Side-chain sulfonic acid type polyarylether, preparation method thereof and application of polyarylether in preparation of proton exchange membrane
A technology of polyarylether and chain sulfonic acid, which is applied in the field of polymer functional materials, can solve the problems of polymers losing mechanical properties, polymer swelling rate is serious, and polymer phase separation is not obvious enough, etc.
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[0023] Example 1: Preparation of 4-(3-(4-(2,6-difluorobenzoyl)phenoxy)propoxy)benzenesulfonate sodium difluorosulfonated monomer
[0024] Put 4-(2,6'-difluorophenylcarbonyl) diphenylpropyl ether (10g) into 30mL, 95~98% concentrated sulfuric acid solution at 50℃, stir for 4h; then discharge into 100ml Use 1mol / l sodium hydroxide solution to neutralize to ph=7 in the ice water, and filter to obtain a white solid. After recrystallization, 4-(3-(4-(2,6-difluorobenzoyl)phenoxy)propoxy)benzenesulfonate sodium difluorosulfonated monomer is obtained, and the yield is 40%. FT-IR(KBr: 1 034cm -1 (-SO 3 Na), 1 660cm -1 (C=O), 1257cm -1 (C-O-C). 1 H NMR (300MHz, DMSO) δ 7.78 (d, J = 8.4 Hz, 2H), 7.65 (d, J = 7.1 Hz, 1H), 7.52 (d, J = 8.3 Hz, 2H), 7.30 (t, J = 8.1 Hz, 2H), 7.14 (d, J = 8.7 Hz, 2H), 6.88 (d, J = 8.5 Hz, 2H), 4.26 (t, J = 5.9 Hz, 2H), 4.14 (t, J = 5.7 Hz, 2H), 2.41-1.98 (m, 2H).
Example Embodiment
[0025] Example 2: Preparation of polymer PAEK-1
[0026] In a three-necked flask equipped with a stirrer, a water device and a nitrogen port, add 10mmol of 4,4'-dihydroxydiphenyl ether, 7.36mmol of 4-(3-(4-(2,6-difluoro Benzoyl) phenoxy) propoxy) benzene sulfonate, 2.64mmol of 4,4'-difluorobenzophenone, 11mmol of anhydrous potassium carbonate, 40ml of sulfolane and 8ml of toluene into the above three-necked flask In the middle, nitrogen gas was added and the temperature was raised to 120°C. Reflux with water for 2 hours, evaporate the dehydrating agent, heat up to 175℃ and react for 6 hours, then pour the reaction mixture into water to obtain the polymer, then use a pulverizer to pulverize into particles of about 10 mesh, and then filter with a Buchner funnel for more After washing with deionized water, washing with ethanol and vacuum drying at 100°C for 12 hours, the polymer PAEK-1 was obtained, with a yield of over 90%. Its sulfonation degree is 0.74, and its glass transition...
Example Embodiment
[0027] Example 3: Preparation of polymer PAEK-2
[0028] In a three-necked flask equipped with a stirrer, a water device and a nitrogen port, add 10 mmol of 4,4'-dihydroxydiphenyl ether and 8.1 mmol of 4-(3-(4-(2,6-difluoro Benzoyl)phenoxy)propoxy)benzenesulfonate, 1.9mmol of 4,4'-difluorobenzophenone, 11mmol of anhydrous potassium carbonate, 45ml of sulfolane and 9ml of toluene into the above three-necked flask In the middle, nitrogen gas was added and the temperature was raised to 120°C. Reflux with water for 2 hours, evaporate the dehydrating agent, heat up to 175℃ and react for 6 hours, then pour the reaction mixture into water to obtain the polymer, then use a pulverizer to pulverize into particles of about 10 mesh, and then filter with a Buchner funnel for more After washing with deionized water, washing with ethanol and vacuum drying at 100°C for 12 hours, the polymer PAEK-2 was obtained with a yield of over 90%. Its sulfonation degree is 0.81, and its glass transition t...
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