Method for preparing carbon nanofibers

A technology of carbon nanofibers and nanofibers, applied in the direction of carbon fibers, fiber treatment, fiber chemical characteristics, etc., can solve the problems of complex catalysts and equipment, high cost, low production efficiency, etc., achieve high interlayer shear strength and maintain stability The effect of stability and good stability

Inactive Publication Date: 2010-06-02
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method prepares hollow carbon nanofibers, which involves complex cataly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Acrylonitrile and methylene succinic acid are used as monomers, azobisisobutyronitrile with 1% of monomer mass is used as initiator, mercaptan with 0.5% of monomer mass is used as chain transfer agent, and dimethyl sulfoxide is used as solvent. Solution polymerization at 65°C for 5 hours to obtain an acrylonitrile-methylene succinic acid copolymer solution with a mass percent content of copolymer of 10% and a molar content of methylene succinic acid of 5%, after measuring the intrinsic viscosity with an Ubbelohde viscometer The calculated weight-average molecular weight of the copolymer is 82000g / mol. The copolymer solution is passed through a 24-hole strip spinneret with an aperture of 0.1mm on an electrospinning machine, at 25°C and 15kV, and the receiving distance is 25cm. The stainless steel mesh conveyor belt rotating at m / min collects the generated nanofibers. The average diameter of the fibers observed by the scanning electron microscope is 400nm. The nanofibers a...

Embodiment 2

[0042] Adopting the same process and technical parameters as in Example 1 to prepare carbon nanofibers; then adopting 5% ammonium bicarbonate solution by mass percentage as electrolyte, carbon nanofibers as anodes, and carbon electrodes immersed in electrolytes as cathodes, With a voltage of 1.2V, a temperature of 30°C, and a current density of 20A / m 2 After treating the carbon nanofibers for 4 minutes, the carbon nanofibers containing carboxyl and amino functional groups are obtained. The carbon nanofiber is measured by XPS photoelectron spectroscopy, and the surface carbon element content is 80.1%, the oxygen element content is 17.2%, and the nitrogen element content is 2.6%. It shows that the content of carboxyl group, hydroxyl group and amino group or amide group on the surface of carbon nanofibers increases significantly after electrochemical treatment.

[0043] The carbon nanofiber and phenolic resin are made into a composite material, and the interlaminar shear strengt...

Embodiment 3

[0045] Place 1 kg of carboxylated carbon nanofibers prepared in Example 1 in an enamel reaction kettle, add 20 L of thionyl chloride, stir and reflux in a water bath at 70 ° C for 24 h, filter the mixed solution obtained after the reaction, and wash with 10 L of tetrahydrofuran (THF) Repeated cleaning, drying the filtered material at 50°C for 5 hours in vacuum to obtain acyl chloride carbon nanofibers, put the fibers in a reaction kettle, add 5kg of ammonium carbonate to it, add dropwise 50L of concentrated ammonia water, and stir the reaction at room temperature 6 hours, after the completion of the reaction, remove residual ammonium carbonate and ammonia water, repeatedly wash and filter the resulting substance with distilled water, then dry at 50°C for 5 hours in a vacuum drying oven to obtain amidated carbon nanofibers, and the prepared amidated carbon Put the nanofibers into the reaction kettle, slowly add 30L of sodium hypochlorite solution with a concentration of 20% by m...

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Abstract

The invention relates to a method for preparing carbon nanofibers. The method comprises the following steps: taking a polyacrylonitrile solution or an acrylonitrile copolymer solution or melt as materials, preparing nanofibers by the electrostatic spinning or the airflow spray method, and then preparing the nanofibers into carbon nanofibers. The method is characterized in that the carbon nanofibers are acidified or electrochemically treated into carbon nanofibers containing oxygen or nitrogen functional groups. The acidifying process comprises the following steps of: placing the carbon nanofibers in a nitric acid solution with the mass concentration of 30-68% and treating for 1-10 hours at 10-50 DEG C; rinsing with deionized water and drying; thus, obtaining the carbon nanofibers containing carboxyl functional groups. The electrochemical treating process comprises the steps of: placing the carbon nanofibers in a nitric acid or phosphoric acid solution with the mass percentage concentration of 1-20% at 10-50 DEG C, or in ammonium carbonate or ammonium hydrogen carbonate, and treating with the apparent current density of 10-100A/m2 for 1-120 minutes to obtain the carbon nanofibers containing carboxyl or amino functional groups.

Description

technical field [0001] The invention relates to fiber preparation and application technology, in particular to a preparation method of carbon nanofibers containing functional groups. Background technique [0002] Carbon fiber is a fibrous carbon material formed by heating organic fiber or low-molecular hydrocarbon gas raw materials to 1500°C, with a carbon content of more than 90%, and has low density, high strength, high modulus, high temperature resistance, chemical corrosion resistance, low resistance, It has excellent properties such as high thermal conductivity, low thermal expansion, and radiation resistance. It also has the flexibility of fibers, and its specific strength and specific modulus are superior to other fibers. It has a wide range of applications in the fields of aerospace industry, aviation industry, transportation, and sports equipment. application. [0003] The diameter of conventional carbon fiber is generally 3-10 μm, and the specific surface area is ...

Claims

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Application Information

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IPC IPC(8): D01F9/21D01F9/22D06M11/64D06M11/70D06M11/76D06M101/40
Inventor 张兴祥王宁靳艳梅乔志军刘海辉
Owner TIANJIN POLYTECHNIC UNIV
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