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A kind of preparation method of nano polyimide film

A technology of polyimide film and polyimide, applied in the field of preparation of nanometer polyimide film

Active Publication Date: 2019-06-28
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Ultra-thin film materials have always played an important role in aerospace, microelectronics, automobiles, chemical separation and new printing industries. Polyamide ultra-thin film materials with high tolerance and electrical insulation have received more attention. With the development of the electronics industry and new printing industry, the emergence of new technologies and the development of components in the direction of miniaturization and light weight, the existing polyamide film materials can no longer meet the needs of technology, and there is an urgent need for film materials with better performance

Method used

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  • A kind of preparation method of nano polyimide film
  • A kind of preparation method of nano polyimide film
  • A kind of preparation method of nano polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1) Mix 3,4,3',4'-terphenyl dianhydride and 4,4'-diaminodiphenylmethane evenly, then add 20 parts of high boiling point solvent N-methylpyrrolidone and mix to form a uniform system , and then under the protection of nitrogen, the homogeneous system was heated to 180°C for 1 hour, and then slowly cooled to 50°C to obtain a polyimide precursor with a carboxylic acid structure, and then to the polyimide with a carboxylic acid structure 4,4'-diphenylmethane diisocyanate was added to the precursor, and the temperature was raised to 120°C for 3 hours to obtain a polyimide resin with a viscosity of 4500 centipoise, wherein the 3,4,3',4'-para Terphenyldianhydride, 4,4'-diaminodiphenylmethane and 4,4'-diphenylmethane diisocyanate are proportioned according to a molar ratio of 1:0.5:0.3;

[0052] 2) In parts by mass, 10 parts of polyimide resin, 85 parts of polar organic solvent N,N-dimethylformamide, 0.1 part of diluent chlorobenzene, 1 part of film-forming agent cresol , the mo...

Embodiment 2

[0055] 1) Mix 3,4,3',4'-terphenyl dianhydride and 4,4'-diaminodiphenylmethane evenly, then add 30 parts of high boiling point solvent N-methylpyrrolidone and mix to form a uniform system , and then under the protection of nitrogen, the homogeneous system was heated to 180°C for 0.5 hours at a constant temperature, and slowly cooled to 55°C to obtain a polyimide precursor with a carboxylic acid structure, and then to the polyimide precursor with a carboxylic acid structure Add 4,4'-diphenylmethane diisocyanate to the body and slowly raise the temperature to 140°C for 0.5 hours to obtain a polyimide resin with a viscosity of 4000 centipoise, wherein the 3,4,3',4'-pair triple Phthalic anhydride, 4,4'-diaminodiphenylmethane and 4,4'-diphenylmethane diisocyanate are proportioned according to the molar ratio of 0.9:0.5:0.4;

[0056] 2) In parts by mass, 45 parts of polyimide resin, 90 parts of polar organic solvent pyridine, 0.2 part of thinner dimethyl phthalate, 1 part of film-for...

Embodiment 3

[0059] 1) Mix 3,4,3',4'-terphenyl dianhydride and 4,4'-diaminodiphenylmethane evenly, then add 50 parts of high boiling point solvent N-methylpyrrolidone and mix to form a uniform system , and then under the protection of nitrogen, the homogeneous system was heated to 180°C for 2 hours at a constant temperature, and slowly cooled to 60°C to obtain a polyimide precursor with a carboxylic acid structure, and then to the polyimide precursor with a carboxylic acid structure Add 4,4'-diphenylmethane diisocyanate to the body and slowly raise the temperature to 140°C for 3 hours to obtain a polyimide resin with a viscosity of 2800 centipoise, wherein the 3,4,3',4'-pair triple Phthalic anhydride, 4,4'-diaminodiphenylmethane and 4,4'-diphenylmethane diisocyanate are proportioned according to the molar ratio of 0.8:0.5:0.5;

[0060] 2) In parts by mass, 20 parts of polyimide resin, 80 parts of polar organic solvent dimethyl sulfone, 0.2 part of diluent isophorone, 1 part of film-forming...

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Abstract

The invention provides a method for preparing a polyimide nano-film. The method comprises the steps: firstly, synthesizing polyimide resin from aromatic tetracid dihydride, aromatic diamine and aromatic diisocyanate; and then, mixing the polyimide resin, a polar organic solvent, a diluent, a film forming agent and a molecular weight regulator so as to obtain a polyimide solution system, then, carrying out nano-scale uniform spreading on a clean substrate by dint of the action of a mechanical external force of 0.5N to 30N, and then, carrying out an imidization method, thereby preparing the polyimide nano-film. According to the film, the high-temperature resistance is 10 seconds at the high temperature of 400 DEG C to 750 DEG C, and the electrical insulation property is that the dielectric constant is 1.5 to 4.5 at the frequency of 103Hz. Compared with the prior art, the polyimide nano-film prepared by the method has the advantages of excellent surface physical properties and stable chemical properties, high-temperature resistance, electrical insulation properties and chemical corrosion resistance.

Description

technical field [0001] The invention belongs to the field of ultra-thin film materials, and in particular relates to a preparation method of a nanometer polyimide film. Background technique [0002] Ultra-thin film materials have always played an important role in aerospace, microelectronics, automobiles, chemical separation and new printing industries. Polyamide ultra-thin film materials with high tolerance and electrical insulation have received more attention. With the development of the electronics industry and new printing industry, the emergence of new technologies and the development of components in the direction of miniaturization and light weight, the existing polyamide film materials can no longer meet the technical needs, and there is an urgent need for film materials with better performance. In order to meet the needs of the market, a new type of polyimide nano-ultra-thin film with excellent surface physical and chemical properties, chemical corrosion resistance...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10
CPCC08G73/1035C08G73/1067C08G73/1071C08J5/18C08J2379/08
Inventor 刘保健杨军陆洪林王新玲杨强杨辉郭博毅崔瑞王阳安赵璐李国栋向富康
Owner SHAANXI UNIV OF SCI & TECH
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