A kind of high heat-resistant hyperbranched polyimide and its preparation method and application
A polyimide and thermal imidization technology, applied in the field of material science, can solve the problems of limited wide application, large inter-chain distance, decreased heat resistance, etc., achieve good application prospects, improve heat resistance, increase heat resistance, etc. The effect of a large free volume
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Embodiment 1
[0038] Add 0.4362g (2mmol) of pyromellitic dianhydride (PMDA) and 36ml of N,N-dimethylformamide into a three-necked flask, blow in argon, raise the temperature to 30°C, and add the triamine monomer N 4 ,N 4 -bis(4-aminophenyl)-[1,1'-biphenyl]-4,4'-diamine 0.3665g (1mmol) dissolved in 40ml N,N-dimethylformamide with constant pressure dropping funnel in 1~2h Evenly drop into a three-necked flask, then continue to react for 12 hours, then add 6ml of acetic anhydride and 2ml of triethylamine, heat up to 45°C and continue to react for 10 hours, after the reaction is completed, cool to room temperature and discharge in methanol, filter, wash, repeat 2~ 3 times, and finally placed in a vacuum drying oven at 80°C for 24 hours to obtain a yellow hyperbranched polyimide polymer, whose structural formula is as follows:
[0039]
Embodiment 2
[0041] Add 0.903g (4.14mmol) of pyromellitic dianhydride (PMDA) and 3ml of N,N-dimethylacetamide into a three-necked flask, blow in argon, raise the temperature to 30°C, and add the triamine monomer N 3 ,N 3 -bis(4-aminophenyl)-[1,1'-biphenyl]-3,4'-diamine 0.733g (2mmol) dissolved in 2ml N,N-dimethylacetamide with constant pressure dropping funnel in 1~2h Evenly drop into the three-necked flask, then continue to react for 15 hours, then add 12.4ml of acetic anhydride and 4.2ml of triethylamine, heat up to 45°C and continue to react for 12 hours, after the reaction is completed, cool to room temperature and discharge in ethanol, filter, wash, repeat 2 to 3 times, and finally placed in a vacuum drying oven at 80°C for 24 hours to obtain a brown hyperbranched polyimide polymer, whose structural formula is as follows:
[0042]
Embodiment 3
[0044] Add 0.4413g (1.5mmol) of 3,3',4,4'--biphenyltetracarboxylic dianhydride (BPDA) and 10ml of N-methylpyrrolidone into a three-necked flask, pass in argon, raise the temperature to 30°C, and Triamine Monomer N 2 ,N 2-bis(4-aminophenyl)-[1,1'-biphenyl]-2,4'-diamine 0.3665g (1mmol) dissolved in 8ml of N-methylpyrrolidone using a constant pressure dropping funnel in 1 ~ 2h evenly drop into three In the flask, continue to react for 24 hours, then add 12ml of acetic anhydride and 3ml of triethylamine, heat up to 45°C and continue to react for 10h, after the reaction is completed and cooled to room temperature, discharge the material in methanol, filter, wash, repeat 2 to 3 times, and finally Place it in a vacuum oven at 80°C and dry it for 24 hours to obtain a brown hyperbranched polyimide polymer, which has the following structural formula:
[0045]
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