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Colorless and transparent polyimide film and preparation method thereof

A technology of transparent polyimide and polyimide film, applied in the field of polymer materials, can solve problems such as reducing heat resistance, achieve high glass transition temperature and thermal decomposition temperature, reduce intermolecular interactions, improve Effects of Transparency and Heat Resistance

Active Publication Date: 2014-05-14
HANGZHOU FIRST APPLIED MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] From the above review, it can be seen that the introduction of alicyclic dianhydride groups into the molecular structure of polyimide can greatly improve the optical transmittance and solubility of the film, but compared with the traditional aromatic polyimide, its resistance Reduced thermal performance

Method used

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  • Colorless and transparent polyimide film and preparation method thereof
  • Colorless and transparent polyimide film and preparation method thereof
  • Colorless and transparent polyimide film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] At room temperature, add 4.1634g (8mmol) 4,4'-bis(4-amino-2-trifluoromethylphenoxy)diphenyl ether into 37.30ml DMAc, nitrogen protection, mechanical stirring, until it is completely Dissolve and add 2.0016g (8mmol) bicyclo[3,3,0]octane-2,4,6,7-tetraacid dianhydride, continue to stir, and react for 24 hours under the protection of nitrogen to obtain a colorless, transparent, viscous, Polyamic acid solution (PAA) with a solid content of 15%. Place the obtained PAA solution in a vacuum oven with a relative vacuum of 0.08MPa to remove air bubbles at room temperature for 2 hours. After the air bubbles are removed, apply a film on a glass plate with a smooth surface, and the glass after coating The plate was first dried at 70°C for 2 hours, raised to 300°C at a rate of 5°C / min, and kept for 1 hour, and then naturally cooled to room temperature. The cooled glass plate was deionized in deionized water to obtain a colorless Transparent polyimide film, sampled by gel permeation ...

Embodiment 2

[0043] At room temperature, 5.2356g (8mmol) of 2,2'-bis[4-(4-amino-2-trifluoromethylphenoxy)phenyl]hexafluoropropane was added to 43.79ml of DMAc under nitrogen protection, Stir mechanically, until it is completely dissolved, add 2.0016g (8mmol) bicyclo[3,3,0]octane-2,4,6,7-tetraacid dianhydride, continue to stir, and react for 24 hours under nitrogen protection to obtain a colorless , Transparent, viscous, polyamic acid solution (PAA) with a solid content of 15%. Add 0.90 g of acetic anhydride and 1.33 g of pyridine to the obtained PAA solution, stir for 30 minutes under nitrogen protection, then increase the reaction temperature to 120 ° C, continue the reaction for 24 hours under nitrogen protection, and pour the resulting reaction solution into 5 times the volume of ethanol , precipitated, filtered, collected, washed with ethanol and dried to obtain polyimide resin (PI resin). Weigh 2g of polyimide resin and dissolve it in 12.10ml of DMAc to obtain a PI solution with a so...

Embodiment 3

[0045] At room temperature, 4.1634g (8mmol) of 4,4'-bis(4-amino-2-trifluoromethylphenoxy)diphenyl ether was added to 37.98ml of DMAc, nitrogen protection, mechanical stirring, until it was completely Dissolve and add 2.1138g (8mmol) of bicyclo[4,3,0]nonane-3,4,7,9-tetraacid dianhydride, continue to stir, and react for 24 hours under nitrogen protection to obtain a colorless, transparent, viscous, A polyamic acid solution (PAA) with a solid content of 15%, followed by the same operation in Example 1 to obtain a colorless and transparent polyimide film, and the weight average molecular weight detected by sampling gel permeation chromatography (GPC) was 3.5×10 4 . The main properties of the film are shown in Table 1 and Table 2.

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Abstract

The invention discloses a colorless and transparent polyimide film, the molecular structural formula as shown in a formula I. A preparation method of the polyimide film comprises the following steps: polymerizing a fluorine-containing diamine monomer and a dianhydride monomer which have same moles in a polar aprotic solvent to produce a colorless and transparent poly(amicacid) solution, carrying out dehydration and ring closing on the colorless and transparent poly(amicacid) solution by using a hot imidization method or a chemical imidization method to produce the colorless and transparent polyimide film, wherein the dianhydride monomer is one or two of compounds selected from bicyclic (3,3,0)octane-2,4,6,7-tetracid dihydride or bicyclic (4,3,0)nonane-3,4,7,9-tetracid dihydride, the fluorine-containing diamine monomer is one or a combination of two of compounds selected from 4,4'-di(4-amino-2-trifluoromethylphenoxy)diphenyl ether, 4,4'-di(4-amino-2- trifluoromethylphenoxy) biphenyl and 2,2'-di(4-(4-amino-2- trifluoromethylphenoxy) phenyl) hexafluoropropane. The colorless and transparent polyimide film produced by using the alicyclic type dianhydride monomer has excellent performances such as good heat resistance, good solubility and high light transmittance.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a colorless and transparent polyimide film and a preparation method thereof. Background technique [0002] Colorless and transparent polyimide film has excellent properties such as good heat resistance, low thermal expansion coefficient and high light transmittance, and can replace glass as a transparent substrate for flexible displays and thin-film solar cells. However, the heat resistance of other transparent polymer materials, such as polyethylene terephthalate, polycarbonate, polyacrylate, polyethersulfone, etc., cannot meet the process requirements. [0003] Traditional aromatic polyimide films have a high density of aromatic rings and are prone to form charge transfer complexes (CTCs), making them appear yellow-brown, which limits their applications in the field of optoelectronics. Moreover, due to the high rigidity of the molecular chain of the traditional aromatic polyimid...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08G73/10C08J5/18
CPCC08G73/1007C08J5/18C08J2379/08C08L79/08
Inventor 李奇琳周慧周光大林建华
Owner HANGZHOU FIRST APPLIED MATERIAL CO LTD
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