Preparation method for polyimide film
A polyimide film and imide technology, applied in the field of polymer materials, can solve problems such as poor light transmittance, and achieve the effects of good light transmittance, improved solubility, and increased distance
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[0026] The embodiment of the invention discloses a preparation method of a polyimide film, comprising the following steps:
[0027] A) mixing triphenylene ether tetracarboxylic dianhydride mixture and 2,2'-bistrifluoromethyl-4,4'-biphenylenediamine in an organic solvent to obtain a polyamic acid solution;
[0028] The triphenylene ether tetracarboxylic dianhydride mixture includes 2,3,3',4'-triphenylene ether tetracarboxylic dianhydride, 3,3',4,4'-triphenylene ether tetracarboxylic dianhydride and 2,2',3,3'-Triphenylene ether tetracarboxylic dianhydride;
[0029] B) the polyamic acid solution in the step A) is reacted under the action of a dehydrating agent and an imide catalyst to obtain a polyimide solution;
[0030] C) Casting the polyimide solution in the step B) into a film to obtain a polyimide film.
[0031] The present invention uses triphenylene ether tetracarboxylic dianhydride mixture and 2,2'-bistrifluoromethyl-4,4'-biphenylenediamine as raw materials, and the tr...
Embodiment 1
[0067] Add 109.5g of 3-chlorophthalic anhydride and 55.9g of aniline into 200ml of xylene, heat to reflux under the protection of nitrogen, azeotropically remove water for 5 hours, stop heating after no water evaporates, and when the temperature drops to room temperature, crude product. The crude product was filtered, washed three times with ethanol, and vacuum-dried at 80° C. to obtain 146.1 g of N-phenyl-3-chlorophthalimide with a yield of 94.5%.
[0068] Add 109.5g of 4-chlorophthalic anhydride and 55.9g of aniline into 200ml of xylene, heat to reflux under the protection of nitrogen, azeotropically remove water for 5 hours, stop heating after no water evaporates, and precipitate crude product. The crude product was filtered, washed three times with ethanol, and vacuum-dried at 80° C. to obtain 145.6 g of N-phenyl-4-chlorophthalimide with a yield of 94.2%.
[0069] Add 55.0g (0.50mol) of hydroquinone and 40g (1.0mol) of sodium hydroxide to a mixed solution of 400ml of N,N...
Embodiment 2
[0072] At room temperature, dissolve 6.4052 g of 2,2'-bistrifluoromethyl-4,4'-biphenylenediamine into 49 g of dimethylformamide, stir mechanically, and after it is completely dissolved, under stirring conditions Add 5.8845 g of the triphenylenediyl ether tetracarboxylic dianhydride mixture prepared in Example 1 therein. Stirring was continued for 24 hours to form a polyamic acid glue solution with a solid content of 20 wt%.
[0073] The obtained polyamic acid glue was left standing still for 24 hours. After the air bubbles were eliminated, it was cast on a clean glass plate and baked in an oven at 80° C. for 2 hours to cure the film. Move the glass plate coated with polyimide film into a high-temperature oven, heat the high-temperature oven from room temperature to 350 °C at a rate of 2 °C / min, turn off the high-temperature oven and let the temperature drop to room temperature naturally, and take out the coated glass plate from the oven. A glass plate with polyimide is placed...
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