Method for preparing graphite fluoride

A technology of fluorinated graphite and graphite, applied in the field of preparation of fluorinated graphite, can solve the problems of not disclosing key synthesis technologies, multiple side reactions and side reaction products, affecting the quality of fluorinated graphite, etc., and achieves stable properties and high utilization value. , the effect of promoting development

Inactive Publication Date: 2010-12-29
BEIJING GENERAL RES INST OF MINING & METALLURGY
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Problems solved by technology

[0010] In the preparation method involving fluorine gas, there are great risks in the production, transportation and use of fluorine gas, and there are many side reactions and side reaction products, which greatly affect the quality of fluorinated graphite
The "solid phase method" preparation technology is a safe and efficient new technology for the preparation of fluorinated graphite, which shows a very high research prospect, but the relevant research did not disclose the key synthesis technology

Method used

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  • Method for preparing graphite fluoride
  • Method for preparing graphite fluoride
  • Method for preparing graphite fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Molby K 2 MnF 6 :SbF 5 =1:2 Configure inorganic fluoride mixture, add pretreated flake graphite, the mass ratio of inorganic composite fluoride to graphite is 43:1. The mixed material was moved into the reactor, and the reactor was sealed, and finally filled with nitrogen at a pressure of 0.5Mpa. Set the heating rate of the reactor to 15°C / min, the reaction temperature to 500°C, and the time for 3 hours, heat the reactor, close the reactor after the reaction, cool to room temperature, take out the reaction product, purify and dry to obtain the product, the fluorine content of the product is 35.5 %. figure 2 with image 3 Respectively, the XRD analysis spectrum and the EDS analysis spectrum of the product obtained.

Embodiment 2

[0070] Molby K 2 MnF 6 :SbF 5 =1:2 Configure inorganic fluoride mixture, add pretreated flake graphite, the mass ratio of inorganic composite fluoride to graphite is 43:1. Move the mixed material into the reactor, seal the reactor, and finally fill the reactor with nitrogen pressure of 2.5Mpa, set the reactor heating rate to 15°C / min, and the reaction temperature to 500°C for 3 hours, heat the reactor, close the reactor after the reaction is completed, and cool to At room temperature, the reaction product was taken out, purified and dried to obtain a product with a fluorine content of 45.1%. Figure 4 with Figure 5 Respectively, the XRD analysis spectrum and the EDS analysis spectrum of the product obtained.

Embodiment 3

[0072] Molby K 2 MnF 6 :SbF 5 =1:2 Configure inorganic fluoride mixture, add pretreated flake graphite, the mass ratio of inorganic composite fluoride to graphite is 97:1. The mixed material was moved into the reactor, and the reactor was sealed, and finally filled with nitrogen at a pressure of 5Mpa. Set the heating rate of the reactor to 20°C / min, the reaction temperature to 500°C, and the reaction time to 3 hours, heat the reactor, close the reactor after the reaction, cool to room temperature, take out the reaction product, purify and dry to obtain the product, the fluorine content of the product is 59.3%. Image 6 with Figure 7 Respectively, the XRD analysis spectrum and the EDS analysis spectrum of the product obtained.

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Abstract

The invention discloses a method for preparing graphite fluoride. The graphite fluoride is prepared from inorganic composite fluridizer and graphite as raw materials by heating and reaction in the presence of high-purity nitrogen, wherein the inorganic composite fluridizer is the mixture of potassium hexafluoromanganate and antimony pentafluoride. Due to the adoption of the method, the fluorine content of the finally obtained graphite fluoride can reach 59%, and the graphite fluoride can be used as the anode material and the solid lubricating material of lithium ion batteries; the purity of the graphite fluoride product prepared by a solid phase method is greater than 99%, and the use value is high; moreover, the invention is simple in operation and has high safety without needing external fluorine; and the properties of hexafluoromanganate and antimony pentafluoride are stable at normal temperature and therefore the safety is high.

Description

technical field [0001] The invention relates to the technical field of graphite new materials, in particular to a preparation method of fluorinated graphite. Background technique [0002] Graphite fluoride is one of the research hotspots of high-tech and high-performance graphite materials, and its chemical formula is CF x (0.5≤x≤1.3), graphite fluoride is mainly used as a positive electrode material for solid lubricants and high energy density batteries, and its physical and chemical properties are superior. The synthesis methods of graphite fluoride can be divided into the following three types: [0003] (1) "Gas phase method" high temperature synthesis technology [0004] "Gas-phase method" high-temperature synthesis technology is the most mature and traditional preparation method. In the temperature range of 350°C to 610°C, the graphite raw material is directly contacted with elemental fluorine gas, and it is prepared by heat preservation for a certain period of time (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B9/08
Inventor 刘建远申士富刘海营
Owner BEIJING GENERAL RES INST OF MINING & METALLURGY
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