HQDA-type fluorine-containing branched polyimide resin film and preparation method thereof

A technology of polyimide resin and polyamic acid resin, 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, there are no published documents or patent reports, The overall performance of film products is reduced and other problems, to achieve the effect of excellent dimensional stability, simple operation, and obvious comprehensive performance superiority.

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 is no published literature or patent report on the HQDA type fluorine-containing branched polyimide resin film and its preparation method.

Method used

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  • HQDA-type fluorine-containing branched polyimide resin film and preparation method thereof
  • HQDA-type fluorine-containing branched polyimide resin film and preparation method thereof
  • HQDA-type fluorine-containing branched polyimide resin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Combine 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 g of N-methyl-2-pyrrolidone (NMP) were added to the polymerization flask, stirred at room temperature, after complete dissolution, cooled in an ice water bath to below 5°C, added 406.0 g (1.01 mole) 1,4-Bis(3,4-dicarboxyphenoxy)phthalic anhydride (HQDA), stirred and reacted at 5°C for 1 hour to obtain 2291.6 grams of homogeneous, transparent and viscous HQDA polyamic acid resin The solution is denoted as HQDA-PAA-1. Using Brookfield CAP2000+ lamina viscometer, the viscosity at 50°C is 1241mPa.s.

Embodiment 2

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

Embodiment 3

[0039] Combine 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 ) Was added to the polymerization bottle, stirred at room temperature, after complete dissolution, cooled in an ice-water bath to below 5 ℃, added 434.1 g (1.08 mol) 1,4-bis(3,4-dicarboxyphenoxy)phthalic anhydride (HQDA ), stirring, and reacting at 10°C for 6 hours to obtain 4433.5 grams of a homogeneous, transparent and viscous HQDA-type polyamic acid resin solution, denoted as HQDA-PAA-3. Using Brookfield CAP2000+ lamina viscometer, its viscosity at 50℃ is 956mPa.s.

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Abstract

The invention relates to a HQDA-type fluorine-containing branched polyimide resin film and a preparation method thereof. The mass ratio of BDAPFP-type linear polyamide acid resin to HQDA-type linear polyamide acid resin in the raw materials of the film is 1: (100 to 800). The preparation method comprises the following steps: mixing aromatic primary diamine with a strongly-polar aprotic organic solvent, stirring at room temperature, cooling to a temperature of below 5 DEG C, adding HQDA, stirring, and reacting for 1-6h at 5-10 DEG C to obtain a HQDA-type polyamide acid resin solution; and mixing the resin solution with BDAPFP at room temperature, stirring, carrying out film formation, heating, carrying out a dehydration thermal-imidization reaction, cooling, and carrying out film release to obtain the product. The method disclosed by the invention is moderate in reaction condition, simple to operate, low in cost, environment-friendly, beneficial to realizing large-scale industrial production, and capable of being applied to the high-technology fields of flexible solar cells, space telescopes, large motor main insulation, electromagnetic wire-lapping electrical insulation materials, flexible copper-clad plates and the like.

Description

Technical field [0001] The invention belongs to the field of polyimide film and its preparation, and particularly relates to an HQDA type fluorine-containing branched polyimide resin film and a preparation method thereof. Background technique [0002] Polyimide film is a kind of polymer material with excellent comprehensive performance. It has particularly excellent heat resistance, low temperature resistance, flame resistance, electrical and mechanical properties. It is widely used in electronic microelectronics and printing High-tech fields such as circuit boards, wires and cables, main insulation of motors, shipping, aerospace, lasers, and optoelectronics. [0003] However, the traditional polyimide film, such as the KAPTON film produced by DUPONT in the United States and the domestic H film, their molecular structure is pyromellitic dianhydride type, that is, the main monomer raw material is pyromellitic dianhydride. Anhydride and 4,4'-diaminodiphenyl ether. [0004] NASA plans...

Claims

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Application Information

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