A kind of graphene material based on solid-phase mechanochemical reactor and preparation method thereof

A chemical reactor, graphene technology, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve the problem that batch production technology and high performance cannot be balanced, large-scale production cannot be achieved, and preparation conditions are harsh, etc. problem, to achieve the effect of low production cost, good heat, and mild reaction conditions

Active Publication Date: 2019-07-23
SICHUAN UNIV
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  • Application Information

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Problems solved by technology

The preparation process is simple, the obtained graphene is of high quality, can grow in a large area, and is easier to transfer to various substrates. This method is now widely used in the preparation of graphene transistors and transparent conductive films, and has gradually become a high-quality material for the preparation of high-quality graphene. An important method for high-quality graphene, but the conditions for its preparation are extremely harsh, the equipment used is a high-temperature tube furnace, and the cost is extremely high, making it impossible to achieve large-scale production
[0008] At present, the patents on graphene production are mainly for the improvement of the chemical redox method, which still cannot fundamentally solve the problem of redox reaction. For example, the Chinese patent "Preparation of High-quality Graphene with Controllable Layer Method "(CN103342358A) uses the Hummers method to prepare graphene by regulating the degree of oxidation and dissociation of graphene. In this method, a mixed gas of hydrogen and argon is used to reduce graphene oxide at 300-1000 ° C. There is a reduction time Long time, high requirements for equipment, dangerous reaction and high cost
[0009] Since the quality, output and application of graphene are closely related to the preparation method of graphene, the current production technology cannot balance mass production and high performance

Method used

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  • A kind of graphene material based on solid-phase mechanochemical reactor and preparation method thereof
  • A kind of graphene material based on solid-phase mechanochemical reactor and preparation method thereof
  • A kind of graphene material based on solid-phase mechanochemical reactor and preparation method thereof

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Effect test

Embodiment 1

[0051] Embodiment one uses the inventive method to prepare graphene

[0052] Dry graphite flakes (325 mesh, carbon content>99%) and sodium chloride at a temperature of 90° C. for 4 hours, weigh 30 g of graphite flakes and 1 kg of sodium chloride and add them to a high-speed mixer to mix evenly, then place them in a solid In the phase force chemical reactor, the cooling circulating water at room temperature is fed into the cooling device during the milling process, and the temperature of the disc surface is controlled at 25°C, the pressure is 15KN, the speed is 150 rpm, and the circular grinding is performed 50 times to obtain graphene. Composite with NaCl. Transfer the graphene and sodium chloride composite material into distilled water, remove the sodium chloride therein, and then treat the obtained product with 1mol / L hydrochloric acid for 12 hours, and centrifuge and wash for 20 minutes at a speed of 8000 rpm to obtain The precipitate was vacuum-dried at 60°C for 12 hours ...

Embodiment 2

[0053] Embodiment two uses the method of the present invention to prepare graphene

[0054] Dry graphite flakes (325 mesh, carbon content>99%) and sodium chloride at a temperature of 90° C. for 4 hours, weigh 30 g of graphite flakes and 1 kg of sodium chloride and add them to a high-speed mixer to mix evenly, then place them in a solid In the phase force chemical reactor, cooling circulating water at room temperature is introduced during the milling process, and the temperature of the disc surface is controlled at 30°C, the pressure is 20KN, the speed is 150 rpm, and the grinding cycle is 50 times to obtain graphene and chloride. Sodium composites. Transfer the graphene and sodium chloride composite material into distilled water, remove the sodium chloride therein, and then treat the obtained product with 1mol / L dilute sulfuric acid for 12 hours, and centrifuge and wash it for 20 minutes at a speed of 8000 rpm The obtained precipitate was vacuum-dried at 60° C. for 12 hours t...

Embodiment 3

[0055] Embodiment three uses the method of the present invention to prepare graphene

[0056] Mix graphite powder (325 mesh, carbon content>99%) with SiO 2 Dry at 90°C for 6 hours, weigh 10g of graphite powder and 1kg of SiO 2Add it into a high-speed mixer and mix evenly, then put it into a solid-phase force chemical reactor, pass cooling circulating water at room temperature during the milling process, and control the temperature of the disc surface to 40°C, the pressure to 25KN, and the speed to 200 rpm. Circular grinding 50 times to obtain graphene and SiO 2 of composite materials. Graphene and SiO 2 The composite material is dispersed in hydrofluoric acid, and then the graphene is separated by centrifugation, and the centrifugation is repeated 3 times to completely remove the SiO 2 , and then the product obtained was treated with 1mol / L dilute sulfuric acid for 12 hours, and the precipitate obtained after centrifugation and washing for 30 minutes at a speed of 5000 rpm...

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Abstract

The invention belongs to the technical field of graphene preparation, and in particular relates to a preparation method of graphene material based on the principle of solid-phase mechanochemical reaction. The technical solution of the present invention is to use the three-dimensional strong shear structure of the solid-phase mechanochemical reactor to introduce grinding aids in the process of grinding graphite, and the three-dimensional shear force induced by the three-dimensional shear structure makes the grinding aids and graphite strongly The frictional interaction of graphite exfoliates to prepare single-layer or few-layer graphene. The method of the present invention is to dry the graphite and the grinding aid separately, add them to a mixer and mix them evenly, move them into a solid-phase mechanochemical reactor for grinding, remove the grinding aids and impurity ions, and dry at a temperature of 60-90°C to obtain A high-performance graphene material with less than 8 layers and few base defects. The new method for preparing the graphene material of the present invention has the characteristics of simplicity, high efficiency, cleanliness and low cost, and the prepared graphene material has few substrate defects, and the surface functionalization of the graphene can be realized in one step.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a graphene material based on a solid-phase mechanochemical reactor and a preparation method thereof. Background technique [0002] Graphene, as an emerging 2D carbon material, has become a research frontier in the fields of new energy materials, photocatalytic materials, and biological materials due to its unique chemical structure, large specific surface area, and excellent electrical, mechanical, and thermal properties. hotspot. Graphene has single-layer and few-layer. Single-layer graphene refers to a two-dimensional carbon material composed of a layer of carbon atoms closely packed periodically in a benzene ring structure (ie, hexagonal honeycomb structure). Few-layer graphene refers to the stacking of 3-10 layers of carbon atomic layers that are periodically densely packed in a benzene ring structure (ie, hexagonal honeycomb structure) in different ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/194
CPCC01P2002/72C01P2004/03C01P2004/04
Inventor 张楚虹白时兵刘超文豪谭讲
Owner SICHUAN UNIV
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