6FDA-type fluorine-containing 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 of difficulty in preparing high-molecular-weight polyimide resin, the decline of comprehensive performance of film products, and the cost of film products. Advanced problems, to achieve the effect of excellent dimensional stability, significant comprehensive performance superiority, excellent electrical performance and optical performance

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 6FDA type fluorine-containing branched polyimide resin film and its preparation method

Method used

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  • 6FDA-type fluorine-containing branched polyimide resin film and preparation method thereof
  • 6FDA-type fluorine-containing branched polyimide resin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 20.0 grams (0.1 moles) of 3,4'-diaminodiphenyl ether (34ODA), 160.0 grams (0.8 moles) of 4,4'-diaminodiphenyl ether (44ODA), 22.4 (0.1 moles) of 2-(4 -Aminophenyl)-5-aminobenzimidazole (APABI) and 1960 grams of N-methyl-2-pyrrolidone (NMP) were added to the polymerization bottle, stirred at room temperature, and after completely dissolving, the ice-water bath was cooled to below 5°C, Add 448.4 grams (1.01 moles) of 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6FDA), stir, and react at 5°C for 1 hour to obtain 2610.8 grams of homogeneous, transparent, viscous The 6FDA type polyamic acid resin solution is denoted as 6FDA-PAA-1. Using Brookfield CAP2000+ vertebral plate viscometer, its viscosity at 50°C was measured as 997mPa.s.

Embodiment 2

[0037] 175.2 grams (0.6 moles) of 1,3-bis(4-aminophenoxy)benzene (134BAPB), 43.2 grams (0.4 moles) of p-phenylenediamine (PPDA), 2000 grams of N,N-dimethylacetamide ( DMAc) and 740 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 466.2 grams (1.05 moles) of 2,2-bis( 3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6FDA), stirred, and reacted at 8°C for 3 hours to obtain 3424.6 grams of homogeneous, transparent, viscous 6FDA type polyamic acid resin solution, denoted as 6FDA -PAA-2. Using Brookfield CAP2000+ disc viscometer, the viscosity at 50°C is 864mPa.s.

Embodiment 3

[0039] 180.0 grams (0.9 moles) of 4,4'-diaminodiphenyl ether (44ODA), 19.8 grams (0.1 moles) of 4,4'-diaminodiphenylmethane and 4000 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 479.5 grams (1.08 moles) of 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride ( 6FDA), stirred, and reacted at 10° C. for 6 hours to obtain 4679.3 grams of homogeneous, transparent, viscous 6FDA type polyamic acid resin solution, which was designated as 6FDA-PAA-3. Using Brookfield CAP2000+ vertebral plate viscometer, the viscosity at 50°C was measured as 587mPa.s.

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Abstract

The invention relates to a 6FDA-type fluorine-containing branched polyimide resin film and a preparation method thereof. In the raw materials of the film, the mass ratio of BDAPFP to 6FDA-type linear polyamide acid resin is 1:(100-800). The preparation method comprises the following steps: mixing eldest aromatic binary amine with a strong-polar aprotic organic solvent, stirring at room temperature, and cooling to a temperature below 5 DEG C; adding 6FDA, stirring, and reacting for 1-6 hours at 5-10 DEG C to obtain a 6FDA-type fluorine-containing branched polyimide resin solution; and mixing the resin solution with BDAPFP at room temperature, stirring, forming a film, heating and increasing the temperature, performing dehydration and thermal imidization reaction, cooling and removing the mold. The method has the advantages of mild reaction conditions, simple operation, low cost and environmental friendliness, is favorable for implementing industrial large-scale production, and can be applied to high-tech fields, including flexible solar cells, space telescopes, large generator main insulation materials, electromagnetic wire lapped 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, in particular to a 6FDA type fluorine-containing 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 ...

Claims

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Application Information

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