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A kind of fully aromatic colorless transparent polyimide film and preparation method thereof

A technology of transparent polyimide and polyimide film, which is applied in the field of all-aromatic colorless and transparent polyimide film and its preparation, and can solve the problems of difficulty in obtaining uniform materials, unfavorable film forming performance, and molecular chain Problems such as fracture, to achieve the effect of retaining solubility and transparency, avoiding cross-linking reaction and darkening of color, and low order

Active Publication Date: 2021-03-23
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these patents use monomers containing alicyclic structures, which have poor thermal stability
In addition, many high-temperature thermal imidization processes are used in the preparation process, resulting in high energy consumption. At the same time, problems such as molecular chain breakage, recombination, and equilibrium will occur during the high-temperature thermal imidization process, which is not easy to obtain. Uniform material, detrimental to film formability

Method used

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  • A kind of fully aromatic colorless transparent polyimide film and preparation method thereof
  • A kind of fully aromatic colorless transparent polyimide film and preparation method thereof
  • A kind of fully aromatic colorless transparent polyimide film and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Under nitrogen protection and a reaction temperature of 20°C, first dissolve 4.28g of diamine 1,4-bis(2-trifluoromethyl-4-aminophenoxy)benzene (6FAPB) in 18g of N-methylpyrrolidine In the ketone, after the diamine is completely dissolved, add 3.1g 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA) and the remaining organic solvent, so that the solid content of the solution is 20%, After stirring and reacting for 24 hours, the resulting polyamic acid solution was added dropwise with 2.04 g of acetic anhydride and 2.02 g of triethylamine, and the reaction was continued for 8 hours at 30 ° C. Finally, the obtained solution was washed with excess distilled water, and the obtained product Put it in a vacuum oven at 100° C. and fully dry it to finally obtain 6.99 g of thermoplastic polyimide material with a yield of 94.7%. Finally, the polyimide film can be prepared by dissolving, coating and volatilizing the synthesized polyimide material.

[0030] figure 1 Show...

Embodiment 2

[0035] Under nitrogen protection and a reaction temperature of 0°C, firstly, 4.28g of diamine 1,4-bis(2-trifluoromethyl-4-aminophenoxy)benzene (6FAPB) was dissolved in 18g of N-methylpyrrolidine In the ketone, after the diamine is completely dissolved, add 3.1g 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA) and the remaining organic solvent, so that the solid content of the solution is 20%, After stirring and reacting for 24 hours, the resulting polyamic acid solution was added dropwise with 3.06 g of acetic anhydride and 3.03 g of triethylamine, and the reaction was continued for 12 hours at 60°C. Finally, the obtained solution was washed with excess distilled water, and the obtained product Put it in a vacuum oven at 100° C. and fully dry it to finally obtain 7.02 g of thermoplastic polyimide material with a yield of 95.1%. Finally, the polyimide film can be prepared by dissolving, coating and volatilizing the synthesized polyimide material.

Embodiment 3

[0037] Under nitrogen protection and a reaction temperature of 0°C, first dissolve 4.28g of diamine 1,4-bis(2-trifluoromethyl-4-aminophenoxy)benzene (6FAPB) in 35g of N,N-dimethyl In acetamide (DMAc), after the diamine is completely dissolved, add 3.1g of 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA) and the remaining organic solvent, so that the solid content of the solution 10%, stirred and reacted for 48 hours to form a polyamic acid solution, then added 3.06 g of acetic anhydride and 3.03 g of triethylamine dropwise, continued the reaction for 12 hours at 30 ° C, and finally washed the obtained solution with excess distilled water, while The obtained product was fully dried in a vacuum oven at 100° C. to finally obtain 6.87 g of thermoplastic polyimide material with a yield of 93.1%. Finally, the polyimide film can be prepared by dissolving, coating and volatilizing the synthesized polyimide material.

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Abstract

The invention relates to a wholly aromatic colorless and transparent polyimide thin film and a preparation method thereof. The preparation method comprises the following steps: taking diamine monomer1,4-bis(2-3-trifluoromethyl-aminophenoxy)benzene with trifluoromethyl side group and middle ether bond connection as a raw material, carrying out polymerization reaction on the raw material and isomeric 2,3,3',4'-diphenyl ether tetracarboxylic acid dianhydride which contains an ether bond in the middle; then synthesizing a thermoplastic polyimide material by adopting a chemical imidization method;dissolving, coating a film and volatilizing a solvent to prepare the polyimide thin film. Compared with the prior art, the wholly aromatic colorless and transparent polyimide thin film prepared by the preparation method has high optical transparency and thermal stability, and has a very good application potential in the fields including high-transparency flexible device substrates and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer films, in particular to a fully aromatic colorless and transparent polyimide film and a preparation method thereof. Background technique [0002] Polyimide (PI) refers to a class of high-performance polymers containing imide rings on the main chain. The unique aromatic ring structure makes polyimide materials have the advantages of high temperature resistance, solvent resistance, dimensional stability, good electrical insulation and excellent mechanical properties. It can be used in films, fibers, coatings, gas separation membranes, advanced Composite materials, molded parts, and adhesives are widely used in high-tech fields such as mechanical engineering, microelectronics, petrochemicals, and aerospace. Although polyimide has excellent overall performance, it also has some defects. The highly rigid and conjugated aromatic heterocyclic structure in its molecular chain will make polyimide very dif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J5/18
CPCC08G73/1007C08G73/1071C08J5/18C08J2379/08
Inventor 宇平王巍薛敏钊刘燕刚
Owner SHANGHAI JIAOTONG UNIV
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