HQDA type 14BDAPB branched polyimide resin 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: 2017-05-10
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 HQDA type 14BDAPB branched polyimide resin film and its preparation method

Method used

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  • HQDA type 14BDAPB branched polyimide resin film and preparation method thereof
  • HQDA type 14BDAPB branched polyimide resin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 43.2 (0.4 mol) p-phenylenediamine (PPDA), 100.0 g (0.5 mol) 4,4'-diaminodiphenyl ether (44ODA), 22.4 (0.1 mol) 2-(4-aminophenyl)-5 -Aminobenzimidazole (APABI) and 1720 grams of N-methyl-2-pyrrolidone (NMP) were added to the polymerization bottle, stirred at room temperature, after completely dissolving, cooled in an ice-water bath to below 5°C, and 406.0 grams (1.01 moles) were added 1,4-bis(3,4-dicarboxyphenoxy)phthalic anhydride (HQDA), stirred, reacted at 5°C for 1 hour, and obtained 2291.6 grams of homogeneous, transparent, viscous HQDA type polyamic acid resin solution, denoted as HQDA-PAA-1. Using Brookfield CAP2000+ vertebral plate viscometer, its viscosity at 50°C is measured as 1241mPa.s.

Embodiment 2

[0037] 175.2 grams (0.6 moles) of 1,4-bis(4-aminophenoxy)benzene (144BAPB), 10.8 grams (0.1 moles) of p-phenylenediamine (PPDA), 67.8 grams (0.3 moles) of 3,3'-bis Add methyl-4,4'-diaminodiphenylmethane (MDT), 2000 grams of N,N-dimethylacetamide (DMAc) and 700 grams of N-methyl-2-pyrrolidone (NMP) into the polymerization bottle, Stir at room temperature, after complete dissolution, cool in an ice-water bath to below 5°C, add 422.1 g (1.05 moles) of 1,4-bis(3,4-dicarboxyphenoxy)phthalic anhydride (HQDA), stir, 8°C After reacting for 3 hours, 3375.9 grams of homogeneous, transparent and viscous HQDA polyamic acid resin solution was obtained, which was designated as HQDA-PAA-2. Using Brookfield CAP2000+ vertebral plate viscometer, its viscosity at 50°C is measured as 1054mPa.s.

Embodiment 3

[0039] 140.0 grams (0.7 moles) of 4,4'-diaminodiphenyl ether (44ODA), 59.4 grams (0.3 moles) of 4,4'-diaminodiphenylmethane and 3800 grams of N-methyl-2-pyrrolidone (NMP ) into the polymerization bottle, stirred at room temperature, after completely dissolving, cooled in an ice-water bath to below 5°C, and added 434.1 g (1.08 moles) of 1,4-bis(3,4-dicarboxyphenoxy)phthalic anhydride (HQDA ), stirred, and reacted at 10°C for 6 hours to obtain 4433.5 grams of homogeneous, transparent, viscous HQDA polyamic acid resin solution, which was designated as HQDA-PAA-3. Using Brookfield CAP2000+ vertebral plate viscometer, the viscosity at 50°C was measured as 956mPa.s.

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Abstract

The invention relates to an HQDA type 14BDAPB branched polyimide resin film and a preparation method thereof. The mass ratio of 14BDAPB and HQDA type linear polyamide acid resin in raw materials of the film is 1 to 100-800. The preparation method comprises the steps that aromatic binary primary amine and a strong-polarity and non-proton organic solvent are mixed and stirred at room temperature, cooling is performed to reach 5 DEG C or below, HQDA is added, stirring is performed, reaction is performed at the temperature of 5-10 DEG C for 1-6 hours, and an HQDA type polyamide acid resin solution is obtained; the resin solution and the 14BDAPB are mixed at room temperature, stirring is performed, film formation, heating, dehydration and thermal imidization, cooling and mold release are performed to obtain the film. The method is mild in reaction condition, simple in operation, low in cost and environmentally friendly, facilitates industrial large-scale production and can be applied to the high-tech fields such as flexible solar cells, space telescopes, large motor major insulators, electromagnetic wire lapped electrical insulating materials and flexible copper-clad plates.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to a HQDA type 14BDAPB 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 launch the Next Gen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08G73/10C08J5/18
CPCC08G73/1071C08J5/18C08J2379/08C08L79/08
Inventor 虞鑫海周志伟
Owner DONGHUA UNIV
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