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Carbon nano-tube with fluorine-containing surface and preparation method thereof

A technology of carbon nanotubes and multi-walled carbon nanotubes, which is applied in the field of modified carbon nanotubes and its preparation, can solve the problems of poor thermal stability of surface functionalized groups, achieve reduced production costs, good heat resistance, suitable for The effect of mass production

Active Publication Date: 2012-10-17
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the related research on low-temperature fluorinated carbon nanotubes, the inventors found that when fluorinated at low temperature (room temperature - 100°C), the fluorination method introduces a relatively high fluorine content (7- 9%), but the fluorine content dropped to about 2% after treatment at 250-300°C for 40 minutes to 2 hours, indicating that the thermal stability of the surface functional groups is poor, which shows that the main formation is not thermally stable C-F bond, but a fluorination reaction with the existing oxygen-containing functional groups on the surface of carbon nanotubes. The reason is that at low temperature, the carbon of the carbon tube itself has obvious chemical inertness relative to the oxygen-containing functional groups on the surface. , not easy to react with fluorine gas

Method used

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  • Carbon nano-tube with fluorine-containing surface and preparation method thereof
  • Carbon nano-tube with fluorine-containing surface and preparation method thereof

Examples

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Effect test

Embodiment 1

[0026] After mixing the multi-walled carbon nanotube body and hydrochloric acid uniformly by ultrasonic, stir and reflux at the reflux temperature of 25°C for 15 hours, take out and wash with deionized water until neutral, and dry in vacuum; the multi-walled carbon nanotubes treated with acid and vacuum-dried The tube is placed in a closed vacuum reactor, then evacuated, and the air in the reactor is replaced with nitrogen for three times, then the vacuum reactor is filled with fluorine / nitrogen mixed gas, and the partial pressure of fluorine in the reactor is controlled to 10KPa , and the temperature was raised to 300° C., and the fluorination reaction was carried out for 0.5 hour. After the reactor was naturally cooled, the sample was taken out to obtain fluorinated carbon nanotubes. The XPS test shows that the fluorine content of the fluorinated carbon nanotubes is 4%. After the obtained fluorinated carbon nanotubes were treated under vacuum conditions at 350 °C for 1 hour,...

Embodiment 2

[0028]After mixing the multi-walled carbon nanotube body and nitric acid uniformly by ultrasonic, stir and reflux at the reflux temperature of 100°C for 48 hours, take out and wash with deionized water until neutral, and dry in vacuum; the multi-walled carbon nanotubes treated with acid and vacuum-dried The tube is placed in a closed vacuum reactor, then vacuumed, and the air in the reactor is replaced with nitrogen three times, then the vacuum reactor is filled with fluorine / nitrogen mixed gas, and the partial pressure of fluorine in the reactor is controlled to 30KPa , and the temperature was raised to 250° C., and the fluorination reaction was carried out for 1 hour. After the reactor was naturally cooled, the sample was taken out to obtain fluorinated carbon nanotubes. The XPS test shows that the fluorine content of the fluorinated carbon nanotubes is 8%. After the obtained fluorinated carbon nanotubes were treated under vacuum conditions at 350 °C for 1 hour, the fluorine...

Embodiment 3

[0030] After mixing the double-walled carbon nanotube body and sulfuric acid uniformly by ultrasonic, stir and reflux at the reflux temperature of 30°C for 30 hours, take out and wash with deionized water until neutral, and dry in vacuum; the double-walled carbon nanotubes treated with acid and vacuum-dried The tube is placed in a closed vacuum reactor, then evacuated, and the air in the reactor is replaced with nitrogen for three times, and then the vacuum reactor is filled with a fluorine / nitrogen / argon mixture to control the distribution of fluorine in the reactor. The pressure is 50KPa, and the temperature is raised to 200°C, and the fluorination reaction is carried out for 2 hours. After the reactor is naturally cooled, the sample is taken out to obtain fluorinated carbon nanotubes. The XPS test shows that the fluorine content of the fluorinated carbon nanotubes is 7.45%. After the obtained fluorinated carbon nanotubes were treated under vacuum at 350°C for 1 hour, the fl...

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Abstract

The invention discloses a carbon nano-tube with a fluorine-containing surface, wherein the surface of the carbon nano-tube is of a carbon-fluorine covalent bond structure, the content of fluorine in the surface is 4-14%, and the decrease rate of the content of the fluorine is smaller than 5% after a produced fluorocarbon nano-tube is treated for 1 hour under a vacuum condition at 350 DEG C. The preparation method of the carbon nano-tube comprises the following steps of: firstly treating the carbon nano-tube by utilizing strong acid, secondly placing the carbon nano-tube in a vacuum reactor, charging fluorine / inert gas mixture with fluorine partial pressure of 10-100KPa in nitrogen atmosphere under room temperature to react for 0.5-4 hours at 150-300 DEG C, and cooling down to be the room temperature to obtain the carbon nano-tube. The fluorocarbon nano-tube prepared by the preparation method disclosed by the invention has the advantages of high fluorine content, low reaction temperature, high safety, energy conservation, and simple process, a fluorine-containing group of the surface of the treated prepared fluorocarbon nano-tube has good heat resistance and lower cost, and the fluorocarbon nano-tube is suitable for large-batch production and has stronger application prospect.

Description

technical field [0001] The invention belongs to the technical field of modified carbon nanotubes and preparation thereof, and in particular relates to a surface fluorine-containing carbon nanotube and a preparation method thereof. Background technique [0002] Carbon nanotubes have potential application value in many aspects because of their outstanding physical and mechanical properties, peculiar electrical properties, good chemical stability and thermal stability, especially in the field of polymer nanocomposites. However, due to the "inertness" of the surface of carbon nanotubes and the strong van der Waals force, they are very easy to agglomerate, which makes it difficult for carbon nanotubes to disperse uniformly in common organic solvents and resin matrices, which limits their application in polymer nanocomposites. field research and applications. Therefore, surface treatment of carbon nanotubes is particularly important in order to obtain polymer nanocomposites with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C01B31/02B82Y30/00C01B32/10C01B32/174
Inventor 刘向阳王旭陈一高杰
Owner SICHUAN UNIV
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