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BTDA-type 14BDAPB 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: 2017-05-10
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 documents or patent reports about BTDA type 14BDAPB branched polyimide resin film and its preparation method

Method used

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  • BTDA-type 14BDAPB branched polyimide resin thin film and preparation method thereof
  • BTDA-type 14BDAPB branched polyimide resin thin film and preparation method thereof
  • BTDA-type 14BDAPB branched polyimide resin thin film and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] 160.0 grams (0.8 moles) of 4,4'-diaminodiphenyl ether (44ODA), 19.8 grams (0.1 moles) of 4,4'-diaminodiphenylmethane, 22.4 grams (0.1 moles) of 2-(4-amino Phenyl)-5-aminobenzimidazole (APABI) and 1600 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 added 325.2 Gram (1.01 mole) 3,3',4,4'-tetracarboxylic benzophenone dianhydride (BTDA), stirred, reacted at 5°C for 1 hour, and obtained 2127.4 grams of homogeneous, transparent, viscous BTDA type The polyamic acid resin solution is referred to as BTDA-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] 146.0 grams (0.5 moles) of 1,3-bis(4-aminophenoxy)benzene (134BAPB), 19.8 grams (0.1 moles) of 4,4'-diaminodiphenylmethane, 43.2 grams (0.4 moles) of p-benzene Add diamine (PPDA), 1000 grams of N,N-dimethylacetamide (DMAc) and 1180 grams 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 338.1 g (1.05 moles) of 3,3',4,4'-tetracarboxylic benzophenone dianhydride (BTDA), stir, and react at 8°C for 3 hours to obtain 2727.1 g of homogeneous, transparent , Viscous BTDA type polyamic acid resin solution, denoted as BTDA-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 3280 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 347.8 g (1.08 moles) of 3,3',4,4'-tetracarboxylic benzophenone dianhydride (BTDA), stir, and react at 10°C for 6 hours to obtain 3827.8 g of homogeneous, transparent , viscous BTDA type polyamic acid resin solution, denoted as BTDA-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 a BTDA-type 14BDAPB branched polyimide resin thin film and a preparation method thereof. In raw materials of the thin film, the mass ratio of 14BDAPB to the BTDA-type linear polyamide acid resin is 1:100-800. The preparation method includes the steps of: 1) mixing aromatic binary primary amine and a strong-polar non-protonic organic solvent, and stirring the mixture at room temperature, cooling the mixture to lower than 5 DEG C and adding the BTDA with stirring to carry out a reaction for 1-6 h at 5-10 DEG C to prepare a BTDA-type polyamide acid resin solution; and 2) mixing the resin solution and the 14BDAPB at room temperature, stirring the mixture to forming film, heating the mixture to perform dehydrating thermal imidization reaction, cooling the reaction product and releasing the film. The method has mild reaction conditions, is simple in operations, is low in cost and is environment-friendly, is beneficial to achievement of industrial large-scale production. The thin film can be applied in high-tech fields such as flexible solar cells, space telescope, major insulation of large motors, electrical insulating materials for lapping of electromagnetic wires, flexible copper-clad foil plates, etc.

Description

technical field [0001] The invention belongs to the field of polyimide film and its preparation, in particular to a BTDA 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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