Polyimide adhesive and preparation method thereof
A technology of polyimide adhesives and adhesives, which is applied in the direction of adhesives, etc., can solve the problems of decreased adhesive performance, heat-resistant instability of polyimide adhesives, etc., to achieve glass transition temperature increase, lower melting The effect of improving the bulk viscosity and improving the adhesive performance
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[0058] Example 1
[0059] (1) In a three-necked flask equipped with mechanical stirring, water trap, nitrogen inlet and outlet and thermometer, add 28.82g (0.09mol) 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, 3.49g (0.01mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 110g of N-methylpyrrolidone were stirred under nitrogen protection until completely dissolved. Then, 16.11 g (0.05 mol) of 3,3’,4,4’-benzophenone tetracarboxylic dianhydride and 24.82 g (0.10 mol) of 4-phenylethynyl phthalic anhydride were added, and stirred under a nitrogen atmosphere until completely dissolved. Stir at room temperature for 12 hours to obtain a homogeneous solution with a solid content of 40 wt.%.
[0060] (2) 16 grams of toluene was added to the above homogeneous solution, the reaction system was heated to 175°C, reacted for 12 hours under nitrogen protection, and then heated to 200°C to distill off the toluene and stop heating.
[0061] (3) Cool the reaction solution to 100°C, pour it into et...
Example Embodiment
[0065] Example 2
[0066] (1) In a three-necked flask equipped with mechanical stirring, water trap, nitrogen inlet and outlet and thermometer, add 25.62g (0.08mol) 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, 6.97g (0.02mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 215g of N,N-dimethylacetamide were stirred under nitrogen protection until completely dissolved. Then, 19.33g (0.06mol) of 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 19.86g (0.08mol) of 4-phenylethynylphthalic anhydride were added, and stirred under nitrogen atmosphere until completely dissolved. Stir at room temperature for 12 hours to obtain a homogeneous solution with a solid content of 25 wt.%.
[0067] (2) 11 g of xylene was added to the above homogeneous solution, the reaction system was heated to 150°C, reacted for 12 hours under nitrogen protection, and then heated to 166°C to distill out xylene and stop heating.
[0068] (3) Cool the reaction solution to 80°C, pour it into methanol to obtain ...
Example Embodiment
[0072] Example 3
[0073] (1) In a three-necked flask equipped with mechanical stirring, water trap, nitrogen inlet and outlet and thermometer, add 22.42 g (0.07 mol) 4,4'-diamino-2,2'-bistrifluoromethyl biphenyl, 10.46g (0.03mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 165g of N,N-dimethylformamide were stirred under nitrogen protection until completely dissolved. Then 21.49g (0.067mol) of 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 16.56g (0.067mol) of 4-phenylethynylphthalic anhydride were added, and stirred under nitrogen atmosphere until completely dissolved. Stir at room temperature for 8 hours to obtain a homogeneous solution with a solid content of 30 wt.%.
[0074] (2) Add 8 grams of toluene to the above homogeneous solution, the reaction system is heated to 140° C., reacted for 12 hours under nitrogen protection, and then heated to 153° C. to distill toluene and stop heating.
[0075] (3) Cool the reaction solution to 120°C, pour it into propanol to obta...
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