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
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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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