Method for preparing graphene/polyimide composite fibers

A composite fiber and polyimide technology, applied in the direction of fiber chemical characteristics, conductive/anti-static filament manufacturing, single-component synthetic polymer rayon, etc., can solve spinning forming difficulties, uneven dispersion and interface bonding etc., to achieve the effect of solving the interface adhesion problem, solving the uneven dispersion and improving the stability

Inactive Publication Date: 2012-07-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by this invention is to provide a kind of preparation method of graphene/polyimide composite fiber, this method overcomes the difficult problem of the sp...

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  • Method for preparing graphene/polyimide composite fibers
  • Method for preparing graphene/polyimide composite fibers
  • Method for preparing graphene/polyimide composite fibers

Examples

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Embodiment 1

[0034] (1) Using natural graphite as raw material, the Hummer method is used to prepare graphite oxide. That is, 92ml concentrated sulfuric acid was added to the three-necked flask, stirred in an ice water bath until the temperature dropped to 0℃~3℃, and then 4g natural graphite powder and 2g sodium nitrate (NaNO 3 ), then stir evenly, while stirring, slowly add 60g potassium permanganate (KMnO 4 ) And ensure that the temperature is less than 20°C. After the addition is complete, heat the solution to 35±3°C and keep it for 30min, then slowly add distilled water and control the temperature within 100°C; after 15min, add a lot of distilled water and 10ml 30% hydrogen peroxide (H 2 O 2 ), the reaction is terminated. The mixture was centrifuged, filtered, washed several times with an aqueous solution containing 5% HCl, and dried in vacuum at 50°C to obtain a graphite oxide sample; then 2.5g of graphite oxide was dispersed in 100ml of N,N'-dimethylacetamide ( In DMAc), a yellow-brow...

Embodiment 2

[0040] (1) Using artificial graphite as raw material, graphite oxide is prepared by the Staudenmaier method. Disperse graphite oxide in water, ultrasonic power of 500W, ultrasonic for 60 minutes, first centrifuge at 5000 rpm for 4 minutes, collect the upper layer solution, then centrifuge at 15000 rpm for 2 minutes, collect the precipitate, and vacuum dry at 60°C to obtain graphene oxide powder. Take 2.5g of graphene oxide and disperse it in 100ml of N,N'-dimethylacetamide (DMAc) to obtain a yellow-brown dispersion. After 30 minutes of sonication, the exfoliated graphene oxide suspension uniformly dispersed in DMAc is obtained .

[0041] (2) Put 18.02g of 4,4'-diaminodiphenyl ether (ODA) into a three-necked flask, then add 150ml of DMAc solvent, deoxidize with nitrogen, and mechanically stir until completely dissolved, add 28.98g of ketone in batches Anhydride (BTDA), 50ml of DMAc solvent was added again, and stirring was carried out for 3 hours in an ice bath to obtain a light...

Embodiment 3

[0046] (1) Using artificial graphite as raw material, the Brodie method is used to prepare graphite oxide. Disperse graphite oxide in water, ultrasonic power of 500W, ultrasonic for 60 minutes, first centrifuge at 5000 rpm for 4 minutes, collect the upper layer solution, then centrifuge at 15000 rpm for 2 minutes, collect the precipitate, and vacuum dry at 60°C to obtain graphene oxide powder. Take 5g of graphene oxide and disperse it in 100ml of N,N'-dimethylacetamide (DMAc) to obtain a yellow-brown dispersion. After sonicating for 100 minutes, an exfoliated graphene oxide suspension uniformly dispersed in DMAc is obtained.

[0047] (2) Add 20.18g of benzimidazole (BIA) into a three-necked flask, then add 150ml of DMAc solvent, deoxidize with nitrogen, stir mechanically until it is completely dissolved, add 27.92g of ether anhydride (ODPA) in batches, and again Add 50ml of DMAc solvent and stir for 3h in an ice bath to obtain a light yellow polyamic acid (PAA) solution with a s...

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Abstract

The invention relates to a method for preparing graphene/polyimide composite fibers. The method comprises the following steps of: (1) preparing graphene or graphene oxide; (2) preparing a graphene/polyamic acid spinning solution; and (3) preparing graphene/polyimide or graphene oxide/polyimide composite fibers. According to the method, through adopting stripped graphene layers as addition materials of polyimide fibers, the spinnability of the polyamic acid spinning solution is improved, the stability of the polyamic acid fibers is improved, the improvement on the performance of the fibers is facilitated, and thus, the polyimide fibers with excellent performance are prepared; and with the adoption of the method, the problem of difficulty in the spinning and the forming of the polyamic acid fibers is solved, the mechanical properties of the composite fibers is improved, meanwhile, the problems of uneven dispersion and interfacial adhesiveness of the graphene in a matrix polymer are solved.

Description

Technical field [0001] The invention belongs to the field of preparation of polyimide fibers, and particularly relates to a preparation method of graphene / polyimide composite fibers. Background technique [0002] Polyimide is a type of polymer with imide ring as its characteristic structure. 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, various polyimide products have been widely used in aerospace, electronic and electrical, automotive and other industries, but with the continuous development of modern industry, the performance requirements of materials are becoming higher and higher. As a kind of high-tech fiber, polyimide fiber not only has high strength and modulus, but also has excellent thermal oxidation stability. Polyimide fiber has a small thermal expansion coefficient, low water absorption, and good electrical insulation. Excellent rad...

Claims

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Application Information

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IPC IPC(8): D01F6/94D01F1/09D01F1/10C08G73/10D01D5/06D01D5/12
Inventor 张清华尹朝清王亚平夏清明董杰陈大俊
Owner DONGHUA UNIV
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