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A kind of colorless transparent polyimide film and preparation method thereof

A transparent polyimide and film technology, which is applied in the field of heat-resistant polymer film preparation, can solve the problems of reduced mechanical properties, poor adhesion, and low mechanical strength of fluorine element films, and achieves excellent colorless and transparent properties, The effect of small thermal expansion coefficient and high mechanical strength

Active Publication Date: 2018-10-02
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, PI films are roughly divided into two categories: (1) Introducing fluorine-containing groups (such as fluorine substituents and trifluoromethyl substituents) into the polyimide structure can obtain colorless and transparent polyimide films, But at the same time, there are also certain defects, such as fluorine-containing monomers are generally expensive and the preparation process is very complicated; the introduction of fluorine will also lead to a decrease in the mechanical properties of the film, a decrease in thermal stability, poor adhesion, and affinity with other substrates. (2) The synthesis of colorless and transparent polyimide through alicyclic monomers will also bring a series of problems, and its mechanical strength is generally low, and its tensile strength is generally less than 100 MPa
The preparation of colorless and transparent polyimide films by the above two methods limits the application of such materials in high-performance flexible solar cell backplanes, flexible displays, and optical waveguide materials in the field of optical communications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a reactor equipped with a thermometer and mechanical stirring, 0.90 mol of 3,3'-bis(4-nitrophenoxy)benzidine and 0.09 mol of 3,4'-diaminodiphenyl ether were dissolved in N- Methylpyrrolidone, then lower the temperature to 10°C, add 0.90mol of 4,4'-bis(3,4-dicarboxyphenoxy)diphenyl ether dianhydride in 6 times within 2 hours, 0.10mol of Pyromellitic dianhydride, the solid content of the reactant is maintained at about 10%, after another 10 hours of reaction, the temperature of the reactor is raised to 40°C, and 0.025 mol of N,N'-dicyclohexylcarbodiimide is added, and then Stir for 5 h, then add ethanol, wash the precipitate, filter it with suction, and dry it under vacuum at 120° C. for 10 hours to obtain a colorless powder product. Dissolve the colorless powder in N-methylpyrrolidone to make a solution with a mass content of 7%, coat it on a clean and smooth glass plate, dry it in a vacuum oven at 100°C for 12 hours, and cool it down to room temperature to obtain a t...

Embodiment 2

[0023] In a reactor equipped with a thermometer and mechanical stirring, 0.90 mol of 3,3'-bis(4-nitrophenoxy)benzidine and 0.04 mol of 2,2-bis[4-(3-aminophenoxy Base) phenyl] propane 4,4'-diaminobiphenyl was dissolved in N,N-dimethylacetamide, then the temperature was lowered to 15°C, and 1.0 mol of 4 was added in 6 portions within 2 hours, 4'-bis(3,4-dicarboxyphenoxy)diphenyl ether dianhydride, the solid content of the reactant was maintained at about 15%, and after another 10 hours of reaction, the temperature of the reactor was raised to 40°C, and 0.035 mol of N,N'-dicyclohexylcarbodiimide was stirred for 5 hours, then ethanol was added, the precipitate was washed, filtered with suction, and vacuum-dried at 120°C for 10 hours to obtain a colorless powder product. Dissolve the colorless powder in N-methylpyrrolidone to prepare a solution with a mass content of 5%, coat it on a clean and smooth glass plate, dry it in a vacuum oven at 100°C for 12 hours, and cool it down to ro...

Embodiment 3

[0025] In a reactor equipped with a thermometer and mechanical stirring, 0.94 mol of 3,3'-bis(4-nitrophenoxy)benzidine was dissolved in N,N-dimethylformamide, and then the temperature was lowered to At 12°C, add 0.82 mol of 4,4'-bis(3,4-dicarboxyphenoxy)diphenyl ether dianhydride and 0.18 mol of 3,3',4,4'- Tetraformic acid biphenyl dianhydride, the solid content of the reactant is maintained at about 13%. After another 10 hours of reaction, the reaction kettle is heated to 40°C, and 0.030 mol of N,N'-dicyclohexylcarbodiimide is added, and stirred After 5 hours, ethanol was added, the precipitate was washed with water, filtered with suction, and dried under vacuum at 120° C. for 10 hours to obtain a colorless powder product. The colorless powder was dissolved in N-methylpyrrolidone to prepare a solution with a mass content of 6%, coated on a clean and smooth glass plate, dried in a vacuum oven at 100°C for 12 hours, and cooled to room temperature to obtain a film The average t...

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Abstract

The invention discloses a colorless transparent polyimide film and a preparation method thereof. The polyimide film is composed of a diamine monomer containing 3,3'-bis(4-nitrophenoxy) benzidine and a dianhydride monomer containing 4,4'-bis(3,4-dicarboxylphenoxy)benene dianhydride, wherein a molar fraction of the 3,3'-bis(4-nitrophenoxy) benzidine in the diamine monomer is not less than 90%; a molar fraction of 4,4'-bis(3,4-dicarboxylphenoxy)benene dianhydride in the dianhydride monomer is not less than 82%; a molar ratio of the diamine monomer to the dianhydride monomer is (0.94-0.99):1. According to the polyimide film prepared by the invention, monomers containing fluorine or aliphatic cycles are not used, and the obtained film has excellent colorless and transparent property, and is high in mechanical strength, small in coefficient of thermal expansion and excellent in heat resistance.

Description

technical field [0001] The invention relates to the field of preparation of heat-resistant polymer films, in particular to a colorless and transparent polyimide film and a preparation method thereof. Background technique [0002] At present, colorless and transparent polyimide film (PI film) is mainly obtained by introducing fluorine-containing groups or alicyclic groups into the polyimide molecular chain. Due to the introduction of fluorine atoms, the distance between the molecular chains of the fluorine-containing aromatic PI film is increased, which hinders the formation of intermolecular charge transfer complexes (CTC). The large electronic energy level band gap greatly improves the light transmittance of the material. The introduction of alicyclic groups can destroy the conjugated structure on the main chain of the molecule, and also make it difficult to form charge transfer complexes between molecular chains, which improves the transparency of alicyclic PI (Ren Xiaolo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1071C08J5/18C08J2379/08C08L79/08C08L2201/10C08L2203/16
Inventor 王雅婷徐勇李林霜吕珊珊
Owner NANJING UNIV OF SCI & TECH
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