A chemically bonded hydroxyethylidene diphosphonic acid medium-temperature organopolysiloxane phosphonic acid proton exchange membrane and its preparation method
A technology for compounding hydroxyethylidene diphosphonic acid and polysiloxane phosphonic acid groups, which can be used in electrochemical generators, solid electrolyte fuel cells, fuel cells, etc., and can solve the problem of low proton conductivity and restrictions on phosphonic acid content, etc. problem, achieve good proton conductivity, improve flexibility, excellent flexibility and mechanical strength
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Embodiment 1
[0039] A chemically bonded hydroxyethylidene diphosphonic acid medium-temperature organopolysiloxane phosphonic acid proton exchange membrane, which is prepared according to the following steps:
[0040] 1) Weigh the raw materials according to the mass ratio of hydroxyethylidene diphosphonic acid: dimethyl sulfoxide as 1:4; under the protection of nitrogen, slowly add hydroxyethylidene diphosphine into the three-necked flask with dimethyl sulfoxide acid, stir at room temperature until the solution is clear and transparent, heat the oil bath to 160°C and reflux for 0.5 hours; after the solution is cooled to 110°C, use an oil pump to distill off dimethyl sulfoxide under reduced pressure to obtain 1,1-vinyl diphosphonic acid liquid;
[0041] 2) According to the molar ratio of 1,1-vinyl diphosphonic acid: 3-(methacryloyloxy)propyltrimethoxysilane (DB-570): azobisisobutylcyanide: ethanol is 1:1 : 1×10 -3 : 10 Weigh the raw material, put it into the reactor, heat up to 60°C, and s...
Embodiment 2
[0045] A chemically bonded hydroxyethylidene diphosphonic acid medium-temperature organopolysiloxane phosphonic acid proton exchange membrane, which is prepared according to the following steps:
[0046] 1) Weigh the raw materials according to the mass ratio of hydroxyethylidene diphosphonic acid: dimethyl sulfoxide as 1:6; under the protection of nitrogen, slowly add hydroxyethylidene diphosphine into the three-necked flask with dimethyl sulfoxide acid, stir at room temperature until the solution is clear and transparent, heat the oil bath to 160°C and reflux for 1 hour; after the solution is cooled to 110°C, use an oil pump to distill off dimethyl sulfoxide under reduced pressure to obtain 1,1-vinyl diphosphonic acid liquid;
[0047] 2) According to the molar ratio of 1,1-vinyl diphosphonic acid: 3-(methacryloxy)propyltrimethoxysilane (DB-570): azobisisobutylcyanide: ethanol is 1:2 : 1×10 -3 : 10 Weigh the raw material, put it into the reactor, heat up to 60°C, and stir fo...
Embodiment 3
[0051] A chemically bonded hydroxyethylidene diphosphonic acid medium-temperature organopolysiloxane phosphonic acid proton exchange membrane, which is prepared according to the following steps:
[0052] 1) Weigh the raw materials according to the mass ratio of hydroxyethylidene diphosphonic acid: dimethyl sulfoxide as 1:8; under the protection of nitrogen, slowly add hydroxyethylidene diphosphine into the three-necked flask with dimethyl sulfoxide acid, stir at room temperature until the solution is clear and transparent, heat the oil bath to 160°C and reflux for 1.5 hours; after the solution is cooled to 110°C, use an oil pump to distill off dimethyl sulfoxide under reduced pressure to obtain 1,1-vinyl diphosphonic acid liquid;
[0053] 2) According to the molar ratio of 1,1-vinyl diphosphonic acid: 3-(methacryloyloxy)propyltrimethoxysilane (DB-570): azobisisobutylcyanide: ethanol is 1:3 : 1.5×10 -3 : 10 Weigh the raw material, put it into the reactor, heat up to 70°C, and...
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