A kind of cross-linked colorless transparent high temperature resistant polyimide film material and preparation method thereof
A polyimide film, cross-linked technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve the problems of CPI film brittleness, affecting performance and application, etc.
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Embodiment 1
[0057] Example 1 Novel diamine monomer DFPTM.
[0058]
[0059] Vacuum, pass N 2 Three times to exhaust air and moisture. 3.3640g (11.60mmol) of 4,4'-diamino-4"-hydroxytriphenylmethane, 0.9768g (23.20mmol) of calcium hydride, 0.1762g (1.16mmol) of cesium fluoride and 2,3,4,5 , 2.7174 g (14.00 mmol) of 6-pentafluorostyrene, and then 52 mL of DMAc was added as a solvent. The mixture was placed under N 2 The mixture was heated to 80 °C with stirring in the dark and the reaction was maintained for 18 h. After the solution was cooled to room temperature, it was filtered through a G6 sand core funnel to remove inorganic solids, and then excess DMAc was removed by distillation under reduced pressure, and then purified using silica gel column chromatography (ethyl acetate / n-hexane, gradient elution) to obtain pale The yellow solid was finally recrystallized 3 times by the mixed solvent recrystallization method, that is, ethyl acetate was used as the good solvent to dissolve the ...
Embodiment 2
[0061] Example 2 Novel diamine monomer DFPTM.
[0062] Vacuum, pass N 2 Three times to exhaust air and moisture. 3.3640g (11.60mmol) of 4,4'-diamino-4"-hydroxytriphenylmethane, 1.4650g (34.8mmol) of calcium hydride, 1.0572g (6.96mmol) of cesium fluoride and 2,3,4,5 , 2.7174 g (14.00 mmol) of 6-pentafluorostyrene, and then 52 mL of DMAc was added as a solvent. The mixture was placed under N 2 The mixture was heated to 100 °C with stirring in the dark to reflux for 15 h. After the solution was cooled to room temperature, it was filtered through a G6 sand core funnel to remove inorganic solids, and then excess DMAc was removed by distillation under reduced pressure, and then purified using silica gel column chromatography (ethyl acetate / n-hexane, gradient elution) to obtain pale The yellow solid was finally recrystallized 3 times by the mixed solvent recrystallization method, that is, ethyl acetate was used as the good solvent to dissolve the light yellow solid obtained after ...
Embodiment 3
[0063] Example 3 Novel diamine monomer DFPTM.
[0064] Vacuum, pass N 2 Three times to exhaust air and moisture. 3.3640g (11.60mmol) of 4,4'-diamino-4"-hydroxytriphenylmethane, 1.2209g (29.00mmol) of calcium hydride, 0.4405g (2.90mmol) of cesium fluoride and 2,3,4,5 , 2.7174 g (14.00 mmol) of 6-pentafluorostyrene, and then 52 mL of DMAc was added as a solvent. The mixture was placed under N 2 The mixture was heated to 75°C with stirring in the dark to reflux for 24h. After the solution was cooled to room temperature, it was filtered through a G6 sand core funnel to remove inorganic solids, and then excess DMAc was removed by distillation under reduced pressure, and then purified using silica gel column chromatography (ethyl acetate / n-hexane, gradient elution) to obtain pale The yellow solid was finally recrystallized 3 times by the mixed solvent recrystallization method, that is, ethyl acetate was used as the good solvent to dissolve the light yellow solid obtained after pu...
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