Method for preparing carbon monofluoride or fluorocarbon through inner circulation of fluorine

A technology of fluorinated graphite or carbon fluoride, which is applied in the direction of fluorinated carbon, can solve the problems of low fluorocarbon ratio, poor safety, and poor quality, and achieve the effects of lower temperature, higher safety, and lower pressure

Inactive Publication Date: 2013-10-02
HUBEI ZHUOXI FLUOROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a method for preparing fluorinated graphite or carbon fluoride...

Method used

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  • Method for preparing carbon monofluoride or fluorocarbon through inner circulation of fluorine

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Effect test

Embodiment 1

[0036] Dry the graphite powder at 110°C for 24 hours and put it into the reaction kettle, feed high-purity nitrogen and high-purity fluorine gas to make the concentration of fluorine gas 50%, keep the reaction temperature at 400°C, and the reaction pressure at 0.05MPa. Lasts 30 hours. The fluorocarbon ratio of the product is 0.61, and the yield is 94%.

Embodiment 2

[0038] Dry 5 kg of graphene at 110°C for 36 hours and put it into the reactor, feed high-purity nitrogen and high-purity fluorine gas to make the concentration of fluorine gas 60%, keep the reaction temperature at 450°C, and the reaction pressure at 0.05MPa , the reaction lasted for 40 hours. The fluorocarbon ratio of the product was 0.72, and 5.1 kg of fluorinated graphite was obtained.

Embodiment 3

[0040] Dry the graphite powder at 110°C for 40 hours and put it into the reaction kettle, feed high-purity nitrogen and high-purity fluorine gas to make the concentration of fluorine gas 80%, keep the reaction temperature at 450°C, and the reaction pressure at 0.05MPa. Lasts 40 hours. The fluorocarbon ratio of the product is 0.8, and the yield is 97%.

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Abstract

The invention provides a method for preparing carbon monofluoride or fluorocarbon through inner circulation of fluorine. The method comprises the following steps of: (1) firstly passivating a reaction system, and then loading the pretreated graphite or carbon material into a reaction kettle with a cycling passage; (2) adding argon or nitrogen into the reaction kettle, adding fluorine to obtain the fluorine nitrogen or fluorine argon mixed gas; (3) heating the reaction kettle, setting and maintaining a reaction temperature and reaction pressure, and stopping the heating after the reaction is carried out for 1 to 70h under the inner circulation working condition; and (4) taking out the carbon monofluoride or fluorocarbon when the reaction kettle is cooled to the room temperature. The invention also provides a synthesizing device for preparing the carbon monofluoride or fluorocarbon through the inner circulation of the fluorine. The carbon monofluoride or fluorocarbon is synthesized by adopting the fluorine nitrogen mixed gas with high concentration of fluorine, the passivated reaction system, automatic control of a remote computer and a novel fluorine inner circulation process. The cost is low, the safety is high, the yield is high, and the fluorine-carbon ratio of a product is precisely controlled.

Description

technical field [0001] The invention relates to a preparation method of fluorinated graphite or fluorinated carbon, in particular to a method for preparing fluorinated graphite or fluorinated carbon by internal circulation of fluorine gas. Background technique [0002] Graphite fluoride is a graphite interlayer compound synthesized by the direct reaction of carbon and fluorine (or hydrogen fluoride). The interlayer substance is fluorine atoms, which is a covalent interlayer compound. The molecular formula is represented by CFx, where x is an indeterminate value, and its range is between 0 and 1.25. The synthesis methods of graphite fluoride can be roughly divided into high temperature synthesis method (dry method) and low temperature synthesis method (wet method). [0003] (1) High temperature synthesis method [0004] When the reaction temperature is between 375°C and 640°C, fluorine gas can react with graphite to synthesize graphite fluoride, and within this temperature ...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B32/10
Inventor 谢子卓谢学归
Owner HUBEI ZHUOXI FLUOROCHEM
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