Branching block-type polymer used for proton exchange membrane, preparation method and application
A technology of proton exchange membrane and block type, which is applied in the field of branched block type polymers and its preparation, and can solve the problems that proton conductivity and mechanical properties cannot be balanced.
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[0056] The present invention also provides a preferred embodiment of the preparation method of the branched block polymer of formula (I), including the following:
[0057] Step A1. In a protective atmosphere, add 3,3'-diaminobenzidine, 1,3,5-tris(4-carboxyphenyl)benzene and 1,4-phthalic acid to the temperature of 130-150℃. In polyphosphoric acid (PPA), the temperature is kept and stirred for 1.5-2.5h, then the temperature is raised to 165-175°C for prepolymerization for 20-60min, and then the temperature is raised to 210-230°C for 40min-1.5h to obtain the intermediate product (Brp-PBI- Am);
[0058] Step B1. Cool the reacted mixture in the step A1 to 130-150°C, and then add 3,3'-diaminobenzidine and 2,2-bis(4-carboxyphenyl)hexafluoropropane in sequence, Incubate and stir for 1.5-2.5h, then heat to 210-230℃ for 3-5h;
[0059] Step C1: Cool the reacted mixture in the step B1 to 20-40°C, then use saturated sodium bicarbonate solution to soak, filter, and wash the precipitate to obtain...
Embodiment 1
[0071] Example 1 Synthesis of polymer of formula (I) (branched poly(p-phenylene bibenzimidazole) block fluorine-containing polybenzimidazole)
[0072] (1) Install a 100 mL three-necked flask with a condenser on the magnetic stirrer, and place the flask in an oil bath.
[0073] (2) Add 45 g of polyphosphoric acid to a three-necked flask in a nitrogen atmosphere, raise the temperature to 140 °C, and keep it for 2 hours until the magneton runs smoothly at high speed.
[0074] (3) Add 0.4543 g 3,3'-diaminobenzidine (2.12 mmol), 0.1052g 1,3,5-tris(4-carboxyphenyl)benzene (0.24 mmol) and 0.2725 g 1 to the three-necked flask in turn , 4-phthalic acid (1.64 mmol), the molar ratio of the three is 53:6:41.
[0075] (4) Stir at 140 °C for 2 h, then heat to 170 °C for prepolymerization for 0.5 h, and then react at 220 °C for 1 h to obtain the intermediate product Brp-PBI-Am.
[0076] (5) Cool the reacted mixture to 140 °C, and then add 0.4285 g 3,3'-diaminobenzidine (2 mmol) and 0.8316 g 2,2-bis(4...
Embodiment 2
[0080] Example 2 Synthesis of polymer of formula (II) (branched fluorine-containing polybenzimidazole block poly(p-phenylene bibenzimidazole))
[0081] (1) and (2) The steps are the same as in Example 1.
[0082] (3) Add 0.4285 g of 3,3'-diaminobenzidine (2 mmol) and 0.3522 g of 1,4-phthalic acid (2.12 mmol) into a three-necked flask successively, and the molar ratio of the two is 1:1.06.
[0083] (4) The steps are the same as in Example 1, to obtain the intermediate product p-PBI-Ac.
[0084] (5) Cool the reacted mixture to 140 °C, and then add 0.4543 g 3,3'-diaminobenzidine (2.12 mmol) and 0.1052 g 1,3,5-tris(4-carboxybenzene) to a three-necked flask. Benzene (0.24 mmol) and 0.6433 g of 2,2-bis(4-carboxyphenyl)hexafluoropropane (1.64 mmol), the molar ratio of the three is 53:6:41.
[0085] (6), (7), (8) The steps are the same as in Example 1, and finally a branched fluorine-containing polybenzimidazole block poly(p-phenylene bibenzimidazole) polymer (BrF6-PBI-bp-PBI) The yield is 91...
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