Preparation method of polyimide with fluorine-silicon modified main chain

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

Active Publication Date: 2016-02-10
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 2.31g (5mmol) 1H, 1H, 10H, 10H-perfluoro-1,10-decanediol, 5mL N, N-dimethylformamide in turn to a 10mL round bottom flask, then slowly add 1.74g (10mmol) toluene diisocyanate, stirred and reacted 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 1.55g (5mmol) 4,4'-oxydiphthalic anhydride (ODPA) and 15mLN, N-dimethylformamide successively in a 25mL two-necked round-bottomed flask that is dry and ventilated with nitrogen, and heat up to 60 ℃, then slowly add 5 mmol of freshly prepared perfluorodiol isocyanate dropwise, react in a nitrogen atmosphere for 4 hours, and obtain a colorless and transparent fluorine-containing polyimide solution.

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

[0025] Take 1 mmol of fluorine-containing polyimide s...

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 2.22g (5mmol) 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) and 15mLN,N-dimethylformamide successively in a 50mL two-necked round-bottomed flask that is dry and ventilated with nitrogen, and heat up to 70°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 fluorine-containing 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) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane under nitrogen atmosphere , then add 0.444g (1mmol) 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) and stir for 4h at room temperature, apply the prepa...

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Abstract

The invention discloses a preparation method of polyimide with a fluorine-silicon modified main chain. The preparation method sequentially comprises the following steps: (A) reacting perfluoroalkyl glycol with toluene diisocynate at room temperature for 8-16 hours, so as to obtain perfluoroalkyl glycol isocyanate; (B) sequentially dissolving perfluoroalkyl glycol isocyanate and aromatic dianhydride into an organic solvent, heating to 50-80 DEG C in the presence of nitrogen, and stirring for 4-6 hours, so as to obtain polyimide with a fluorine-containing main chain; and (C) sequentially adding silicon-containing diamine and aromatic dianhydride into a polyimide solution with the fluorine-containing main chain, reacting at the room temperature for 4-8 hours in the presence of nitrogen so as to obtain a prepolymer of polyimide with a main chain containing fluorine-silicon polyimide, coating, and baking, so as to obtain a polyimide material with the fluorine-silicon modified main chain. A fluorine-silicon modified polyimide membrane prepared by virtue of the preparation method has good hydrophobicity, translucency, film-forming property and adhesion property; furthermore, an operation method is simple and is applicable to industrial expansion.

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 high-transparency polyimides can be used in optical or opto-electrical fields, such as flexible solar radiation protection films, liquid crystal display alignment films and optical semi-waveguide materials. 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 and low...

Claims

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Application Information

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Patent Type & Authority Applications(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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