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Fluorinated graphite and preparation method thereof

A technology of fluorinated graphene and graphene, applied in the direction of single-layer graphene, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as low fluorine content

Active Publication Date: 2016-08-24
湖北高地石墨烯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fluorinated graphene prepared by the prior art has a low fluorine content

Method used

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  • Fluorinated graphite and preparation method thereof

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[0025] The invention discloses a preparation method of fluorinated graphene, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The method and application of the present invention have been described through preferred embodiments, and the relevant personnel can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention to realize and Apply the technology of the present invention.

[0026] The embodiment of the present invention provides a kind of preparation method of fluorinated graphene, comprising:

[0027] S1), under the protection of an inert gas, fluorination reacti...

Embodiment 1

[0064] Weigh 1 g of graphene powder obtained by oxidation-reduction method and put it into a reactor. After replacing the reactor with nitrogen atmosphere, raise the temperature to 150°C, start to feed the fluorine-nitrogen mixed gas with the volume ratio of fluorine to the mixed gas at a volume ratio of 1:100, control the system pressure at 0.1Mpa, and control the gas flow rate at 0.1L / min, after 2 hours of fluorination, stop feeding fluorine-nitrogen mixed gas, change to nitrogen gas, and keep warm for 1 hour to complete the preliminary fluorination reaction, and obtain the crude product of preliminary fluorinated graphene fluoride powder. Next, the system is maintained at a temperature of 150°C, and the sulfur tetrafluoride gas diluted and protected by nitrogen is introduced. The volume ratio of sulfur tetrafluoride gas to the mixed gas is 20:100, and the system pressure is controlled at 0.1Mpa. Stop after 2 hours Sulfur tetrafluoride gas was introduced, replaced by nitrog...

Embodiment 2

[0066] Weigh 1 g of graphene powder obtained by oxidation-reduction method and put it into a reactor. After replacing the reactor with nitrogen atmosphere, raise the temperature to 550°C, start to feed the fluorine-nitrogen mixed gas whose volume ratio of fluorine to the mixed gas is 30:100, control the system pressure at 0.2Mpa, and control the gas flow rate at 20L / min After 20 hours of fluorination, stop feeding fluorine-nitrogen mixed gas, change to nitrogen gas, and keep warm for 1 hour to complete the preliminary fluorination reaction, and obtain the crude product of preliminary fluorinated graphene fluoride powder. Next, the temperature of the system was lowered to 400°C, and the phosphorus trifluoride gas diluted and protected by nitrogen gas was introduced. The volume ratio of phosphorus trifluoride gas to the mixed gas was 80:100, and the system pressure was controlled at 0.2Mpa. Stop after 10 hours Phosphorus trifluoride gas was introduced, replaced by nitrogen gas, ...

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Abstract

The invention relates to the technical field of new materials, in particular to a preparation method of fluorinated graphite. The preparation method of the fluorinated graphite includes the following steps that S1, graphene and a first fluorinating agent perform fluorinating reaction under inert gas protection to obtain a fluorinated graphite coarse product, wherein the reaction temperature is 150-550 DEG C, the reaction time is 2-20 hours, the graphene is graphene powder or a graphene film, and the first fluorinating agent contains fluorine gas; S2, the fluorinated graphite coarse product and a second fluorinating agent perform fluorinating reaction under inert gas protection to obtain fluorinated graphite, wherein the reaction temperature is 150-400 DEG C, the reaction time is 2-10 hours, and the second fluorinating agent is gas-phase fluoride. By the adoption of the method, the fluorinated graphite with high fluoride content can be prepared, the fluorine content is close to the theoretical level, and the defect density is low.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a fluorinated graphene, and also to a preparation method of the fluorinated graphene. Background technique [0002] Fluorinated graphene is a new material with unique properties. Its structure is similar to graphene, and it exhibits excellent insulator or semiconductor properties. It can also control its band gap by controlling the size of fluorinated graphene sheets. . At the same time, similar to two-dimensional isotactic polytetrafluoroethylene, fluorinated graphene is modified by introducing fluorine to make its surface have extremely low surface energy, so it is very easy to achieve super-oleophobic and super-hydrophobic amphiphobic properties. , has broad application prospects in the fields of surface treatment and lubrication. [0003] The ideal fluorinated graphene should have a fluorine content close to 61% or even higher, and there should be no other heteroatoms...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00
CPCC01P2004/03C01B32/194C01B2204/02C01P2002/50
Inventor 严瑾
Owner 湖北高地石墨烯科技有限公司
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