Method of preparing graphene by using supercritical CO2 assisted liquid phase stripping

A technology of CO2 and auxiliary liquid, which is applied in the production of graphene, bulk chemicals, nano-carbon, etc., can solve the problems of poor quality and low production efficiency of graphene, and achieve good structural integrity, green production process, and preparation The effect of simple process

Active Publication Date: 2019-12-10
霖和气候科技(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems of low production efficiency and poor quality of graphene, the present invention provides a method using supercritical CO 2 A method for quickly and efficiently preparing high-quality graphene by assisting liquid phase exfoliation. The method is simple to operate, mild in conditions, and requires less organic solvent 2 Environmental protection, low cost, therefore, this method is a technology for industrial production of graphene with practical application prospects

Method used

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  • Method of preparing graphene by using supercritical CO2 assisted liquid phase stripping

Examples

Experimental program
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Effect test

Embodiment 1

[0024] (1) Weighing 60 mg of natural graphite powder and 60 mL of NMP to form a reaction solution with a concentration of 1 mg / mL, and ultrasonically mixing in a water bath for 10 minutes;

[0025] (2) Add the solution to figure 1 In the reaction kettle shown, after heating the reaction kettle to 40°C through the control module, turn on the mechanical stirring (1000rpm) and use the booster pump to pump the CO in the carbon dioxide bottle 2 Pump it into the reaction kettle, and the reaction will start after the pressure reaches 12MPa;

[0026] (3) After reacting for 2 hours, take out the reactor and place it in a water bath to cool to below 25°C, open the exhaust valve to let the CO 2 go through figure 1 After washing the bottle shown, pour the solution into the beaker;

[0027] (4) Ultrasonic disperse the taken-out solution for 45 minutes, pour it into a centrifuge tube and centrifuge at 2500rpm for 30 minutes, and then take the supernatant to obtain a graphene solution wit...

Embodiment 2

[0029] (1) Weigh 210mg of expandable graphite powder and 70mL of NMP to form a reaction solution with a concentration of 3mg / mL, and ultrasonically mix in a water bath for 5 minutes;

[0030] (2) Add the solution to figure 1 In the reaction kettle shown, after heating the reaction kettle to 50°C through the control module, turn on the magnetic stirring (1500rpm) and use the booster pump to remove the CO in the carbon dioxide bottle. 2 Pump it into the reaction kettle, and the reaction will start after the pressure reaches 16MPa;

[0031] (3) After reacting for 4 hours, take out the reaction kettle and place it in a water bath to cool to below 25°C, open the exhaust valve to drain the CO 2 go through figure 1 The indicated scrubber bottle is drained, and the solution is poured into a beaker;

[0032] (4) Ultrasonic disperse the taken-out solution for 45 minutes, pour it into a centrifuge tube and centrifuge at 2500 rpm for 30 minutes, and then take the supernatant to obtain ...

Embodiment 3

[0034] (1) Weigh 300mg of expandable graphite powder and 60mL of DMF to form a reaction solution with a concentration of 5mg / mL, and ultrasonically mix in a water bath for 15 minutes;

[0035] (2) Add the solution to a preheated to 80°C figure 1 In the reactor, open mechanical stirring (2000rpm) and utilize figure 1 The booster pump in the reactor feeds CO into the reactor 2 , the reaction starts after the pressure reaches 20MPa;

[0036] (3) After reacting for 6 hours, take out the reactor and place it in a water bath to cool to below 25°C, open the exhaust valve to drain the CO 2 go through figure 1 The washing bottle is discharged, and the solution is poured into the beaker;

[0037] (4) Ultrasonic disperse the taken-out solution for 60 minutes, pour it into a centrifuge tube and centrifuge at 2500 rpm for 30 minutes, and then take the supernatant to obtain a graphene solution with a concentration of 0.46 mg / mL. Graphene sheets with less than ten layers accounted for 8...

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Abstract

The invention relates to a method of preparing graphene by using supercritical CO2 assisted liquid phase stripping. The method comprises the steps that graphite powder and an organic solvent are evenly mixed and then added into a preheated reaction still, CO2 is introduced into the reaction still, continuous stirring is conducted, and a reaction starts to be conducted after the preset supercritical pressure is reached; and after the reaction is completed, the reaction still is cooled to be the CO2 critical point or below, the CO2 is discharged, a solution is taken out to be subjected to ultrasonic treatment and then centrifuged, then supernate is taken, and thus a graphene solution is obtained. The method is easy to operate, mild in condition and high in product quality, the CO2 is environmentally friendly and low in cost, and the using amount of the organic solvent is small; and therefore, the method is a technology, with actual application prospects, for producing the graphene in industrial and environmentally friendly modes.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a method of using supercritical CO 2 A method for preparing graphene with assisted liquid phase exfoliation. Background technique [0002] As a member of the family of two-dimensional nanomaterials, graphene has a typical sheet structure, with horizontal dimensions ranging from several nanometers to several micrometers or even larger, but the thickness is only one or several atoms thick. Although the search for two-dimensional materials dates back decades, it was not until 2004 that marked the birth of graphene. How to achieve low-cost and large-scale preparation of high-quality graphene is still one of the main bottlenecks restricting the development of graphene industrialization at this stage. At present, the commonly used graphene preparation methods mainly include redox method, chemical vapor deposition (CVD) method and liquid phase exfoliation method. However...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01P2004/04C01P2004/62Y02P20/54
Inventor 刘立熙朱亮亮肖航陈曦
Owner 霖和气候科技(北京)有限公司
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