Self-repairing and recoverable polyimide insulating film as well as preparation method and application thereof

A polyimide and insulating film technology, which is applied in the field of self-repairing and recyclable polyimide insulating film and its preparation, can solve the problem of limited repair times of polymer matrix, difficulty in achieving material properties, and reduced material use efficiency, etc. problem, to achieve a balance between repair performance and high glass transition temperature, to facilitate recycling and repair, and to ensure the effect of insulating performance

Active Publication Date: 2022-05-10
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has a limited number of repairs to the polymer matrix and is not conducive to the repair of electrical dendrites after electrical damage.
In addition, the performance of the material itself after repeated repairs is also difficult to reach the original level, which reduces the use efficiency of the material
[0004] Therefore, it is still a great challenge to be able to design and prepare high-performance self-healing, recyclable polyimide insulation materials

Method used

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  • Self-repairing and recoverable polyimide insulating film as well as preparation method and application thereof
  • Self-repairing and recoverable polyimide insulating film as well as preparation method and application thereof
  • Self-repairing and recoverable polyimide insulating film as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0041] In the first aspect, a method for preparing self-repairing and recyclable polyimide insulating film is provided, comprising the steps of:

[0042] S1. In the presence of the first solvent, the amino monomer, 4,4'-(4,4'-isopropyldiphenoxy)bis(phthalic anhydride) is subjected to the first polymerization reaction to obtain amino-blocked Terminal copolymerized polyamic acid solution; the amino monomers include 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (ie 6FAPB) and / or 9,9-bis(3- Fluoro-4-aminophenyl)fluorene (i.e. FFDA);

[0043]S2. The copolymerized polyamic acid solution obtained in step S1 is subjected to azeotropic water removal treatment with an organic solvent, and then subjected to precipitation and drying to obtain amino-terminated low molecular weight copolymerized polyimide powder.

[0044] Preferably, the precipitation is carried out in absolute ethanol.

[0045] S3. In the presence of a second solvent, the polyimide powder obtained in step S2 and the t...

Embodiment 1

[0100] 0.857g 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene and 0.769g 9,9-bis(3-fluoro-4-aminophenyl)fluorene were equally divided into two parts, followed by Dissolve 0.385g of 9,9-bis(3-fluoro-4-aminophenyl)fluorene in 30mL of N-methylpyrrolidone and stir until completely dissolved; then add 1.041g of 4,4'-(4,4' -isopropyldiphenoxy)bis(phthalic anhydride), and in N 2 Stir at 0°C for 30min in the atmosphere; then add 0.429g 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene into the solution, and 2 Stir at 0°C for 30min in the atmosphere; finally add 0.385g 9,9-bis(3-fluoro-4-aminophenyl)fluorene, 0.429g 1,4-bis(4-amino-2-trifluoromethyl Phenoxy) benzene was added at intervals of 30min respectively, and in N 2 Stirred at 0°C for 18h in atmosphere.

[0101] Add 4.5mL of toluene to the polyamic acid solution obtained above and transfer it to a three-necked flask with a Dean-Stark condenser; then heat to 210°C, azeotropically remove water for 9h; then cool the solution to r...

Embodiment 2

[0104] According to the method of Example 1, the difference is that one of the amino monomers is different, specifically, 0.857 g of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene in Example 1 replaced by 0.585 g of 1,3-bis(4'-aminophenoxy)benzene, and an additional 0.429 g of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene was replaced by 0.293 g 1,3-bis(4'-aminophenoxy)benzene, other parameters are the same as in Example 1, (that is, two amino monomers, 4,4'-(4,4'-isopropyldi The volume ratio of the total mass of phenoxy) two (phthalic anhydride) and solvent is preferably 2.4g: (25~30) mL), obtain polyimide film, denoted as RPI2, thickness is 15-20 μ m, It can perform multiple monomer recovery and repolymerization, and self-repair under certain conditions.

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Abstract

The invention provides a self-repairing and recoverable polyimide insulating film as well as a preparation method and application thereof, and belongs to the technical field of insulating films. Comprising the following steps: S1, carrying out first polymerization reaction on an amino monomer and 4, 4 '-(4, 4'-isopropyl diphenoxy) bis (phthalic anhydride) to obtain an amino-terminated copolymerized polyamide acid solution; the amino monomer comprises 1, 4-bis (4-amino-2-trifluoromethyl phenoxy) benzene and/or 9, 9-bis (3-fluoro-4-aminophenyl) fluorene, and the amino monomer comprises 1, 4-bis (4-amino-2-trifluoromethyl phenoxy) benzene and/or 9, 9-bis (3-fluoro-4-aminophenyl) fluorene; s2, carrying out azeotropic water removal treatment on the copolymerized polyamide acid solution and an organic solvent to obtain polyimide powder; s3, carrying out a second polymerization reaction with a tri-aldehyde group cross-linking agent; and S4, carrying out a thermal cross-linking reaction at the temperature of 250-300 DEG C. The film disclosed by the invention can be recycled and repaired for multiple times, and has the advantages of low dielectric constant, good mechanical property, high thermal stability, high insulation characteristic and excellent insulation property recovery capability.

Description

technical field [0001] The invention relates to the technical field of self-repairing and recyclable polyimide insulating film, in particular to a self-repairing and recyclable polyimide insulating film and its preparation method and application. Background technique [0002] Polyimide (Polyimide), as a high-performance polymer material with an imide ring structure, is widely used in electrical, electronic and Insulation technology and other fields. However, due to the insoluble properties of traditional polyimide films, they cannot be repaired and recycled in time after damage, especially electrical damage, resulting in serious waste of resources and environmental pollution. [0003] In existing technical means, in order to increase the utilization rate of macromolecule insulating material, generally be to fill in the microcapsule filler that has solidification characteristic in matrix, as the epoxy resin of surface grafted amino group and calcium alginate base microcapsul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08C08K5/07C08J5/18C08J3/24
CPCC08G73/1071C08G73/1039C08G73/1007C08J5/18C08J3/247C08J2379/08C08K5/07
Inventor 查俊伟万宝全
Owner UNIV OF SCI & TECH BEIJING
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