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Polyimide precursor, polyimide film and preparation method thereof, and display device

A technology of polyimide precursor and polyimide film, which is applied in the direction of identification devices, instruments, etc., can solve the problems of poor interface compatibility between silicon dioxide and polyimide, transparency, thermal performance and mechanical performance attenuation , reduce the quality of polyimide film and other problems, and achieve the effects of easy long-term storage, inhibition of charge transfer complexation, and excellent interfacial binding force

Active Publication Date: 2021-03-30
武汉柔显科技股份有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Especially in the field of optoelectronics, as one of the most promising materials for the cover or substrate of a new generation of mobile phones, it is necessary to maintain high heat resistance while maintaining high transparency of polyimide films. The role of internal and intermolecular charge transfer complexes, the color is generally light yellow or brownish yellow, which limits its application in this field. Some scholars have realized the synthesis of silicon dioxide and polyimide by introducing nano-silica materials. Complementary properties, a polyimide film with high heat resistance and high transparency has been prepared
[0003] In the preparation of nano-silica / polyimide composite materials, it is actually a condensed state structure in which silica is dispersed in the polyimide matrix, and the two phases are phase-separated microscopically, thus forming a high-performance composite material There are still two major technical difficulties: 1) the particle size of nano-silica is small, it is easy to agglomerate, and it is not easy to disperse in the polyimide matrix; 2) the current preparation method of the composite material uses nano-silica doped to poly In the amic acid slurry, the subsequent high-temperature drying process can easily lead to poor interfacial compatibility between silica and polyimide
[0004] Under the combined effect of the above two unfavorable factors, the nano-silica / polyimide composite film has the problems of transparency, thermal properties and mechanical properties attenuation, which greatly reduces the quality of the polyimide film.

Method used

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  • Polyimide precursor, polyimide film and preparation method thereof, and display device
  • Polyimide precursor, polyimide film and preparation method thereof, and display device
  • Polyimide precursor, polyimide film and preparation method thereof, and display device

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[0044]

[0045] As mentioned above, the polyimide precursor of the present invention comprises polyimide prepolymer and hydrophilic nano silicon dioxide, and described polyimide prepolymer is made of dianhydride and diamine in ionic liquid obtained by polymerization.

[0046] The present invention does not specifically limit the preparation of the polyimide prepolymer, which can be prepared by methods known to those skilled in the art, such as polymerization of dianhydride and diamine. The upper limit of the reaction temperature in the polymerization is preferably 220°C, more preferably 200°C. On the other hand, the lower limit of the reaction temperature is preferably 150°C, more preferably 180°C. The upper limit of the reaction time in the polymerization is preferably 24 h, more preferably 20 h. On the other hand, the lower limit of the reaction time is preferably 10 h, more preferably 12 h.

[0047] In a preferred version of the present invention, the preparation metho...

Embodiment 1

[0065] (1) Under nitrogen protection, 10g 4,4'-diaminodiphenyl ether and 0.018g 4,4'-diaminodiphenyl ether-2,2'-disulfonic acid were added to 90.18g ionic liquid 1- In butyl-3-methylimidazolium bromide, stir at 25°C until completely dissolved to obtain a diamine solution;

[0066] (2) Add 11.45g of pyromellitic dianhydride to the diamine solution in five times, the amount of dianhydride added each time is 50% of the remaining dianhydride amount, and the interval between each addition is 30min. After complete addition, the temperature is raised to 180°C for reaction After 10 hours, cool down to room temperature to obtain a polyimide prepolymer solution;

[0067] (3) Disperse hydrophilic silicon dioxide into 10g ionic liquid 1-butyl-3-methylimidazolium bromide to obtain a silicon dioxide solution with a content of 20wt%, and then slowly add it dropwise to the polyimide Continue to react in the prepolymer solution for 8 hours. After the reaction is complete, add a large amount o...

Embodiment 2

[0070] (1) Under nitrogen protection, 10g 2,2'-bis(trifluoromethyl)diaminobiphenyl and 0.011g 4,4'-diaminodiphenyl ether-2,2'-disulfonic acid were added to 580.66g of ionic liquid 1,3-bis(2-methoxy-2-oxyethyl)imidazolium hexafluorophosphate was stirred at 50°C until completely dissolved to obtain a diamine solution;

[0071] (2) Add 13.89g of 2,2'-bis(3,4-dicarboxylic acid)hexafluoropropane dianhydride in four times, and the amount of dianhydride added each time is 50% of the remaining amount of dianhydride until it is completely added , the interval between each addition is 60 minutes, after complete addition, the temperature is raised to 200 ° C for 24 hours, and the temperature is lowered to room temperature to obtain a polyimide prepolymer solution;

[0072](3) dispersing hydrophilic silicon dioxide into 20 g of ionic liquid 1,3-bis(2-methoxy-2-oxyethyl) imidazole hexafluorophosphate to obtain a silicon dioxide solution with a content of 20 wt%, Then slowly drop it into t...

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Abstract

The invention provides a polyimide precursor, a polyimide film, a preparation method of the polyimide film and a display device; the polyimide precursor is synthesized in ionic liquid by using sulfonated diamine, dianhydride and hydrophilic nano silicon dioxide, and the polyimide film containing nano silicon dioxide is prepared by using the polyimide precursor. The polyimide film has good mechanical properties and heat resistance, the 1% thermal weight loss temperature is 430-540 DEG C, the glass transition temperature is 330-480 DEG C, the tensile strength is 220-450 MPa, the transmittance at400 nm is 60-86%, and an effective solution is provided for the defects of polyimide as a transparent substrate or a transparent cover plate at the present stage.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a polyimide precursor, a polyimide film, a preparation method thereof, and a display device. Background technique [0002] As a special engineering plastic with imide ring and rigid chain structure in the main chain, polyimide has excellent mechanical properties, heat resistance, flame retardancy, solvent resistance, radiation resistance and electrical properties, and is widely used In a series of high-tech fields such as aerospace, optoelectronics, and automobiles. Especially in the field of optoelectronics, as one of the most promising materials for the cover or substrate of a new generation of mobile phones, it is necessary to maintain high heat resistance while maintaining high transparency of polyimide films. However, due to the presence of molecular The role of internal and intermolecular charge transfer complexes, the color is generally light yellow or brownish ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08K3/36C08L79/08G09F9/30
CPCC08G73/1071C08G73/1078C08G73/1039C08G73/1067C08G73/1075C08G73/1007C08J5/18C08K3/36G09F9/301C08J2379/08Y02P20/54
Inventor 付华肖桂林阮敏鲁丽平朱双全
Owner 武汉柔显科技股份有限公司
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