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New type fluorine-containing copolyimide and preparation method thereof

A technology of thermal imidization of fluorine-containing copolymerized polyimide, which is applied in the field of new fluorine-containing copolymerized polyimide and its preparation, and can solve problems such as limited application and difficulty in product processing

Inactive Publication Date: 2010-09-15
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the large category of polyimides, the most typical representative is linear PI synthesized by pyromellitic anhydride and 4,4'-diaminodiphenyl ether. This type of PI has a large main chain rigidity. High heat resistance level, good mechanical properties at high and low temperature, but due to the rigid structure of the main chain, it does not melt or dissolve, which brings difficulties to product processing
Moreover, due to the easy formation of charge transfer complexes (CTC) within or between molecules, it often has a certain color, which also limits its application in the field of optics.

Method used

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  • New type fluorine-containing copolyimide and preparation method thereof
  • New type fluorine-containing copolyimide and preparation method thereof
  • New type fluorine-containing copolyimide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] First, in a three-necked reaction flask equipped with a stirrer, a thermometer and a nitrogen inlet, 2.1417 g (5 mmol) of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene was dissolved in 20.76 In mLDMF, add 1,2,3,4-cyclobutanetetracarboxylic dianhydride 0.4903g ​​(2.5mmol) and 1,2,3,4-cyclobutane-symmetric (3,6- Oxygen bridge-1,2,3,6-tetrahydrobenzene-1,2-dimethylformic anhydride) 0.8307g (2.5mmol), stir the above mixed solution under nitrogen atmosphere, react at 0~25℃ for 15~25h , Obtain a uniform and viscous polyamic acid (PAA) solution, the solid content of PAA by weight is 15wt%, and the intrinsic viscosity is 1.20dL / g. The PAA solution was coated on a clean glass plate, placed in a drying oven with nitrogen protection, and the temperature was raised according to the following program: 80°C 2hrs, 120°C 1hr, 150°C 1hr, 200°C 1hr, 250°C 1hr, 280°C 0.5hr. After the temperature dropped to room temperature, the glass plate was taken out and placed in warm water to re...

Embodiment 2

[0041] First, in a three-necked reaction flask equipped with a stirrer, a thermometer and a nitrogen inlet, 1.3011 g (2.5 mmol) of 4,4'-bis(4-amino-2 trifluoromethylphenoxy) diphenyl ether and 0.8006 g (2.5 mmol) of 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl were dissolved in 18.48 mL of DMF, and after it was completely dissolved, 1,2,3,4-cyclobutane was added Tetracarboxylic dianhydride 0.9806g (5mmol), stir the above mixed solution under a nitrogen atmosphere, react at 0-25°C for 15-25h to obtain a uniform and viscous polyamic acid (PAA) solution, the solid content of PAA by weight It is 15wt%, and the intrinsic viscosity is 1.25dL / g. The PAA solution was coated on a clean glass plate, placed in a drying oven with nitrogen protection, and the temperature was raised according to the following program: 80°C 2hrs, 120°C 1hr, 150°C 1hr, 200°C 1hr, 250°C 1hr, 280°C 0.5hr. After the temperature dropped to room temperature, the glass plate was taken out and placed in warm water...

Embodiment 3

[0045] First, in a three-necked reaction flask equipped with a stirrer, a thermometer and a nitrogen inlet, 2,2-bis[4-(4-amino-2trifluoromethylphenoxy)phenyl]hexafluoropropane 3.2723 g (5mmol) was dissolved in 28.94mLDMF, and after it was completely dissolved, 0.2242g (1mmol) of 1,2,4,5-cyclohexanetetracarboxylic dianhydride and 1,2,3,4-cyclobutane- Symmetrical (3,6-oxo-1,2,3,6-tetrahydrobenzene-1,2-dimethylformic anhydride) 1.3290g (4mmol), stir the above mixed solution under nitrogen atmosphere, at 0~25℃ The reaction was carried out for 15-25 hours to obtain a uniform and viscous polyamic acid (PAA) solution, the solid content of PAA by weight was 15wt%, and the intrinsic viscosity was 1.18dL / g. The PAA solution was coated on a clean glass plate, placed in a drying oven with nitrogen protection, and the temperature was raised according to the following program: 80°C 2hrs, 120°C 1hr, 150°C 1hr, 200°C 1hr, 250°C 1hr, 280°C 0.5hr. After the temperature dropped to room tempera...

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Abstract

The invention relates to new type fluorine-containing copolyimide and a preparation method thereof. The fluorine-containing copolyimide is obtained by condensation copolymerization of three monomers, i.e. the fluorine-containing copolyimide is prepared by the steps of carrying out condensation copolymerization reaction on one type of alicyclic dianhydride monomer and two types of fluorine-containing aromatic diamine monomers, or two types of the alicyclic dianhydride monomers and one type of the fluorine-containing aromatic diamine monomer in an aprotic polar solvent at low temperature, and then carrying out a thermal imidization reaction, and the new type fluorine-containing copolyimide has the advantages of high transparency, good heat resistance and the like. A fluorine-containing copolyimide film has a glass transition temperature of 200 DEG C to 350 DEG C, and is colorless and transparent; the ultraviolet absorption cutoff wavelength is between 270nm and 340 nm; the light transmittance at 450 nm is between 88% and 98%; and the fluorine-containing copolyimide film has good processing performance, and can be used as a bottom plate of a solar cell, a liquid crystal display material, a flexible transparent conductive film substrate material, an electromagnetic shielding material and the like.

Description

technical field [0001] The invention relates to a novel fluorine-containing copolymerized polyimide and a preparation method thereof, belonging to the preparation category of polymer materials in photoelectric devices. Background technique [0002] In the field of optoelectronics, polymer materials, especially colorless and transparent polymer materials, can be used in products such as photosensors, flexible displays, and solar cells. The requirements for polymer materials are mainly optical transparency, mechanical properties and heat resistance. At present, the colorless and transparent polymer materials that can be used in the field of optoelectronics include polyethylene terephthalate (PET), polycarbonate (PC), polypropylene (PP), polyimide (PI), poly Propylene diester (PPA), polytetrafluoroethylene (PTFE), etc. Among them, PET and PI have higher heat resistance grades. However, in the large category of polyimides, the most typical representative is linear PI synthesiz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18
Inventor 鲁云华胡知之王永飞房庆旭雷芃张志强肖国勇迟海军董岩赵洪斌李晓王翠苹
Owner UNIV OF SCI & TECH LIAONING
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