Transparent polyimide and preparation method thereof

A polyimide resin, polyamic acid technology, applied in the direction of organic chemistry, etc., can solve the problems of inability to large-scale application, hinder the conjugation of electron clouds, high price, etc., achieve low cost, improve transparent performance, transparency high effect

Active Publication Date: 2013-02-06
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the colorless and transparent polyimide film material LaRC developed by NASA TM -CP1 and LaRC TM -CP2 uses hexafluorodianhydride (6FDA), see US patents US 4603061 and US 4595548, but the price of this dianhydride monomer is expensive
[0007] (3) The use of large side groups or asymmetric structural units hinders the conjugation of electron clouds and inhibits the formation of charge transfer complexes. However, the synthesis of such monomers is difficult and cannot be applied on a large scale.

Method used

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  • Transparent polyimide and preparation method thereof
  • Transparent polyimide and preparation method thereof
  • Transparent polyimide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Embodiment 1: the preparation of 1,4-bis(3,4-dicarboxylic acid phenoxy group) cyclohexane dianhydride:

[0058] Under nitrogen protection, add 9.2g (60% solid content, mass percent, 230mmol) of sodium hydride into a 500mL three-necked flask, then add 100mL of N,N-dimethylformamide, and stir at room temperature for 2 hours. Then dropwise add 11.6g (100mmol) of 1,4-cyclohexanediol cis-trans mixture and 100mL of N, N-dimethylformamide mixed solution, after stirring at room temperature for 1 hour, add 36.4g (210mmol) of The mixed solution of 4-nitrophthalonitrile and 100mL of N,N-dimethylformamide was stirred at room temperature for 24 hours, the reaction solution was poured into water, a precipitate was precipitated, filtered, washed with ethanol, and dried to obtain cis Crude product of back-mixed 1,4-bis(3,4-dicyanophenoxy)cyclohexane.

[0059] The above-mentioned crude product was heated to reflux in 200mL of acetonitrile solution, filtered, and dried to obtain 19.3 g ...

Embodiment 2

[0066] In this embodiment, the transparent polyimide resin material has the following structural formula:

[0067]

[0068] The specific preparation method is: under the protection of nitrogen, mix 1.2481g (4.0mmol) of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl and 16ml of N,N-dimethylethane Add the amide into a 50mL reaction flask, stir at room temperature, and after 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl is completely dissolved, add 1.6343g (4.0mmol) of trans 1, 4-bis(3,4-dicarboxylic acid phenoxy group) cyclohexane dianhydride, continued to stir at room temperature for 24 hours to obtain a viscous polyamic acid solution, and then the solution was diluted to a concentration of 10% by weight ( Based on the sum of the mass of raw material dianhydride and diamine, the same below).

[0069]The diluted polyamic acid solution is uniformly coated on a clean glass plate, the thickness of the solution coating film is 0.5mm, the glass plate is placed in a drying oven, ...

Embodiment 3

[0072] In this embodiment, the transparent polyimide resin material has the following structural formula:

[0073]

[0074] The specific preparation method is: under the protection of nitrogen, mix 1.2483g (4.0mmol) of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl and 16ml of N,N-dimethylethane Add the amide into a 50mL reaction flask, stir at room temperature, and then add 1.6351g (4.0mmol) of cis-1 after the 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl is completely dissolved. 4-bis(3,4-dicarboxylic acid phenoxy)cyclohexanedianhydride was stirred at room temperature for 24 hours to obtain a viscous polyamic acid solution, and then the solution was diluted to a concentration of 10% by weight.

[0075] The diluted polyamic acid solution is uniformly coated on a clean glass plate, the thickness of the solution coating film is 0.5mm, the glass plate is placed in a drying oven, and the temperature is raised according to the following procedure: 80°C, 1 hour; 150°C , 1 hour...

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Abstract

The invention discloses a transparent polyimide material. The transparent polyimide material is obtained by performing condensation polymerization on a 1,4-bi(3,4-dicarboxylic phenoxy)cyclohexane dianhydride monomer and a binary primary amine monomer. Because the dianhydride monomer is in an alicyclic structure, the formation of a charge transfer complex in polyimide molecules and between molecules can be effectively suppressed, and the transparent performance of the polymer is greatly improved; and meanwhile, according to the phthalic anhydride structures at two ends, the high reactivity of the dianhydride is kept. The glass transition temperature of the polyimide film is 200 to 300 DEG C, the ultraviolet absorption cutoff wavelength is 340 to 380nm, the light transmissivity at 450nm is 70 to 90 percent, and the transparent polyimide material has good application prospect in the fields of flexible substrate materials of solar cells, flexible transparent conductive film substrate materials, liquid crystal display materials and the like. The invention also discloses a dianhydride monomer which can be used for preparing the transparent polyimide resin material.

Description

technical field [0001] The invention relates to the field of polyimide and its preparation, in particular to a transparent polyimide and its preparation method. Background technique [0002] Polyimide is the most important variety of aromatic heterocyclic polymers developed in the past half century, and it is also a type of polymer material with the highest service temperature. It has high mechanical strength, high temperature resistance, chemical stability, and creep resistance. With excellent comprehensive performance, it has been widely used in aviation, aerospace, electrical, mechanical, microelectronics, chemical industry and other fields. [0003] Recently, with the development of high-tech industries, the demand for high heat-resistant and high-transmittance polyimide in optical fields such as light guides, waveguides and liquid crystal displays is becoming more and more urgent, because polyimide with high temperature resistance and high light transmission Colorless ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C07D307/89
Inventor 陈国飞郭俊超方省众
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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