Phosphorylated polyolefin grafted benzimidazole polymer proton exchange membrane as well as preparation method and application thereof
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. problem, achieve the effect of promoting migration and improving proton conductivity
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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 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, solid content accounted for 0.5% of the total solution, stirred at this temperature for 4h to fully dissolve the solid. The temperature was raised to 150°C and maintained in a nitrogen atmosphere for 3h, and then heated to 200°C for 20h. After the reaction stopped, the solution was precipitated in water, washed twice with deionized water, then added with sodium bicarbonate to make it alkaline, and then washed with deionized water until neutral. The solid was collected and dried under vacuum at 60° C. to obtain hyperbranched polybenzimidazole (HBPBI) with amino as the end group.
[0145] (2) 0.15 g of polyacrylic acid (PAA) was dissolved in DMF, then 0.493 g of alendronic acid (accounting for 95% of carboxyl moles) was added, and reacted at 150° C. for 12 h under the p...
Embodiment 2
[0150] (1) Other operations are the same as in Example 1, the difference is: add polyphosphoric acid (PPA) 1219g to a dry three-necked flask and heat up to 120°C, then add DAB 3.86g and PBTCA 2.70 at the same time with a molar ratio of 1.8:1 g, the solid content accounted for 0.8% of the total solution, stirred at this temperature for 4 hours to fully dissolve the solid. The temperature was raised to 150°C and maintained in a nitrogen atmosphere for 3h, and then heated to 200°C for 20h.
[0151] (2) Dissolve 0.60g of PAA in DMF, then add 1.453g of alendronic acid (accounting for 70% of the carboxyl moles), react at 150°C for 12h under the protection of nitrogen, and then dry the solvent by rotary evaporation to obtain partially phosphonated PAA (LPAA).
[0152] (3) 0.30 g of amino-containing linear mPBI and 2.1 g of the above-prepared HBPBI were dissolved in DMAc to obtain solution a, and 1.948 g of LPAA in step (2) was dissolved in DMF to obtain solution b. 1.414 g of phosp...
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