BPDA type bisphenol A tetramine branched polyimide resin thin film and preparation method thereof

A technology of polyimide resin and polyamic acid resin, which is applied in the field of polyimide film and its preparation, can solve the problem that it is difficult to obtain high molecular weight polyimide resin, the comprehensive performance of film products is reduced, and the cost of film products is reduced. Advanced problems, to achieve the effect of excellent dimensional stability, significant comprehensive performance superiority, excellent electrical properties and optical properties

Inactive Publication Date: 2017-03-22
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Its disadvantages are: (1) the raw material 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride monomer is extremely expensive, resulting in very high cost of film products, which seriously hinders its further application; ( 2) Due to the low reactivity of 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride monomer and aromatic dibasic primary amine, it is difficult to prepare high molecular weight polyimide resin, Therefore, the overall performance of its film products is greatly reduced, especially its mechanical properties.
At present, there are no published literature or patent reports about the BPDA type bisphenol A tetraamine branched polyimide resin film and its preparation method.

Method used

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  • BPDA type bisphenol A tetramine branched polyimide resin thin film and preparation method thereof
  • BPDA type bisphenol A tetramine branched polyimide resin thin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 180.0 g (0.9 mol) of 4,4'-diaminodiphenyl ether (DADPE), 10.8 (0.1 mol) of p-phenylenediamine (PPDA) and 1470 g of N,N-dimethylacetamide (DMAc) to the polymerization In the bottle, stir at room temperature. After completely dissolving, cool in an ice-water bath to below 5°C, add 297.1 grams (1.01 moles) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), stir, and 5 After reacting at °C for 1 hour, 1957.9 g of a homogeneous, transparent and viscous BPDA-type polyamic acid resin solution was obtained, which was designated as BPDA-PAA-1. Using Brookfield CAP2000+ vertebral plate viscometer, its viscosity at 50°C is measured as 630mPa.s. .

Embodiment 2

[0037] 262.8 grams (0.9 moles) of 1,4-bis(4-aminophenoxy)benzene (144BAPB), 10.8 grams (0.1 moles) of m-phenylenediamine (MPDA), 2000 grams of N,N-dimethylacetamide ( DMAc) and 920 grams of N-methyl-2-pyrrolidone (NMP) were added to the polymerization bottle, stirred at room temperature, after they were completely dissolved, cooled in an ice-water bath to below 5°C, and 308.9 grams (1.05 moles) of 3,3',4 , 4'-biphenyltetracarboxylic dianhydride (BPDA), stirred, and after 4 hours of reaction at 8°C, 3502.5 grams of homogeneous, transparent, viscous BPDA-type polyamic acid resin solution was obtained, which was recorded as BPDA-PAA- 2. Using Brookfield CAP2000+ vertebral plate viscometer, the viscosity at 50°C was measured as 572mPa.s.

Embodiment 3

[0039] 51.8 g (0.1 mole) of 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane (BAPFP), 180.0 g (0.9 mole) of 4,4'-diaminodiphenyl ether (DADPE ) and 3,290 grams of N-methyl-2-pyrrolidone (NMP) were added to the polymerization bottle, stirred at room temperature, and after they were completely dissolved, they were cooled in an ice-water bath to below 5°C, and 317.7 grams (1.08 moles) of 3,3',4, 4'-biphenyltetracarboxylic dianhydride (BPDA), stirred, reacted at 10°C for 6 hours, and obtained 3839.5 grams of homogeneous, transparent, viscous BPDA-type polyamic acid resin solution, recorded as BPDA-PAA-3 . Using Brookfield CAP2000+ vertebral plate viscometer, its viscosity at 50°C is measured as 425mPa.s.

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Abstract

The invention relates to a BPDA type bisphenol A tetramine branched polyimide resin thin film and a preparation method thereof. The mass ratio of BDAPP to BPDA type linear polyamide acid resin in raw materials of the thin film is 1:(100-800). The preparation method includes the steps that aromatic binary primary amine and strong-polar non-proton solvent are mixed, stirred at the room temperature and cooled to the temperature below 5 DEG C, BPDA is added, stirring is conducted, the mixture reacts for 1 h to 6 h at the temperature ranging from 5 DEG C to 10 DEG C, and a BPDA type polyamide acid resin solution is obtained; the resin solution and the BDAPP are mixed at the room temperature and stirred, form a film and are heated, the dehydration fever imidization reaction is conducted, cooling is conducted, film stripping is conducted, and the BPDA type bisphenol A tetramine branched polyimide resin thin film is obtained. The method is gentle in reaction condition, easy to operate, low in cost, friendly to the environment, beneficial to implementation of industrialized scale production and capable of being applied to the high-tech fields of flexible solar cells, space telescopes, large generator main insulation, electromagnetic wire lapped electrical insulating materials, flexible copper-clad plates and the like.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to a BPDA type bisphenol A tetramine branched polyimide resin film and its preparation method. Background technique [0002] Polyimide film is a kind of polymer material with excellent comprehensive properties. It has particularly excellent heat resistance, low temperature resistance, flame retardancy, electrical properties and mechanical properties. It is widely used in electronic microelectronics, printing High-tech fields such as circuit boards, wires and cables, motor main insulation, shipping, aerospace, lasers, and optoelectronics. [0003] However, traditional polyimide films, such as the KAPTON film produced by the American DUPONT company and the domestic H film, have a molecular structure of pyromellitic dianhydride, that is, the main monomer raw material is pyromellitic acid di anhydride and 4,4'-diaminodiphenyl ether. [0004] NASA (NASA) plans to launc...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08G73/10C08J5/18
CPCC08L79/08C08G73/1071C08J5/18C08J2379/08C08L2201/08C08L2201/10C08L2203/16
Inventor 虞鑫海周志伟
Owner DONGHUA UNIV
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