Coumarin-based photocyclized crosslinked sulfonated polyimide proton exchange membrane and preparation method thereof
A technology of sulfonated polyimide and proton exchange membrane, which is applied in the field of functional polymer materials and electrochemistry, and can solve the problem of low proton conductivity, reduced application potential of sulfonated polyimide, dimensional stability, and decreased mechanical strength problems such as high proton conductivity, good dimensional stability, and mild process conditions
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Embodiment 1
[0044] Step (1): Synthesis of sulfonated polyimides containing hydroxyl groups with a sulfonation degree of 80%:
[0045] Weigh 0.6957g (4mmol) of 2,2-'benzidine disulfonic acid (BDSA) into a 250mL three-neck flask, add 20mL of m-cresol and 1.67mL (12mmol) of triethylamine. The right end of the three-necked flask is fed with nitrogen gas through a curved pipe, the left end is connected with a reflux condenser, and then passed through a drying pipe into a conical flask filled with water for testing the nitrogen flow rate, and the middle port is connected with a mechanical stirring device. The rotation speed was adjusted to 100r / min, and the temperature was raised to 80°C. After about 30 minutes, BDSA dissolved to obtain a yellow transparent liquid, which was naturally cooled to room temperature. Weigh 2.7936g (10mmol) 1,4,5,8-naphthalene tetracarboxylic dianhydride (NTDA), 2.9898g (6mmol) 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (6FAP ), 2.4547g (20mmol) of benzoic a...
Embodiment 2
[0055] Step (1): Synthesis of a hydroxyl-containing sulfonated polyimide with a sulfonation degree of 100%:
[0056] Weigh 0.6957g (5mmol) BDSA into a 250mL three-neck flask, add 20mL m-cresol and 1.67mL (12mmol) triethylamine. The right end of the three-necked flask is fed with nitrogen gas through a curved pipe, the left end is connected with a reflux condenser, and then passed through a drying pipe into a conical flask filled with water for testing the nitrogen flow rate, and the middle port is connected with a mechanical stirring device. The rotation speed was adjusted to 100r / min, and the temperature was raised to 80°C. After about 30 minutes, BDSA dissolved to obtain a yellow transparent liquid, which was naturally cooled to room temperature. Weigh 2.7936g (10mmol) NTDA, 2.9898g (5mmol) 6FAP, and 2.4547g (20mmol) benzoic acid, add them to the three-necked flask in turn, add 25mL of m-cresol to make the solid content between 16% and 17%, and stir for 30min. Raise the te...
Embodiment 3
[0066] Step (1): Synthesis of sulfonated polyimide containing hydroxyl groups with a sulfonation degree of 120%:
[0067] Weigh 0.6957g (6mmol) BDSA into a 250mL three-neck flask, add 20mL m-cresol and 1.67mL (12mmol) triethylamine. The right end of the three-necked flask is fed with nitrogen gas through a curved pipe, the left end is connected with a reflux condenser, and then passed through a drying pipe into a conical flask filled with water for testing the nitrogen flow rate, and the middle port is connected with a mechanical stirring device. The rotation speed was adjusted to 100r / min, and the temperature was raised to 80°C. After about 30 minutes, BDSA dissolved to obtain a yellow transparent liquid, which was naturally cooled to room temperature. Weigh 2.7936g (10mmol) of NTDA, 2.9898g (4mmol) of 6FAP, and 2.4547g (20mmol) of benzoic acid, add them to the three-necked flask in turn, add 25mL of m-cresol to make the solid content between 16% and 17%, and stir for 30min....
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