Thermoplastic polyimide resin with low thermal expansion coefficient and preparation method thereof
A technology of polyimide resin and low thermal expansion coefficient, which is applied in the field of thermoplastic polyimide resin with low thermal expansion coefficient and its preparation, can solve the problems of complex preparation process, solvent corrosion resistance, degradation of hydrolysis resistance, etc. Improve the effect of thermoplastic
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Embodiment 1
[0031] The preparation method (add catalyst) of low coefficient of thermal expansion thermoplastic polyimide resin is as follows:
[0032] Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then add trimethylchlorosilane (3.2592g, 30.0mmol), pyridine (2.1350g, 27.0mmol) and 4-dimethylaminopyridine (0.3665g, 3.0mmol), stir at room temperature for 15 minutes, then cool to 0 ℃, add isophthaloyl dichloride (4.0929, 20.16mmol) and 4,4-biphenyldianhydride (2.5420g, 8.64mmol), then add 25mL of N,N-dimethylacetamide, naturally warm to room temperature, Stir for 12 hours, then add phthalic anhydride (0.3554g, 2.4mmol) to cap, continue to react for 2 hours, then add a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and react at 80°C for 2 hours. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and...
Embodiment 2
[0034] The preparation method (do not add catalyst) of low coefficient of thermal expansion thermoplastic polyimide resin is as follows:
[0035]Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then cool to 0°C, add isophthaloyl dichloride (4.0929, 20.16mmol) and 4,4-biphenyldianhydride (2.5420g, 8.64mmol), add 25mL of N,N-dimethylethane Amide, naturally warmed to room temperature, stirred for 12 hours, then added phthalic anhydride (0.3554g, 2.4mmol) capping, continued to react for 2 hours, then added a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and reacted at 80°C for 2 hours. Hour. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and dry to obtain polyimide powder. See Table 1 for performance measurements.
Embodiment 3
[0037] Under the protection of nitrogen, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (9.6072g, 30.0mmol) and 25mL of N,N-dimethylacetamide to the reaction flask at room temperature Stir to dissolve, then add trimethylchlorosilane (3.2592g, 30.0mmol), pyridine (2.1350g, 27.0mmol) and 4-dimethylaminopyridine (0.3665g, 3.0mmol), stir at room temperature for 15 minutes, then cool to 0 ℃, add isophthaloyl dichloride (1.7542g, 8.64mmol) and 4,4-biphenyl dianhydride (5.9315g, 20.16mmol), add 25mL of N,N-dimethylacetamide, naturally warm to room temperature , stirred for 12 hours, then added phthalic anhydride (0.3554g, 2.4mmol) to block, continued the reaction for 2 hours, then added a mixture of acetic anhydride (120mmol) and pyridine (60mmol), and reacted at 80°C for 2 hours. Drop the reaction solution into ethanol to obtain fibrous polyimide precipitates, and dry to obtain polyimide powder. See Table 1 for performance measurements.
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