Method for preparing carbon nanometer tube in large-scale

A technology for large-scale preparation of carbon nanotubes, applied in the field of large-scale preparation of soluble carbon nanotubes, can solve problems such as being unsuitable for large-scale preparation of soluble carbon nanotubes, and achieve simple and effective preparation, solvent saving, convenient and effective recovery Effect

Inactive Publication Date: 2004-12-08
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above-mentioned preparation method of soluble carbon nanotubes has certain limitations in the purification of soluble carbon nanotubes and the recovery and reuse of unreacted carbon nanotubes, and is not suitable for large-scale preparation of soluble carbon nanotubes.

Method used

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  • Method for preparing carbon nanometer tube in large-scale
  • Method for preparing carbon nanometer tube in large-scale
  • Method for preparing carbon nanometer tube in large-scale

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Embodiment 1

[0026] 50 g of raw multi-walled carbon nanotubes were heated to reflux in 500 ml of 65% concentrated nitric acid for 24 hours, and after centrifugation, the precipitate was washed with deionized water until it was nearly neutral. The obtained purified multi-walled carbon nanotubes were dried in a vacuum oven at 50° C., and then heated to reflux in 500 ml of freshly steamed thionyl chloride for 24 hours. After the product was centrifuged, the solid was washed several times with anhydrous tetrahydrofuran, dried in a vacuum oven, mixed with 30 g of octadecylamine, heated to 80° C. and stirred for 96 hours under nitrogen protection. After the product is cooled, wrap it with filter paper and place it in a Soxhlet extractor to extract unreacted octadecylamine with 300ml ethanol, and then use 300ml chloroform to extract soluble carbon nanotubes after 24 hours. After 24 hours, the chloroform solution was evaporated to dryness with a rotary evaporator to obtain about 20 g of soluble ca...

Embodiment 2

[0029] 50 g of raw multi-walled carbon nanotubes were heated to reflux in 500 ml of 65% concentrated nitric acid for 24 hours, and after centrifugation, the precipitate was washed with deionized water until it was nearly neutral. The obtained purified multi-walled carbon nanotubes were dried in a vacuum oven at 50° C., and then heated to reflux in 500 ml of freshly steamed thionyl chloride for 24 hours. After the product was centrifuged, the solid was washed several times with anhydrous tetrahydrofuran, dried in a vacuum oven, mixed with 30 g of didecylamine, heated to 80° C. and stirred for 96 hours under nitrogen protection. After the product is cooled, wrap it with filter paper and place it in a Soxhlet extractor to extract unreacted didecylamine with 300ml ethanol, and then use 300ml chloroform to extract soluble carbon nanotubes after 24 hours. After 24 hours, the chloroform solution was evaporated to dryness with a rotary evaporator to obtain about 20 g of soluble carbon...

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Abstract

A process for preparing soluble carbon nanotubes in large scale includes such steps as using concentrated nitric acid to purify and cut the multi-wall carbon nanotubes (MWNTs) prepared by CVD to obtain carboxyl contained carbon nanotubes, reacting on sulfoxide chloride to obtain acyl chloride, and reacting on lipoamine.

Description

technical field [0001] The invention relates to a method for large-scale preparation of soluble carbon nanotubes. Background technique [0002] Carbon nanotubes are a new type of nanomaterials discovered by Japanese scientist Professor Iijima in 1991. They have good performance in many fields such as hydrogen storage materials, field emission materials, battery materials, stealth materials, artificial muscle materials, sensor materials, and catalyst materials. application prospects. However, carbon nanotubes are insoluble and infusible. For a long time, the research on carbon nanotubes has been carried out in the solid state, which has greatly affected the application research of carbon nanotubes. For example, when preparing carbon nanotube-polymer composites, due to the insolubility of carbon nanotubes, the compatibility of carbon nanotubes and polymers has not been well resolved, which greatly affects the application of carbon nanotubes. develop. Therefore, there is an ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 秦玉军郭志新刘璐琪武伟潘华龙李祥龙石家华朱道本
Owner INST OF CHEM CHINESE ACAD OF SCI
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