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Preparation method of graphene/polyimide composite film

A technology of composite film and polyimide, which is applied in the field of preparation of multifunctional films, can solve the problems of long reaction time, high reaction temperature, complicated preparation process, etc., and achieves mild reaction conditions, simple and easy technological process, and preparation cost. low cost effect

Inactive Publication Date: 2016-07-13
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although graphene can be uniformly dispersed in the polyimide matrix resin in the graphene / polyimide composite films prepared by the above two methods, these two methods are based on the two-step process of polyimide The method of preparation technology has the disadvantages of long reaction time, high reaction temperature and complicated preparation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under the protection of nitrogen at room temperature and pressure, first add 30 grams of N,N-dimethylformamide, 0.3 g of graphene oxide and magnetons into a 100 ml three-necked flask, and then add 2.5 grams of polyphenyl polymethylene polycyanide Ester, sonicate for 2 hours to disperse graphite oxide uniformly and fully react with isocyanate groups. Then add 3 grams of 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA), while the three-neck flask was placed in an oil bath heated to 90°C in advance for 2 hours and connected to reflux condensation device, stop the reaction when BTDA is completely dissolved and no bubbles are produced. The prepared composite solution was uniformly coated on a glass plate, and placed in a resistance furnace control box for gradient heating (100°C, 200°C, 300°C for 1 hour) for thermal imidization, and finally prepared graphene / polyamide imine composite film.

Embodiment 2

[0028] Under the protection of nitrogen at room temperature and pressure, first add 30 grams of N-methylpyrrolidone, 0.4 g of graphene oxide and magnetons in a 100 ml three-necked flask, and then add 2.5 grams of polyphenylpolymethylene polycyanate, and ultrasonically 2 hours of treatment to disperse graphite oxide evenly and fully react with isocyanate groups. Then add 3 grams of 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA), while the three-neck flask was placed in an oil bath heated to 90°C in advance for 2 hours and connected to reflux condensation device, stop the reaction when BTDA is completely dissolved and no bubbles are produced. The prepared composite solution was uniformly coated on a glass plate, and placed in a resistance furnace control box for gradient heating (100°C, 200°C, 300°C for 1 hour) for thermal imidization, and finally prepared graphene / polyamide imine composite film.

Embodiment 3

[0030] Under room temperature and normal pressure nitrogen protection conditions, first add 30 grams of N-methylpyrrolidone, 0.4 g of aminated graphene and magnetons in a 100 ml three-necked flask, and then add 2.5 grams of polyphenyl polymethylene polycyanate, Ultrasonic treatment for 2 hours makes graphite oxide uniformly dispersed and fully reacted with isocyanate groups. Then add 2 grams of pyromellitic dianhydride (PMDA), and place the three-neck flask in an oil bath preheated to 90°C for 2 hours and connect it to a reflux condensing device. Stop when BTDA is completely dissolved and no bubbles are produced. reaction. The prepared composite solution was uniformly coated on a glass plate, and placed in a resistance furnace control box for gradient heating (100°C, 200°C, 300°C for 1 hour) for thermal imidization, and finally prepared graphene / polyamide imine composite film.

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Abstract

The invention provides a preparation method of a graphene / polyimide composite film. The preparation method comprises the steps that functionalized graphene is uniformly dispersed into a polar solvent at room temperature; then polyisocyanate is added to the polar solvent containing functionalized graphene, after sufficient reaction of functional groups on functionalized graphene with polyisocyanate, a poly-aromatic anhydride monomer is added for a reaction, and a graphene / polyimide precursor solution is prepared; the graphene / polyimide composite film is obtained finally through gradient heating thermal imidization. The method is based on a one-step preparation technology of polyimide, the preparation time and the preparation process of the graphene / polyimide composite film are shortened greatly on the basis that graphene is uniformly dispersed in polyimide matrix resin, and the reaction temperature is reduced effectively. The preparation process is simple, the preparation cost is low, the reaction conditions are mild, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for preparing a multifunctional film, in particular to a new method for preparing a graphene / polyimide composite film. Background technique [0002] Graphene is composed of single atomic layer sp 2 The two-dimensional material composed of hybridized carbon atoms closely arranged has unique physical and chemical properties such as excellent electrical properties, outstanding thermal conductivity, extraordinary specific surface area and perfect quantum tunneling effect. [0003] Polyimide film is a high-performance polymer film material with excellent electrical properties, mechanical properties, high temperature resistance and corrosion resistance. It has been widely used as high-performance insulating materials in the fields of aerospace, electronics and electrical. [0004] Graphene / polyimide composite film is an advanced film material that combines the excellent properties of graphene and polyimide, two high-perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G73/10C08L79/08C08K9/00C08K3/04
CPCC08J5/18C08G73/1035C08J2379/08C08K3/04C08K9/00C08L2203/16
Inventor 王君孙高辉韩世辉刘连河张超王文鹏魏浩
Owner HARBIN ENG UNIV