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Intrinsic black polyimide as well as preparation method and application thereof

A technology of black polyimide and polyimide, applied in the field of material science, can solve the problems that polyimide has not been reported, and achieve the effect of improving visible light absorption capacity, excellent solubility, and simple preparation method

Inactive Publication Date: 2022-03-22
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the polyimide containing tetraphenyl cyclopentadienone structure has not been reported

Method used

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  • Intrinsic black polyimide as well as preparation method and application thereof
  • Intrinsic black polyimide as well as preparation method and application thereof
  • Intrinsic black polyimide as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a clean room, add 2.8666g (3.5mmol) 3,4-di([1,1'-biphenyl]-4-yl)-2,5-bis(4- (4-aminonaphthalen-1-yl)phenyl)cyclopenta-2,4-dienone and 18.4ml of dry N-methylpyrrolidone (NMP), stir to dissolve it, add 4,4'-(hexafluoroisopropene) Diphthalic anhydride (6FDA) 1.5548g (3.5mmol) with a solid content of about 18% was reacted at 0°C for 8h to obtain the corresponding PAA glue.

[0038] The imidization reagent was prepared at a volume ratio of NMP:acetic anhydride:isoquinoline=2:2:1, 6ml of the imidization reagent was added dropwise to the PAA glue, and the chemical imidization was carried out by stirring at room temperature for 1 hour. Squeeze the chemically imidized PI glue on a clean glass plate, and control the thickness of the liquid film by adjusting the effective height of the scraper. After heating up to 120°C in a high-temperature blast drying oven, keep the temperature for 1 hour to remove the solvent, then transfer to a vacuum drying oven to quickly raise the temp...

Embodiment 2

[0042] In a clean room, add 1.9025g (2mmol) 2,5-bis(4'-amino-[1,1'-biphenyl]-3-yl)-3,4-bis to a 50ml round bottom flask under nitrogen protection (4-(9,9-dimethyl-9H-fluoren-2-yl)phenyl)cyclopenta-2,4-dienone and 21.2ml of dry N,N-dimethylacetamide (DMAc), stirred to dissolve , then add 0.8885g (2mmol) of 6FDA, the solid content is about 13%, and react at -10°C for 48h to obtain the corresponding PAA glue.

[0043] The imidization reagent was prepared at a volume ratio of DMAc:acetic anhydride:pyridine=6:3:1, 5ml of the imidization reagent was added dropwise to the PAA glue, and the chemical imidization was carried out at 30°C for 1.5h. Squeegee-coat the chemically imidized PI glue on a clean glass plate, heat it up to 140°C in a blast drying oven, then keep the temperature constant for 0.8h to remove the solvent, then transfer it to a vacuum drying oven and quickly raise the temperature to 440°C, and keep the temperature constant After 10 minutes, the PI film was fully imidi...

Embodiment 3

[0047] In a clean room, add 2,5-bis(4”-amino-[1,1’:4’,1”-terphenyl]-4-yl)-3,4 to a 50ml round bottom flask under argon protection -bis(3-fluorophenyl)cyclopenta-2,4-dienone 3.0195g (4mmol) and 20ml of dry N,N-dimethylformamide (DMF), after stirring to dissolve, add 6FDA 1.7770g (4mmol), the solid content About 20%, reacted at 0°C for 8 hours to obtain the corresponding PAA glue.

[0048] The imidization reagent was prepared at a volume ratio of DMF:acetic anhydride:isoquinoline=6:3:1, and 6ml of the imidization reagent was added dropwise to the PAA glue solution, and the chemical imidization was carried out by stirring at 40°C for 2 hours. Scrape-coat the chemically imidized PI glue on a clean glass plate, heat it up to 80°C in a blast drying oven, then keep the temperature constant for 0.6h, and then keep the temperature at 160°C for 1h to remove the solvent, and then transfer it to a vacuum drying oven for rapid heating To 330°C, and keep the temperature for 30 minutes to f...

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Abstract

The invention discloses intrinsic black polyimide as well as a preparation method and application thereof. According to the intrinsic black polyimide, a diamine monomer and a tetracid dianhydride monomer which have large conjugation characteristics and contain a tetraphenyl cyclopentadienone structure are adopted as raw materials, polyamic acid is obtained through polymerization, and polyimide is obtained through imidization. The diamine monomer containing the tetraphenylcyclopentadienone structure and having the large conjugation characteristic has wide strong absorption in a visible light region, and when the diamine monomer is introduced into a polyimide molecular chain, polyimide can be endowed with excellent visible light absorption capacity, so that the intrinsic black characteristic is presented; such polyimides also have excellent solubility, heat resistance, electrical insulation properties and mechanical properties. The synthesis process is simple and is suitable for industrial production. The prepared intrinsic black polyimide has excellent visible light shielding performance, mechanical performance and electrical insulation performance, and can be widely applied to the fields of microelectronics, photoelectricity, military industry, aerospace and the like.

Description

technical field [0001] The invention relates to the field of material science, in particular to an intrinsic black polyimide and a preparation method thereof. Background technique [0002] Black polyimide (PI) film has good light-shielding, insulating, high-temperature stability and other properties, and is widely used in optics, electronics, aerospace and other fields. For satellite antennas, it can eliminate or avoid the interference of various stray lights on imaging systems and sensors, and maintain the normal working performance of the antenna; as a light-absorbing film, it can be used in optical fixed attenuators and optical terminal instruments; as a coated electronic component, it can be realized Photocopying method to form an image; as a circuit board cover film, it can be used to cover the circuit to prevent reverse engineering, and can avoid the deterioration of the circuit caused by long-term light radiation; as an optical application for headlights, camera flash...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1007C08G73/1067C08G73/1071C08G73/1039C08G73/1064C08J5/18C08J2379/08
Inventor 刘亦武谢丰云谭井华沈俊逸黄杰陈成亮周栋
Owner HUNAN UNIV OF TECH
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