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Preparation method of polyimide/graphene nanocomposite material

A nanocomposite material and polyimide technology, which is applied in the field of preparation of functional polymer materials, can solve the problems that graphene is not easy to be prepared in large quantities, and achieve the effects of convenient operation, easy industrialization, and simple process

Active Publication Date: 2011-12-07
YANGZHONG HUAXIN FUSHU ELECTRICAL EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, graphene is not easy to prepare in large quantities, and it exists in the form of aggregates in the macroscopic form. In order to make full use of its high strength, high modulus, high electrical conductivity, good chemical and heat resistance, and high specific surface area, it needs to be physically or chemically modified. The method of applying graphene to the reinforcement of polymer materials also has important academic value
To this end, related research Macromolecules 2010, 43, 2357–2363, ACS Nano 2009, 3, 3884-3890, Macromolecules 2010, 43, 6716–6723, ACS Applied Materials & Interface 2010, 2, 1707-1713, added graphene Polyvinyl alcohol, epoxy, nylon 6, chitosan and other polymer matrices to improve the mechanical, thermal and electrical properties of these polymers, and the research on functionalized graphene modified polyimide nanocomposites Not yet reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] a. Synthesis of graphite oxide: use 5 g of natural graphite as raw material, add 200 ml of concentrated sulfuric acid, 5 g of sodium nitrate and stir in an ice bath for 30 min, then slowly add 10 g of potassium permanganate until the potassium permanganate is completely dissolved Finally, transfer the reaction system to a 35°C water bath and stir for half an hour. Slowly add 200 ml of deionized water to the reaction system, continue stirring, then add 50 ml of 30% hydrogen peroxide solution, and finally dissolve the above solution Centrifugal filtration, washing with water several times until neutral, and drying can produce graphite oxide.

[0011] b. Preparation of polyimide / graphene nanocomposites: Disperse 0.1g of graphite oxide in 100 ml of N,N-dimethylacetamide, N,N-dimethylformamide or methylpyrrolidone), ultrasonic After dispersing for 30 minutes, add 10 ml of toluene diisocyanate and continue to sonicate for 30 minutes. Then add 10.05g of diaminodiphenyl eth...

Embodiment 2

[0013] a. The graphite oxide preparation process and steps in the present embodiment are the same as those in Example 1a. The difference is the preparation of polyimide / graphene nanocomposites.

[0014] b. Preparation of polyimide / graphene nanocomposite: Disperse 0.1 g of graphite oxide in 100 ml of organic solvent N,N-dimethylformamide, ultrasonically disperse for 30 minutes, add 10 ml of toluene diisocyanate and continue ultrasonication 30 minutes. Then add 5.05g of diaminodiphenylmethane, stir evenly, add 5.55g of biphenyltetracarboxylic dianhydride, stir at room temperature for 12 hours, and heat the product in an oven at 100°C for 30 minutes, at 180°C for 30 minutes, and at 250°C Heating for 1 hour and heating at 350° C. for 2 hours to obtain a polyimide / graphene nanocomposite material.

Embodiment 3

[0016] a. The graphite oxide preparation process and steps in the present embodiment are the same as those in Example 1a. The difference is the preparation of polyimide / graphene nanocomposites.

[0017] b. Preparation of polyimide / graphene nanocomposite: Take 0.1g of graphite oxide and disperse in 100 ml of organic solvent methylpyrrolidone, after ultrasonic dispersion for 30 minutes, add 10 ml of 1,6 hexamethylene diisocyanate and continue ultrasonication for 30 minutes . Then add 5.05g of diaminodiphenylmethane, stir evenly, then add 5.55g of biphenyltetracarboxylic dianhydride, stir at room temperature for 24 hours, the product is heated in an oven at 100°C for 30 minutes, at 180°C for 30 minutes, at 250°C Heating for 1 hour and heating at 350° C. for 2 hours to obtain a polyimide / graphene nanocomposite material.

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Abstract

The invention discloses a preparation method for a polyimide / graphene nanocomposite material. The method is characterized by: adopting graphite as a raw material; adopting a modified Hummers method for synthesis of a graphene oxide; adopting an organic molecule containing isocyanic acid radical to modify the graphene oxide; uniformly dispersing the surface modified graphene oxide in an organic solvent system, adding equivalent dianhydride monomer and equivalent diamine monomer at a temperature of 0-25 DEG C after uniformly dispersing; continuously carrying out the reaction for 6-24 hours, followed by carrying out heat treatment for the resulting solution to prepare the high-performance polyimide / graphene nanocomposite material. With the prepared polyimide / graphene nanocomposite material through an in situ polymerization method, dispersing problems and compatibility problems of the graphene in the polyimide matrix are solved, the polyimide nanocomposite material with good dispersity isobtained. In addition, the prepared material provided by the present invention has potential application values in the fields of heat resistant materials, structural materials, conductive materials, adhesives, and the like.

Description

technical field [0001] The invention belongs to a preparation method of a functional polymer material, in particular to a preparation method of a polyimide / graphene nanocomposite material. Background technique [0002] Polyimide (PI) is an aromatic heterocyclic polymer containing imide groups in the repeating unit. Polyamic acid is formed by the reaction of organic aromatic diacid anhydride and organic aromatic diamine by melt polycondensation or solution polycondensation. After heating or A polymer material obtained by chemical imidization. Due to the very stable aromatic heterocyclic structural unit in the PI molecule, it has excellent properties unmatched by other polymers, so it is widely used in aerospace, electrical, microelectronics and automobile industries. However, due to the macromolecular orientation effect of the PI with rigid structure prepared by pyromellitic anhydride, which is widely used at present, the dielectric properties are anisotropic, which is diffi...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08K9/04C08K3/04
Inventor 贡津
Owner YANGZHONG HUAXIN FUSHU ELECTRICAL EQUIP
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