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Preparation method for polyimide/oxidized graphene nanocomposite film

A polyimide and nanocomposite technology, applied in the field of preparation of functional polymer materials, can solve the problems of poor dispersion and poor wear resistance, and achieve the effects of simple process, improved tribological performance, and short preparation process

Inactive Publication Date: 2014-02-19
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] From the perspective of improving the comprehensive performance of materials, the present invention prepares a polyimide / graphene oxide nanocomposite film, which solves the problem of poor dispersion of graphene in organic solvents and polymer matrices and the use of polyimide alone Disadvantages such as poor wear resistance

Method used

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  • Preparation method for polyimide/oxidized graphene nanocomposite film
  • Preparation method for polyimide/oxidized graphene nanocomposite film
  • Preparation method for polyimide/oxidized graphene nanocomposite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of graphene oxide:

[0025] Accurately weigh 3g of graphite and 1.5g of sodium nitrate, dissolve them together in 69ml of 98% concentrated sulfuric acid, stir mechanically for 30min in an ice-water bath, slowly add 9g of potassium permanganate, and wait until the potassium permanganate is fully dissolved , the temperature was raised to 35° C. for 1 hour to form a thick liquid. Add 69ml of distilled water dropwise, raise the temperature to 98°C, and react for 15 minutes. Pour the mixture into a mixture of 140ml distilled water, 20ml hydrogen peroxide (30%) and 400ml 20% hydrochloric acid. The mixture was filtered and centrifuged with 20% hydrochloric acid and distilled water and washed until neutral until the sulfate ion could not be detected with barium chloride, and then put into a vacuum drying oven at 40°C for 48 hours to prepare graphite oxide.

[0026] (2) Preparation of polyimide / graphene oxide nanocomposite film:

[0027] Weigh 0.010559g of gr...

Embodiment 2

[0029] (1) Same as (1) in Example 1

[0030] (2) Preparation of polyimide / graphene oxide nanocomposite film:

[0031] Weigh 0.031677g of graphene oxide, and ultrasonically disperse it in N, N′-dimethylformamide solvent, so as to obtain a suspension of graphene oxide flakes. 5g of 4,4'-diaminodiphenylsulfide was added to the mixed solution, and stirred under the protection of nitrogen to make it completely dissolved, and then a small amount of 5.559g of perphthalic anhydride was uniformly added to the solution several times, and the It was reacted in an ice bath for 2 hours to prepare a polyamic acid / graphene oxide composite solution. Coat the polyamic acid / graphene oxide composite solution on the glass mold, then put it in a blast drying oven at 60°C for 2 hours to remove the N, N′-dimethylformamide solvent, and then raise the temperature gradually in the blast drying oven , 100°C for 1h, 150°C for 30min, 200°C for 30min, 250°C for 30min, 300°C for 30min. After the imidizati...

Embodiment 3

[0033] (1) Same as (1) in Example 1

[0034] (2) Preparation of polyimide / graphene oxide nanocomposite film:

[0035] Weigh 0.052795g of graphene oxide, and ultrasonically disperse it in N-methylpyrrolidone solvent to obtain graphene oxide flake suspension. 5g of diaminodiphenylmethane was added to the mixed solution, and stirred under the protection of nitrogen to make it completely dissolved, then a small amount of 5.559g of biphenyltetracarboxylic dianhydride was evenly added to the solution several times, and it was placed in an ice bath. The reaction was carried out for 3 hours to prepare a polyamic acid / graphene oxide composite solution. Coat the polyamic acid / graphene oxide composite solution on the glass mold, and then put it in a blast drying oven at 60°C for 2 hours to remove the N-methylpyrrolidone solvent, then gradually increase the temperature in the blast drying oven at 100°C for 1h, 150°C for 30min, 200°C for 30min, 250°C for 30min, 300°C for 30min. After the...

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Abstract

The invention relates to a preparation method for a polyimide / oxidized graphene nanocomposite film, and belongs to the technical field of preparation of functional polymer materials. The preparation method comprises the following steps: performing ultrasonic even dispersion on the oxidized graphene in an organic solvent to obtain an oxidized graphene sheet suspension, wherein per ml of the oxidized graphene sheet suspension contains 1.3*10<-5>-1.3*10<-4>g oxidized graphene sheets; introducing nitrogen for carrying out deoxidization protection, adding diamine monomers into the suspension, mechanically stirring until full dissolution is achieved, adding dianhydride monomers, the moles of which are equal to that of the diamine monomers, in batches, and mixing for one to six hours under the ice bath conditions, so as to obtain polyamide acid / oxidized graphene composite solution; pouring the polyamide acid / oxidized graphene composite solution onto a die, removing the organic solvent, performing gradient temperature rise within 100-300DEG C, and carrying out thermal imidization to obtain the polyimide / oxidized graphene nanocomposite film.

Description

technical field [0001] The invention relates to a preparation method of a polyimide / graphene oxide nanocomposite film, in particular to a method for preparing a polyimide / graphene oxide nanocomposite film by in-situ polymerization, which belongs to the preparation of functional polymer materials technology field. Background technique [0002] Polyimide usually refers to a special class of polymer materials containing imide groups on the main chain of the molecule. As a matrix of high-performance composite materials, its structural main chain usually contains five-membered heterocyclic units, making it It exhibits very special properties and is widely used in high-tech fields such as high temperature resistance, low temperature resistance, radiation resistance, flame retardancy, self-lubrication and microelectronics; polyimide is used as a self-lubricating and wear-resistant material in aerospace and other fields In the friction system, it has been paid more and more attenti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08G73/10C08K9/00C08K3/04
CPCC08K9/00C08G73/1007C08J5/18C08J2379/08C08K3/04
Inventor 闵春英聂鹏宋浩杰曾名沈聃唐华杨小飞
Owner JIANGSU UNIV
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