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Method for preparing nano graphite fluoride at low temperature

A technology of fluorinated graphite and nano-graphite, applied in the field of non-metallic materials, can solve the problems of high gas-solid fluorination reaction temperature, difficult control of the reaction process, local temperature overheating, etc. The effect of a large contact area

Active Publication Date: 2018-08-24
HUBEI ZHUOXI FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is currently the most mature technology, with high reaction efficiency and simple synthesis process; however, the gas-solid fluorination reaction temperature is high and the reaction is relatively violent, the reaction process is not easy to control, and the heat generated by fluorination will lead to local overheating, making fluorinated graphite Decomposes rapidly, even explodes, leading to a higher risk of reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Dry 100g of nano-graphite, 2g of silver fluoride and 50g of citric acid at 90°C for 3h, add nano-graphite and citric acid into the dry reactor, then add 500ml of absolute ethanol to the reactor, and dehydrate the reactor Stir and mix the materials in the reactor evenly, then pass nitrogen gas to exhaust the air in the reactor, then raise the temperature of the mixed solution in the reactor to 130°C, keep the temperature for 3.5 hours, then lower the temperature of the mixed solution in the reactor to normal temperature, Add silver fluoride and 150g iodine pentafluoride into the reactor, and stir and react at 40°C for 1.5h;

[0018] (2) After the reaction product in the step (1) is vacuum-filtered, a solid substance is obtained, and the solid substance is added in 100ml potassium iodide solution earlier, filtered after stirring, and the filter residue is repeatedly washed with pure water until the pH value of the washing liquid to 7, then suction filter and vacuum dr...

Embodiment 2

[0021] (1) Dry 100g of nano-graphite, 2.5g of silver fluoride and 30g of citric acid at 100°C for 2.5h, add nano-graphite and citric acid into the dry reactor, then add 500ml of absolute ethanol to the reactor, and The materials in the reactor were stirred and mixed evenly, and then argon gas was introduced to exhaust the air in the reactor, and then the temperature of the mixed liquid in the reactor was raised to 120°C, and after holding for 3 hours, the temperature of the mixed liquid in the reactor was lowered to At room temperature, add silver fluoride and 180g iodine pentafluoride to the reactor, and stir at 37°C for 2 hours;

[0022] (2) After the reaction product in the step (1) is vacuum-filtered, a solid substance is obtained, and the solid substance is added in 100ml potassium iodide solution earlier, filtered after stirring, and the filter residue is repeatedly washed with pure water until the pH value of the washing liquid to 7, then suction filter and vacuum dry t...

Embodiment 3

[0025] (1) Dry 100g of nano-graphite, 3g of silver fluoride and 45g of citric acid at 100°C for 2.5h, add nano-graphite and citric acid into the dry reactor, then add 500ml of absolute ethanol to the reactor, and the reaction Stir and mix the materials in the reactor evenly, then pass in argon gas to exhaust the air in the reactor, then raise the temperature of the mixed liquid in the reactor to 125°C, keep the temperature for 4 hours, then lower the temperature of the mixed liquid in the reactor to normal temperature , add silver fluoride and 200g iodine pentafluoride into the reactor, stir and react at 45°C for 2h;

[0026] (2) After the reaction product in the step (1) is vacuum-filtered, a solid substance is obtained, and the solid substance is added in 100ml potassium iodide solution earlier, filtered after stirring, and the filter residue is repeatedly washed with pure water until the pH value of the washing liquid to 7, then suction filtration and vacuum drying of the f...

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Abstract

The invention discloses a method for preparing nano graphite fluoride at a low temperature. The method comprises the following steps that (1) nano graphite, citric acid and absolute ethyl alcohol aremixed to be uniform and activated for 3-5 hours at the temperature of 120-130 DEG C, after the temperature of the mixed liquid is decreased to be room temperature, silver fluoride and iodine pentafluoride are added in the mixed liquid, the mixed liquid is reacted for 1.5 to 2 hours at the temperature of 37-52 DEG C, and a reaction product is obtained; (2) the reaction product is subjected to vacuum filtration to obtain a solid product, the solid product is added into a potassium iodide solution to be stirred and then filtered, after the obtained filter residue is treated, nano graphite subjected to pretreatment is obtained; and (3) mixed gas of fluorine and nitrogen is injected into the nano graphite subjected to pretreatment to react for 1.5-2.5 hours at the temperature of 200-240 DEG C,and a finished product is obtained. Compared with a high temperature gas phase synthesis method, the graphite intercalation compound has higher activity than graphite, is more liable to react with fluorine, the content of fluorine is higher, the reaction temperature is lower, and the safety is higher.

Description

technical field [0001] The invention relates to the technical field of non-metallic materials, in particular to a method for preparing nanometer fluorinated graphite at low temperature. Background technique [0002] 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, fluorinated graphite is modified by introducing fluorine, so that it has low surface energy and interlayer energy, high electrical polarity, good lubricity, and small thermal neutron absorption cross section. The unique physical and chemical properties of the series have been widely used in batteries, nuclear reactors, lubrication, degreasing, antifouling, waterproofing, etc. [0003] The synthesis methods of fluorinated graphite includ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/10B82Y30/00
CPCB82Y30/00C01B32/10
Inventor 谢学归谢子卓张雨寒于铉谢洁珊
Owner HUBEI ZHUOXI FLUOROCHEM
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