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Preparation method of graphite fluoride

A technology of fluorinated graphite and graphite, which is applied in the direction of fluorinated carbon, can solve the problems of high synthesis temperature of fluorinated graphite, low safety in the production process, cumbersome process, etc., to reduce the synthesis temperature, increase the yield, and accelerate the reaction rate Effect

Active Publication Date: 2018-06-22
HUBEI ZHUOXI FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to overcome the above-mentioned technical deficiencies, propose a preparation method of fluorinated graphite, and solve the technical problems of high synthesis temperature, low yield, low safety of production process and cumbersome process in the process of preparing fluorinated graphite in the prior art

Method used

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preparation example Construction

[0012] The present embodiment provides a kind of preparation method of graphite fluoride, specifically comprises the following steps:

[0013] (1) Prepare materials according to the following mass ratio: Weigh graphite and citrate respectively according to the mass ratio of graphite and citrate as 1:0.05~0.1, crush the graphite into graphite powder with uniform particle size, and stir with citrate Mix evenly; then weigh 0.1-0.3% metal fluoride by graphite weight, add graphite and citrate mixture, stir and mix evenly. Citrate is sodium citrate and / or potassium citrate. Adding these two substances to the reaction system can not only reduce the heat required for the reaction, but also be soluble in water, which is more convenient for the subsequent purification of graphite fluoride; the metal fluoride is fluorine At least one of sodium fluoride, potassium fluoride and silver fluoride, these substances have more obvious inhibitory effect on side reactions and more convenient subse...

Embodiment 1

[0019] This embodiment provides a kind of preparation method of fluorinated graphite, and its raw material is: graphite 1kg, sodium citrate 50g, sodium fluoride 2g; Its preparation method specifically comprises the following steps:

[0020] (1) prepare materials according to the following quality: graphite 1kg, sodium citrate 50g and sodium fluoride 2g, graphite is pulverized into graphite powder with uniform particle size, and stirs and mixes with sodium citrate and sodium fluoride;

[0021] (2) After the reaction kettle is passivated, add the mixture of graphite, sodium citrate and sodium fluoride in the step (1) to the reaction kettle, and feed the fluorine gas fraction into the reaction kettle to be 70% The fluorine-nitrogen mixed gas is used for the fluorination reaction at a temperature of 200°C and a pressure of 0.01 MPa. After 4 hours of reaction, the reaction is stopped, and the mixture in the reactor is cooled to room temperature to obtain fluorinated graphite.

[00...

Embodiment 2

[0025] This embodiment provides a kind of preparation method of fluorinated graphite, and its raw material is: graphite 10kg, potassium citrate 800g, sodium fluoride 5g, potassium fluoride 5g; Its preparation method specifically comprises the following steps:

[0026] (1) Prepare materials according to the following quality: graphite 10kg, potassium citrate 800g, sodium fluoride 5g, potassium fluoride 5g, graphite is pulverized into graphite powder with uniform particle size, and mixed with potassium citrate, sodium fluoride and potassium fluoride Stir to mix well;

[0027] (2) After passivating the reactor, add the mixture of graphite, potassium citrate, sodium fluoride and potassium fluoride in step (1) to the reactor, and feed fluorine gas into the reactor The fluorine-nitrogen mixed gas with a concentration of 65% is fluorinated at a temperature of 250°C and a pressure of 1 MPa. After 3 hours of reaction, the reaction is stopped, and the mixture in the reactor is cooled to...

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PUM

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Abstract

The invention discloses a preparation method of graphite fluoride. The preparation method comprises the following steps: uniformly mixing graphite, citrate and metal fluoride, introducing mixed gas containing fluorine gas into a mixture and performing fluoridation reaction at a temperature of 150-250 DEG C, wherein the mass ratio of the graphite to the citrate is 1:(0.05-0.1). The citrate and thefluorine gas in the preparation method disclosed by the invention can generate the fluoridation reaction to release a lot of heat, so that the heat required for the reaction is reduced, and the fluoridation reaction can occur at a lower temperature; by adding the metal fluoride as a catalyst, not only can the reaction rate be increased, but also the reaction selectivity can be improved, and the occurrence probability of side reaction can be reduced; and the reaction temperature is 150-250 DEG C, so that not only can the sufficient reaction between the fluorine gas and the graphite be ensured,but also the yield of the graphite fluoride can be improved. The preparation method disclosed by the invention is low in synthetic temperature, high in yield, simple in process and high in safety.

Description

technical field [0001] The invention relates to the technical field of preparation of new materials, in particular to a preparation method of graphite fluoride. Background technique [0002] Graphite fluoride, the molecular formula is CF X , X is an indefinite value, and its range is between 0 and 1.25. Graphite fluoride is a new material with unique properties. Its structure is similar to graphene, and it exhibits excellent insulator or semiconductor properties. Its band gap can also be controlled by controlling the size of graphite fluoride sheets. At the same time, similar to two-dimensional isotactic polytetrafluoroethylene, graphite fluoride is modified by introducing fluorine to make its surface have extremely low surface energy, so it can easily achieve super-oleophobic and super-hydrophobic amphiphobic properties. It has broad application prospects in the fields of surface treatment and lubrication. [0003] At present, the synthesis methods of graphite fluoride a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/10
CPCC01P2006/80
Inventor 谢学归张雨寒谢子卓于铉谢洁珊
Owner HUBEI ZHUOXI FLUOROCHEM