle is long, it is not suitable for large-scale industrial production, and the dispersion of graphene products is poor, which leads to complicated post-processing processes and increased production costs.
Therefore, there is currently no scheme for the continuous exfoliation of graphene under dry powder conditions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035](1) Take flake graphite powder with a particle size less than or equal to 10 μm as a raw material, ultrasonicate for 1 minute in a HF solution with a solution concentration of 3.5%, remove impurities on the surface of the flake graphite powder, and finally rinse with deionized water to remove HF residual liquid. The purity of argon is 99.9%, the ambient pressure of argon is 100Pa, and the flake graphite powder is dried under the protection of argon, and the drying temperature is 90°C.

[0036] (2) Put the flake graphite powder material and tetramethylammonium bicarbonate into a co-rotating twin-screw group with a length-to-diameter ratio of 60 / 1 and a screw diameter of 20 mm according to a mass ratio of 1:0.01, and set up a continuous screw reaction The temperature of the extruder is 350°C, the extrusion pressure is 20MPa, and the surfactant and the graphite powder are uniformly mixed and peeled off to obtain a surface-modified flake graphite powder;

[0037] (3) The noz...

Embodiment 2

[0040] (1) Take highly oriented graphite powder with a particle size less than or equal to 10 μm as a raw material, ultrasonicate for 0.5 minutes in an HF solution with a solution concentration of 5%, remove impurities on the surface of the highly oriented graphite powder, and finally rinse with deionized water to remove HF residual liquid , the purity of argon gas is 99.9%, the ambient pressure of argon gas is 1000Pa, and the highly oriented graphite powder is dried under the protection of argon gas for use, and the drying temperature is 90°C.

[0041] (2) The high-oriented graphite powder material and tetraethylammonium bicarbonate are mixed according to the mass ratio of 1:0.03 and put into a reverse meshing five-screw group with an aspect ratio of 70 / 1 and a screw diameter of 150mm, and a continuous screw is set The temperature of the reaction extruder is 60°C, and the extrusion pressure is 20MPa, and the surfactant and the graphite powder are uniformly compounded to obtain...

Embodiment 3

[0045] (1) Take expanded graphite powder with a particle size less than or equal to 10 μm as a raw material, ultrasonically 0.7 minutes in a HF solution with a solution concentration of 4%, remove impurities on the surface of the expanded graphite powder, and finally rinse with deionized water to remove HF residual liquid. The purity of argon is 99.9%, the ambient pressure of argon is 500Pa, the expanded graphite powder is dried under the protection of argon, and the drying temperature is 85°C.

[0046] (2) The expanded graphite powder material and sodium dodecylsulfonate are mixed according to the mass ratio of 1:0.05 and put into a co-rotating four-screw group with a length-to-diameter ratio of 55 / 1 and a screw diameter of 70mm, and a continuous screw is set. The temperature of the reaction extruder is 150°C, and the extrusion pressure is 30 MPa, and the surfactant is uniformly compounded with the expanded graphite powder material to obtain a surface-modified expanded graphit...

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Abstract

The invention provides a method for preparing graphene by continuously peeling under a dry powder state by utilizing an alternating electric field. The method comprises the following steps: firstly, dispersing graphite powder and surfactant in advance; applying the alternating electric field between a pair of parallel bar-shaped metal plates; quickly passing the pre-dispersed graphite powder through two parallel bar-shaped metal plate areas in a smog form by utilizing a high-pressure air flow; quickly vibrating and peeling the graphite powder into graphene under the interactive vibration effect of a horizontal high-pressure air shock wave and a longitudinal alternating electric field formed between the two metal plates, thereby realizing the high-quality graphene prepared by continuously peeling under the dry powder state. According to the method, no peeling agent is introduced, the surface of the peeled graphite is clean, the surface structure of the graphene is not damaged in the high-speed air flow peeling process, the peeling efficiency is high, the physical properties of the graphene are reserved, the application scope of the products is wider, the operation is simple and quick, the cost is low, the preparation efficiency is high and the large-scale industrial preparation of graphene is benefited.

Description

technical field [0001] The invention relates to the field of graphene material preparation, in particular to a method for continuously exfoliating graphene in a dry powder state by using an alternating electric field. Background technique [0002] Carbon exists widely in nature, and its unique properties and diverse forms are gradually discovered with the progress of human civilization. There are many allotropes of carbon, the most well-known ones are sp2 hybridized graphite and sp3 hybridized diamond. The discovery of Fullerene in 1985 and the discovery of carbon nanotubes in 1991 expanded the scope of carbon allotropes. In 2004, another allotrope of carbon with an ideal two-dimensional structure and peculiar electrical properties—graphene was successfully prepared, which triggered a new wave of research on carbonaceous materials. [0003] Graphene is a two-dimensional carbon nanomaterial composed of a layer of carbon atoms. It is the thinnest two-dimensional material kno...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/192
CPCC01B2204/04
Inventor 陈庆王镭迪曾军堂
Owner 齐河智谷产业发展有限公司
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