A kind of phosphonated polyolefin grafted benzimidazole polymer proton exchange membrane and its preparation method and application
A technology of olefin polymers and benzimidazoles, which is applied in the field of phosphonated polyolefin grafted benzimidazole polymer proton exchange membranes and its preparation, which can solve the problems of mechanical property decline, phosphoric acid loss, and proton conductivity reduction, etc. problems, to achieve the effect of promoting migration, improving proton conductivity, and high proton conductivity retention
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[0101]
[0102] The present invention also provides a kind of preparation method of above-mentioned graft copolymer, it comprises the steps:
[0103] (1) Mixing the olefinic polymer containing carboxyl group in the side chain and the phosphonic acid containing amino group, and reacting to obtain the partially phosphonated olefinic polymer containing carboxyl group in the side chain;
[0104] (2) Dissolve the linear benzimidazole polymer containing amino group, the hyperbranched benzimidazole polymer containing amino group, the partially phosphonated olefin polymer containing carboxyl group in the side chain and the phosphonic acid containing carboxyl group in organic solvent In, mixing, and reacting under heating conditions, the graft copolymer is prepared.
[0105] In a specific embodiment of the present invention, in step (1), the olefinic polymer containing carboxyl groups in the side chain is selected from, for example, polyacrylic acid (PAA), polymethacrylic acid (PMAA)...
Embodiment 1
[0144] (1) Add 1219g of polyphosphoric acid (PPA) to a dry three-necked flask and heat it up to 120°C, then add 3,3-diaminobenzidine (DAB) 3.43g and 2- Phosphonic acid butane-1,2,4-tricarboxylic acid (PBTCA) 2.70g, the solid content accounts for 0.5% of the total solution, stir at this temperature for 4h to fully dissolve the solid. The temperature was raised to 150 °C and maintained in a nitrogen atmosphere for 3 h, and then heated to 200 °C for 20 h. After the reaction stopped, the solution was precipitated in water, washed twice with deionized water, added with sodium bicarbonate to make it alkaline, and then washed with deionized water until neutral. The solid was collected and dried in vacuo at 60°C to yield amino-terminated hyperbranched polybenzimidazole (HBPBI).
[0145] (2) Dissolve 0.15g of polyacrylic acid (PAA) in DMF, then add 0.493g of alendronic acid (95% of the moles of carboxyl groups), react at 150°C for 12h under nitrogen protection, then rotate the solvent...
Embodiment 2
[0150] (1) Other operations are the same as in Example 1, except that: in the dry three-necked flask, add polyphosphoric acid (PPA) 1219g and heat up to 120°C, then add DAB 3.86g and PBTCA 2.70 simultaneously in a molar ratio of 1.8:1 g, the solid content accounts for 0.8% of the total solution, and the solid is fully dissolved by stirring at this temperature for 4 hours. The temperature was raised to 150 °C and maintained in a nitrogen atmosphere for 3 h, and then heated to 200 °C for 20 h.
[0151] (2) Dissolve 0.60 g of PAA in DMF, then add 1.453 g of alendronic acid (accounting for 70% of the moles of carboxyl groups), react at 150 °C for 12 h under nitrogen protection, then rotate the solvent to evaporate the solvent and then dry to obtain a partial phosphonic acid PAA (LPAA).
[0152] (3) 0.30 g of linear mPBI containing amino group and 2.1 g of HBPBI prepared above were dissolved in DMAc to obtain solution a, and 1.948 g of LPAA of step (2) was dissolved in DMF to obta...
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