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Method for preparing graphene

A technology of graphene and graphite powder, which is applied in the field of graphene preparation by steam explosion, can solve the problems of difficulty in industrial scale preparation, limited graphite exfoliation, and many repeated steps in preparation, so as to achieve abundant raw materials, high exfoliation effect, Efficient peeling effect

Active Publication Date: 2014-11-19
余美群
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 201110021033.0, "Method for preparing graphene with supercritical fluid", this method repeatedly uses high pressure (10-100 MPa) and temperature (200-700°C), and there are many repeated steps in the preparation, making it difficult to achieve industrial-scale preparation
However, the above methods all use rapid pressure relief, which cannot achieve instantaneous (millisecond level) pressure relief, so it is impossible to instantly (millisecond level) release all the materials in the high-pressure container, and the stripping effect on graphite is limited.

Method used

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Examples

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Effect test

Embodiment 1

[0043] Inject 25g of graphite powder and 0.5g of n-butanol into the autoclave to mix the two evenly, select a positive arched rupture disc, seal the autoclave well, and pour 50g of propane into the autoclave after vacuuming; the mass ratio of graphite to propane 1:2, the mass ratio of n-butanol to propane is 1:100, control the temperature of the autoclave to 105°C, stay at this temperature for 15 minutes, then slightly increase the temperature and pressure (you can also maintain the same temperature, use compressor to increase the pressure), when the pressure in the autoclave exceeds the pressure 5MPa that the bursting disc can withstand, the bursting disc bursts, and all the materials rush out instantly, and a long cylindrical stainless steel collector with a port at the end is used to collect the materials. The interface is connected to the solvent recovery system, and the collected materials are put into NN-dimethylformamide, stirred for 5 minutes, and left to stand for 12 h...

Embodiment 2

[0045] Inject 60g of graphite powder and 4.8g of NN-dimethylformamide into the autoclave to mix the two evenly, select a reverse arched rupture disc, seal the autoclave well, and pour 240g of propane into the autoclave after vacuuming, graphite and The mass ratio of propane is 1:4, and the mass ratio of dimethylformamide to propane is 2:100; the temperature of the autoclave is controlled at 120°C, and the temperature is kept at this temperature for 5 minutes, and then the temperature is increased slightly, and the pressure is increased (it can also be maintained Keep the temperature constant, use a compressor to increase the pressure), when the pressure in the autoclave exceeds the pressure 6MPa that the bursting disc can withstand, the bursting disc bursts, and all the materials rush out instantly, and are collected by a long cylindrical stainless steel collector with an interface at the end Materials, the tail port of the collector is connected to the solvent recovery system,...

Embodiment 3

[0047] Inject 60g of graphite powder and 5.4g of N-methylpyrrolidone into the autoclave and mix them evenly. Select a flat bursting disc and seal the autoclave well. After vacuuming, pour 180g of propane. The mass ratio of graphite to propane is 1:3 , the mass ratio of methylpyrrolidone to propane is 3:100, control the temperature of the autoclave to 110°C, stay at this temperature for 10 minutes, then slightly increase the temperature and pressure (you can also maintain the same temperature and increase the pressure with a compressor ), when the pressure in the autoclave exceeds the pressure 8 MPa that the rupture disc can withstand, the rupture disc bursts, and all the materials rush out instantly, and a long cylindrical stainless steel collector with a port at the end is used to collect the materials, and the tail port of the collector is connected to the solvent recovery The system is connected, the collected materials are put into the autoclave again, and the above operati...

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Abstract

Disclosed is a method for preparing graphene. In particular, the method comprises: using n-hexane or propane as a supercritical solvent, filling graphite powder or graphite powder and a cosolvent into an autoclave, sealing the autoclave by selecting an appropriate rupture disk, adding n-hexane or propane after the autoclave is vacuumized, keeping in a supercritical state for a period of time at a temperature and a pressure, then increasing the temperature and the pressure slightly or increasing the pressure alone,, and a collector collecting rushed-out materials instantly for treatment to prepare a graphene product after the rupture disk bursts when the pressure exceeds the pressure which the rupture disk can bear. In the present method, pressure relief occurs in milliseconds, and thereby efficient strip of graphite can be achieved. The method belongs to a physical process, does not cause large damage on the structure of graphene, is simple in the preparation process, does not require a large quantity of inorganic acids and oxidants, and is free of "three wastes". The prepared graphene crystal is intact in structure, good in quality, and capable of achieving large-scale industrial production of graphene.

Description

technical field [0001] The invention relates to a method for preparing graphene products, in particular to a method for preparing graphene by means of steam explosion. Background technique [0002] The appearance of graphene has aroused great repercussions in the scientific community. Because of its extraordinary electrical conductivity, strong strength and toughness, good light transmission, etc., it has triggered a strong research boom in the field of modern electronic technology. Graphene is both the thinnest material and the strongest, with a breaking strength a hundred times higher than the best steel. At the same time, it has good elasticity, and the stretching range can reach 20% of its own size. Although the discovery time of graphene is very short and it is still in the research stage, its unique physical structure and excellent mechanical and electrical properties make it have broad application prospects in the fields of nanoelectronics, microelectronics, composit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
CPCC01B31/04C01B32/19Y02P20/54
Inventor 余检明
Owner 余美群
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