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ODPA-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film and its preparation, can solve the problem of difficult preparation of high molecular weight polyimide resin, unpublished literature or patent reports, Problems such as the decline in comprehensive performance of film products, to achieve excellent dimensional stability, simple operation, and significant 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 are no published literature or patent reports about the ODPA type fluorine-containing branched polyimide resin film and its preparation method.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 180.0 grams (0.9 moles) of 3,4'-diaminodiphenyl ether (34ODA), 22.4 (0.1 moles) of 2-(4-aminophenyl)-5-aminobenzimidazole (APABI) and 1550 grams of N- Add methyl-2-pyrrolidone (NMP) into the polymerization bottle, stir at room temperature, after it is completely dissolved, cool in an ice-water bath to below 5°C, add 313.1 g (1.01 moles) of 3,3',4,4'-tetracarboxylic acid Diphenyl ether dianhydride (ODPA), stirred, reacted at 5° C. for 1 hour, and obtained 2065.5 grams of homogeneous, transparent, viscous ODPA type polyamic acid resin solution, which was recorded as ODPA-PAA-1. The Brookfield CAP2000+ vertebral plate viscometer was used to measure the viscosity, and the performance data are shown in Table 1.

Embodiment 2

[0037] 262.8 grams (0.9 moles) of 1,3-bis(4-aminophenoxy)benzene (134BAPB), 10.8 grams (0.1 moles) of p-phenylenediamine (PPDA), 1000 grams of N,N-dimethylacetamide ( DMAc) and 1,400 grams of N-methyl-2-pyrrolidone (NMP) were added to the polymerization bottle, stirred at room temperature, and after they were completely dissolved, cooled in an ice-water bath to below 5°C, and 325.5 grams (1.05 moles) of 3,3',4 , 4'-tetracarboxylic acid diphenyl ether dianhydride (ODPA), stirred, reacted at 8°C for 3 hours, obtained 2999.1 grams of homogeneous, transparent, viscous ODPA polyamic acid resin solution, recorded as ODPA-PAA -2. The Brookfield CAP2000+ vertebral plate viscometer was used to measure the viscosity, and the performance data are shown in Table 1.

Embodiment 3

[0039] Add 200.0 g (1.0 mole) of 4,4'-diaminodiphenyl ether (DADPE) and 3200 g of N-methyl-2-pyrrolidone (NMP) into the polymerization bottle, stir at room temperature, and cool in an ice-water bath after completely dissolving To below 5°C, add 334.8 g (1.08 moles) of 3,3',4,4'-tetracarboxylic diphenyl ether dianhydride (ODPA), stir, and react at 10°C for 6 hours to obtain 3734.8 g of homogeneous, transparent , viscous ODPA type polyamic acid resin solution, denoted as ODPA-PAA-3. The Brookfield CAP2000+ vertebral plate viscometer was used to measure the viscosity, and the performance data are shown in Table 1.

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Abstract

The invention relates to an ODPA-type fluorine-containing branched polyimide resin film and a preparation method thereof. The mass ratio of BDAPFP and ODPA-type linear polyamide acids resins in the raw materials of the film is 1:100-800. The preparation method comprises the following steps: aromatic dicarboxylic primary amine and an aprotic organic solvent having strong polarity are mixed, a mixture is stirred under room temperature and then is cooled to the temperature of below 5 DEG C, ODPA is added and stirred, then is reacted for 1-6 hours at the temperature of 5-10 DEG C to obtain an ODPA-type polyamide acid resin solution; the resin solution and BDAPFP are mixed at room temperature, the mixture is stirred and is subjected to film forming, the material is heated, then is subjected to dehydration and thermal imidization, and the material is cooled and demoulded to obtain the product. The method has the advantages of mild condition, simple operation, low cost, and environment friendliness, is in favor of realizing industrial scale production, and can be used in the field of high technology such as flexible solar energy cells, space telescopes, large generator winding insulation, insulated wire lapping 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 an ODPA 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
CPCC08L79/08C08G73/1071C08J5/18C08J2379/08C08L2201/08C08L2203/16
Inventor 虞鑫海吴冯周志伟
Owner DONGHUA UNIV
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