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Preparation method of carbon nanometer tube/ polyimide composite fiber

A technology of carbon nanotubes and composite fibers, which is applied in the field of preparation of composite fibers, and can solve problems such as the mechanical properties of fibers that are difficult to spin and form, and the interfacial adhesion of uneven dispersion

Inactive Publication Date: 2008-05-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the difficulty of spinning polyamic acid fibers and the mechanical properties of fibers, and at the same time solves the problems of uneven dispersion of carbon nanotubes in the matrix polymer and interfacial adhesion

Method used

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  • Preparation method of carbon nanometer tube/ polyimide composite fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 6g of multi-walled carbon nanotubes into 120ml of mixed acid of 70% concentrated nitric acid and 98% concentrated sulfuric acid (volume ratio is 1:3), ultrasonicate at 60°C for 2h, then reflux in a water bath at 60°C for 5h, After cooling to room temperature, slowly add deionized water to soak for about 10 hours, pour off the supernatant, add deionized water, use a high-speed centrifuge to wash and separate, and wash with water for several times until the pH value of the product is greater than 6; finally wash it clean The carbon nanotubes were dried in an oven for 48 hours to obtain acidified multi-walled carbon nanotubes MWNTs-COOH. Take by weighing 4g of MWNTs-COOH in a 500ml volumetric flask, add 80ml of N, N-dimethylacetamide (DMAc), ultrasonic 30min; weigh 12g of octadecyl isocyanate (C 18 h 37 NCO) in a 400ml beaker, add 200ml of DMAc solvent, stir until completely dissolved; 200ml of C 18 h 37 Add the DMAc solution of NCO into the DMAc suspension of M...

Embodiment 2

[0031] (1) The multi-walled carbon nanotubes used in step (1) in Example 1 are replaced by single-walled carbon nanotubes, octadecyl isocyanate is replaced by p-chlorophenyl isocyanate, N, N'-dimethylacetamide Change to N, N'-dimethylformamide, and other steps are the same as in Example 1.

[0032](2) Add 250ml of N,N'-dimethylformamide solvent in the flask, pass nitrogen gas for deoxygenation protection, add 24.0288g of diaminodiphenylmethane, mechanically stir until completely dissolved, and add 26.1744 g of pyrobenzene in batches sulfuric anhydride, and stirred for 4 h under an ice bath to obtain a pale yellow polyamic acid (PAA) solution with a solid content of 17%.

[0033] (3) Weigh 1.5 g of alkylated carbon nanotubes, put them into a sample bottle, add 18 ml of N, N'-dimethylformamide solvent, and ultrasonically disperse the carbon nanotubes in the solvent for 2 hours, and the alkylated Add the N, N'-dimethylformamide solution of the carbon nanotubes to the above-menti...

Embodiment 3

[0036] (1) The multi-walled carbon nanotubes used in step (1) in Example 1 are replaced by double-walled carbon nanotubes, and octadecyl isocyanate is replaced by 3,4-dichlorophenylisocyanate, N,N'-dimethyl Base acetamide is changed into N-methylpyrrolidone, and other steps are with embodiment 1.

[0037] (2) Add 150ml of N-methylpyrrolidone solvent in the flask, nitrogen deoxygenation protection, add 24.0288g 4,4,-diaminodiphenyl sulfide, mechanically stir until completely dissolved, add 26.1744g of biphenyl in batches Tetraformic acid dianhydride was stirred for 5 h under an ice bath to obtain a light yellow polyamic acid (PAA) solution with a solid content of 25%.

[0038] (3) Weigh 2.5g of alkylated carbon nanotubes, put them into a sample bottle, add 20ml of N-methylpyrrolidone solvent, and ultrasonically 2h, so that the carbon nanotubes are dispersed in the solvent, and the alkylated carbon nanotubes Add the N-methylpyrrolidone solution of the tube into the above-mentio...

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Abstract

The invention relates to a process for preparing carbon nano-tube / polyimide compound fiber, which comprises the steps that: (1) the carbon nano-tube happens ultrasound in concentrated nitric acid and concentrated sulfuric acid, happens a reflux reaction and is cooled, washed and dried in a water bath, the carbon nano-tube which is acidulated and isocyanate are acted at room temperature through ultrasound, washing and drying. (2) Damine monomer is added into organic solvent and is mechanically stirred until being completely dissolved, equimolar dianhydride monomers are added in batches and are stirred in water bath, and polyamide acid solution is obtained. (3) The carbon nano-tube which is functionalized by the isocyanate is added into the polyamide acid solution to do the wet spinning, and then the carbon nano-tube / polyimide compound fiber which is made through the processes of amination and stretching. The invention has the advantages of simple preparation technology, low cost and no environmental pollution.

Description

technical field [0001] The invention belongs to the field of preparation of composite fibers, in particular to a preparation method of carbon nanotube / polyimide composite fibers. Background technique [0002] Polyimide is a class of polymers characterized by imide rings. This type of polymer has excellent heat resistance, mechanical and dielectric properties, as well as good impact resistance, radiation resistance and solvent resistance. At present, all kinds of polyimide products have been widely used in aerospace, electronic and electrical, automobile and other industries, but with the continuous development of modern industry, the performance requirements of materials are getting higher and higher. As a kind of high-tech fiber, polyimide fiber not only has high strength and modulus, but also has excellent thermo-oxidative stability. Polyimide fiber has a small coefficient of thermal expansion, low water absorption and good electrical insulation. Excellent radiation resi...

Claims

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Application Information

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IPC IPC(8): D01F1/10D01F6/60D01D5/06
Inventor 张清华李静罗伟强陈大俊程健
Owner DONGHUA UNIV
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