A kind of thermosetting polyimide and its application
A technology of polyimide and thermosetting, applied in the field of thermosetting polyimide, can solve the problems of thermosetting polyimide, low mechanical properties, and far difference, etc., and achieve good reprocessing characteristics and strong mechanical properties , good recyclable effect
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Embodiment 1
[0031] 1. Add 4,4'-diaminodiphenyl ether (33.15 mmol) into a 250 mL three-neck flask, add 100 mL of N,N-dimethylacetamide, add 2,3' in portions after dissolving, 3',4-biphenyltetracarboxylic dianhydride (30 mmol) was stirred at room temperature under nitrogen atmosphere for 24 h to obtain a polyamic acid solution with a certain viscosity.
[0032] 2. Measure toluene (10 mL) and add it to the prepared polyamic acid solution, heat reflux at 180°C in a dry nitrogen atmosphere for 24 hours, then pour it into industrial ethanol solution to precipitate precipitates, wash, suction filter, and heat at 150°C Dry in an oven for 36 hours to obtain polyimide oligomers.
[0033] 3. First, mix paraformaldehyde (1.25mmol) and deionized water (0.2 mL) into N, N-dimethylacetamide (4 mL), stir at 80 ℃ under a dry nitrogen atmosphere for 30 min until dissolved complete, that is, paraformaldehyde solution; secondly, mix polyimide oligomer (0.5 mmol) and N,N-dimethylacetamide (10 mL) at room temp...
Embodiment 2
[0041] 1,2,3,4,5 are carried out with the method of example 1.
[0042] 6. Configure H 2 SO 4 (16mol / L) solution and NaHCO 3 (24 mol / L) solution, soak the final thermosetting polyimide (0.2 g) in 100 mL H 2 SO 4 In the solution for 1 h, after it was completely decomposed, NaHCO was added dropwise 3 The solution was neutralized (PH=7, detected by test paper), filtered and washed to obtain a light yellow precipitate.
[0043] Carry out performance characterization analysis with the method of example 1.
Embodiment 3
[0045] 1. Add 4,4'-diaminodiphenyl ether (48mmol) and 3,4'-diaminodiphenyl ether (42mmol) into a 250 mL three-necked flask, add 100 mL N-methylpyrrolidone, and wait to dissolve Then, 2,3',3',4-biphenyltetracarboxylic dianhydride (30 mmol) was added in portions, and stirred at room temperature under nitrogen atmosphere for 12 h to obtain a polyamic acid solution with a certain viscosity.
[0046] 2. Measure toluene (10 mL) and add it to the prepared polyamic acid solution, heat reflux at 180°C in a dry nitrogen atmosphere for 36 hours, then pour it into industrial ethanol solution to precipitate precipitates, wash, suction filter, and heat at 150°C Dry in an oven for 24 h to obtain polyimide oligomers.
[0047] 3. First, mix paraformaldehyde (1.35mmol) and deionized water (0.05 mL) into N-methylpyrrolidone (6 mL), and stir at 80 ℃ for 30 min under a dry nitrogen atmosphere until it is completely dissolved, that is, paraformaldehyde solution; secondly, polyimide oligomer (0.5 m...
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