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Preparation method of colorless, transparent polyimide film containing norborene structure

A technology of polyimide film and norbornene is applied in the field of organic polymer materials, which can solve the problems of easy agglomeration and poor film transparency, and achieve the effects of excellent comprehensive performance, improved toughness, and improved toughness and strength.

Active Publication Date: 2018-06-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Invention patent CN 106916324A synthesized a norbornene dioic anhydride-maleimide based heptaphenyl polysilsesquioxane alternating copolymer, and used it as an acid anhydride monomer to prepare 4,4'-(hexafluoro Isopropylene) diphthalic anhydride-diaminodiphenyl ether (6FDA-ODA) type PI, the toughness of the film is greatly improved, the elongation at break is increased to 30.9%, and the dielectric constant is reduced to 2.2, but in the alternating copolymer The maleimide-based heptaphenyl polysilsesquioxane is easy to agglomerate, resulting in poor transparency of the film

Method used

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  • Preparation method of colorless, transparent polyimide film containing norborene structure
  • Preparation method of colorless, transparent polyimide film containing norborene structure
  • Preparation method of colorless, transparent polyimide film containing norborene structure

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Put a magnetic stirring bar into a glass reaction bottle with a stopcock, add 10mmol norbornene, 10mmol maleic anhydride and 15.0g tetrahydrofuran in sequence, stir evenly, then add 0.0329g AIBN, vacuumize, fill with nitrogen, and repeatedly discharge Air three times, airtight, put it in a constant temperature oil bath at 65°C, react for 24 hours, and end the reaction; pour the solution into about 50mL of anhydrous methanol, precipitate out, filter, and wash the solid product three times with methanol, and then in 80 Dry in a vacuum oven at ℃ for 24 hours to obtain a white powdery product, which is a norbornene-maleic anhydride binary copolymer, denoted as PNM1;

[0042] Take a small amount of this product and dissolve it in dimethyl sulfoxide deuterated reagent 1 H NMR test, the results are attached Figure 5 . In the spectrogram, within the scope of δ=0.8~1.8ppm, it is the chemical shift of the methylene proton peak on the norbornene, within the scope of δ=1.8~3...

Embodiment 2

[0047] (1) Put a magnetic stirring bar into a glass reaction bottle with a stopcock, add 5mmol norbornene, 10mmol maleic anhydride and 5.0g 1,4-dioxane in sequence, stir evenly, then add 0.0123g AIBN, and vacuumize , fill with nitrogen, repeatedly exhaust the air three times, seal it, put it in a constant temperature oil bath at 75°C, react for 12 hours, and end the reaction; pour the solution into about 25mL of anhydrous methanol to precipitate, filter, and the obtained solid product is washed with methanol Washed three times, and then dried in a vacuum oven at 140°C for 8 hours to obtain a white powdery product, which is a norbornene-maleic anhydride binary copolymer, denoted as PNM2, and the content of maleic anhydride in the product is calculated by elemental analysis results. The mole fraction is 0.54, the mole fraction of norbornene is 0.46, M n =4220, PDI=1.31, the average repeating unit is about 44;

[0048] (2) 0.10g prepared PNM2 and 1.2746g BPDA are mixed, and are ...

Embodiment 3

[0052] (1) Put a magnetic stirring bar into a glass reaction bottle with a stopcock, add 10mmol norbornene, 10mmol maleic anhydride and 18.0g benzene in sequence, stir evenly, then add 0.0987g AIBN, vacuumize, fill with nitrogen, and repeatedly discharge Air three times, airtight, put the reaction bottle into a constant temperature oil bath at 70°C, react for 16 hours, and end the reaction; pour the solution into about 50mL of anhydrous methanol to precipitate a precipitate, filter, and wash the obtained solid product with methanol three times, then Dry in a vacuum oven at 100°C for 12 hours to obtain a white powdery product, which is a norbornene-maleic anhydride binary copolymer, denoted as PNM3, and the mole fraction of maleic anhydride in the product is calculated by elemental analysis to be 0.53 , the mole fraction of norbornene is 0.47, M n =3780, PDI=1.48, the average number of repeating units is about 40;

[0053] (2) 0.20g prepared PNM3 and 1.2540g BPDA are mixed, an...

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Abstract

The invention discloses a preparation method of a colorless, transparent polyimide film containing norborene structure. The preparation method comprises the steps of firstly, preparing pasty diamine acetate suspension; then grinding and uniformly mixing norborene-maleic anhydride binary copolymer or N-substituted maleimide-norborene-maleic anhydride tercopolymer and 3,3',4,4'-biphenyl tetracarboxylic diandhydride, then adding the mixture into the prepared diamine acetate suspension once, reacting for 6-12h, so as to obtain a polyamic acid solution; uniformly spreading the polyamic acid solution onto clean glass, putting the glass in a vacuum drying oven, and removing bubbles; raising temperature and keeping the temperature according to a set procedure, cooling to room temperature, ultrasonic stripping, vacuum drying, so as to obtain the colorless, transparent polyimide film containing norborene structure. The preparation method keeps the original system colorless and transparent, remarkably improves the heat resistance, strength and toughness of the film, and can prepare the film with high comprehensive performance.

Description

technical field [0001] The invention relates to a method for preparing a high-performance polyimide (PI) film, in particular to a method for preparing a colorless and transparent polyimide film containing a norbornene structure, and belongs to the technical field of organic polymer materials. Background technique [0002] The all-aromatic PI film is brownish-yellow, and its visible light transmittance is low, which is difficult to meet the application requirements in the field of optoelectronics. Semi-aromatic PI and fully aliphatic PI are light or close to colorless, but the heat resistance of this type of PI is usually poor. Introducing rigid and highly conjugated substituents into the molecular chain can improve the heat resistance of the film, but It is usually unavoidable to reduce its optical transparency at the same time and vice versa, and its application in the field of electronics faces the problem of trade-offs between heat resistance, optical transparency, and ot...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08J5/18C08G73/10C08F222/06C08F232/08C08F222/40
CPCC08F222/06C08F232/08C08G73/1007C08G73/1082C08J5/18C08J2379/08C08F222/402
Inventor 赵建青张森刘述梅陈植耿黄皓浩
Owner SOUTH CHINA UNIV OF TECH
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