Carbon nanotubes and graphene covalently connected synergistically reinforced polyimide composite material and preparation method thereof

A technology of carbon nanotubes and covalent connection, which is applied in the field of carbon nanotubes and graphene covalently connected synergistically reinforced polyimide composite materials and its preparation, which can solve the problem that the product performance cannot achieve the desired effect and the application process limitations, etc. problems, to achieve the effect of easy industrial implementation, increased adhesion, and cheap raw materials

Active Publication Date: 2021-03-19
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Carbon nanotubes or graphene-modified polyimides prepared by the prior art fail to achieve the desired product performance, which is greatly restricted in the actual application process

Method used

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  • Carbon nanotubes and graphene covalently connected synergistically reinforced polyimide composite material and preparation method thereof
  • Carbon nanotubes and graphene covalently connected synergistically reinforced polyimide composite material and preparation method thereof
  • Carbon nanotubes and graphene covalently connected synergistically reinforced polyimide composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] One, the preparation of graphene oxide:

[0028] Using natural flake graphite as raw material, the modified Hummers method was used to prepare graphite oxide: 1g of 325 mesh natural flake graphite was added to 60mL of concentrated sulfuric acid, and the three-neck flask was placed in an ice-water bath and mechanically stirred, slowly adding 3g of sodium nitrate, and then adding 6g Potassium permanganate; after stirring in an ice-water bath for 1 hour, raise the temperature to 35°C and continue the reaction for 3 hours; then slowly add 200mL deionized water to the reaction system, raise the temperature to 90°C for 0.5h, and then add 10mL hydrogen peroxide, stirred for 5 min and then cooled to room temperature to obtain a yellow suspension. The suspension was centrifuged and washed with 1mol L -1 HCl was washed 3 times, and then repeatedly centrifuged and washed with deionized water until the pH of the system was about 6, and graphite oxide was obtained after freeze-dryi...

Embodiment 1

[0038] 1) Ultrasonic disperse self-prepared graphene oxide and carboxylated multi-walled carbon nanotubes of equal mass into N,N-dimethylformamide to obtain a co-dispersion with a concentration of 2mg / ml, add N,N- Dicyclohexylcarbodiimide (DCC) condensing agent, stirred for 0.5h, added ethylenediamine, reacted for 20h at 50°C, washed, and dried to obtain covalently connected carbon nanotubes and graphene; wherein ethylenediamine The mass is three times that of graphene oxide and carboxylated multi-walled carbon nanotubes, and the mass of DCC is twice that of ethylenediamine;

[0039] 2) Add 4.2 mg of covalently linked carbon nanotubes and graphene to 24 g of N,N-dimethylformamide, and sonicate for 1 hour; then add 2.0 g of 4,4'-diaminodiphenyl ether, in ice Stir mechanically in a water bath until the 4,4'-diaminodiphenyl ether is completely dissolved, then add 2.2g of pyromellitic dianhydride in batches, continue stirring for 12 hours after the addition, keep the reaction temp...

Embodiment 2～6

[0042] Only change the add-on of ethylenediamine in embodiment 1 step 1), as embodiment 2~6, list is as follows:

[0043]

[0044] Performance tests were performed on the film-like covalently linked carbon nanotubes and graphene / polyimide composite materials prepared in Examples 1-6, and Table 1 was obtained. The test method for the data in Table 1 is as follows:

[0045] X-ray photoelectron spectroscopy (XPS) (EDAX GENESIS) was used to measure the atomic content of N element, using Al Kα, hν=1486.4eV.

[0046] The tensile test was carried out by SSANS-20KN electronic universal testing machine (Shanghai, Xinsansi), the test environment temperature was 25°C, and the tensile speed was 5mm min -1 , each sample was measured 5 times and the average value was taken as the final data.

[0047] DMA242C (Germany, NETZSCH) analyzer was used for dynamic thermal analysis test, using tensile mode, temperature range: 100-500 ° C; heating rate: 5 ° C min -1 ; Static compressive stress:...

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Abstract

The invention discloses a covalently-bonded carbon nanotube and graphene synergistically-enhanced polyimide composite material and a preparation method thereof. The method comprises the following steps: dispersing graphene oxide and carboxylated carbon nanotubes in an organic solution, adding a DCC or EDC / NHS condensing agent, stirring, adding an organic substance containing two or more amino groups, carrying out a reaction, washing, and drying to obtain carbon nanotubes and graphene which are covalently bonded; mixing the carbon nanotubes and graphene, which are covalently bonded, with a dibasic anhydride monomer and a diamine monomer in an organic solvent, and carrying out in-situ polymerization under the protection of nitrogen at 10-30 DEG C to obtain a covalently bonded carbon nanotubeand graphene / polyamic acid solution; preparing the obtained solution into a desired form by using a composite material processing method; removing the solvent, and carrying out heat treatment and polyimidization to obtain the covalently bonded carbon nanotube and graphene / polyimide composite material. The method enables the carbon nanotubes and the graphene to be covalently bonded, thus enhancingthe interfacial action and beneficial to improvement of mechanical properties and heat stability of the product.

Description

technical field [0001] The invention relates to the field of composite materials, in particular to a carbon nanotube and graphene covalently connected synergistically reinforced polyimide composite material and a preparation method thereof. Background technique [0002] Polyimide has many excellent properties such as high temperature resistance, low temperature resistance, high strength and high modulus, radiation resistance, corrosion resistance, high creep resistance, high dimensional stability, low thermal expansion coefficient, low dielectric constant and loss, and high electrical insulation. Widely used in various fields. However, with the rapid development of modern industry, the requirements for the materials used are getting higher and higher, and the traditional polyimide can no longer meet the requirements. Corresponding modification of polyimide is required to prepare polyimide composite materials with higher temperature resistance, high strength and high modulus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08K9/04C08K3/04C08K7/24C08K9/02C08J5/18
CPCC08G73/1071C08J5/18C08J2379/08C08K3/04C08K7/24C08K9/02C08K9/04C08K2201/011
Inventor 石海峰张雨霞王海霞余文凯刘博
Owner TIANJIN POLYTECHNIC UNIV
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