A kind of preparation method of main chain fluorine silicon modified polyimide

A polyimide and fluorosilicon modification technology is applied in the preparation field of main chain fluorosilicon modified polyimide, which can solve the problem of low hygroscopicity, low surface energy and poor adhesion of fluorine-containing polyimide. and other problems, to achieve the effect of excellent light transmittance and simple operation

Active Publication Date: 2017-08-25
甘肃中安瑞科科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although fluorine-containing polyimide has good low moisture absorption, due to its low surface energy, it has poor ductility with other materials and shows poor adhesion to various substrates

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of perfluorodiol isocyanate

[0021] Add 2.31 g (5 mmol) 1H, 1H, 10H, 10H-perfluoro-1,10-decanediol, 5 mL of N,N-dimethylformamide to a 10 mL round bottom flask successively, and then slowly drop Add 1.74g (10mmol) of toluene diisocyanate, stir and react at room temperature for 12h to obtain a colorless and transparent perfluorodiol isocyanate solution.

[0022] (2) Preparation of fluorine-containing polyimide (F-ODPA)

[0023] Add 1.55 g (5 mmol) 4,4'-oxydiphthalic anhydride (ODPA) and 15 mL of N, N-dimethylformamide successively to a 25 mL two-necked round-bottomed flask that is dry and ventilated with nitrogen, and heat up to 60°C, then slowly add 5 mmol of freshly prepared perfluorodiol isocyanate dropwise, and react in a nitrogen atmosphere for 4 hours to obtain a colorless and transparent fluorinated polyimide solution.

[0024] (3) Preparation of main chain fluorine silicon modified polyimide (F-Si-ODPA) film

[0025] Take 1 mmol of fluorine-co...

Embodiment 2

[0027] (1) The preparation of perfluorodiol isocyanate is the same as in Example 1.

[0028] (2) Preparation of fluorine-containing polyimide (F-6FDA)

[0029] Add 2.22 g (5 mmol) of 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) and 15 mL of N,N-dimethylformamide to a 50 mL two-necked round-bottomed flask that is dry and ventilated with nitrogen , the temperature was raised to 70°C, and then 5 mmol of newly prepared perfluorodiol isocyanate was slowly added dropwise, and reacted for 4 hours in a nitrogen atmosphere to obtain a colorless and transparent fluorinated polyimide solution.

[0030] (3) Preparation of main chain fluorine silicon modified polyimide (F-Si-6FDA) film

[0031] Take 1 mmol of fluorine-containing polyimide solution, slowly add 0.248 g (1 mmol) 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane under nitrogen atmosphere Alkanes, then add 0.444g (1mmol) 4,4'- (hexafluoroisopropylene) diphthalic anhydride (6FDA) and stir for 4h at room tempera...

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Abstract

The invention discloses a preparation method of main chain fluorine silicon modified polyimide. The steps of the method are as follows: A. react perfluoroalkyl diol with toluene diisocyanate at room temperature for 8-16 hours to obtain perfluorinated polyimide Diol isocyanate; B Dissolve perfluorodiol isocyanate and aromatic tetraacid dianhydride in an organic solvent in sequence, heat to 50‑80°C and stir for 4~6 h under a nitrogen atmosphere to obtain a polyimide containing fluorine in the main chain. Amine; C. Add silicon-containing diamine and aromatic tetra-acid dianhydride to the polyimide solution containing fluorine in the main chain in sequence, and react at room temperature for 4~8 h under nitrogen atmosphere to obtain the fluorine-containing silicon polyimide in the main chain. The prepolymer of the coating film is baked to obtain the main chain fluorosilicon modified polyimide material. The fluorine-silicon modified polyimide film prepared by the method of the invention has good water repellency, light transmittance, film-forming property and adhesion performance, and the operation method of the invention is simple, and is suitable for industrial scale-up.

Description

technical field [0001] The invention relates to a preparation method of main chain fluorine silicon modified polyimide. Background technique [0002] Polyimide, known as the most promising engineering plastic in this century, has excellent thermal stability, mechanical properties and electrical properties, and has been widely used in aviation, aerospace and microelectronics industries. Especially light-colored or even colorless polyimide with high transparency can be used in optical or optoelectronic fields, such as flexible solar radiation protection film, liquid crystal display alignment film and optical semi-waveguide materials, etc. However, the lack of hygroscopic expansion of traditional polyimides leading to hydrolysis also limits its application in cutting-edge fields such as aerospace and precision electronics. One of the solutions is fluorinated polyimide with high heat resistance and low moisture absorption. Fluorinated polyimide has low electronic polarization a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 周峰叶谦王晓龙
Owner 甘肃中安瑞科科技有限公司
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