A kind of phosphonated (polyolefin-g-hyperbranched polybenzimidazole) graft copolymer and its preparation method and application
A technology of graft copolymer and benzimidazole, which is applied in the field of phosphonated graft copolymer and its preparation, can solve the problems of phosphoric acid loss, reduction of proton conductivity, decrease of mechanical properties, etc., to promote migration and improve proton conductivity. efficiency, high proton conductivity
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[0088]
[0089] The present invention also provides a kind of preparation method of above-mentioned graft copolymer, it comprises the steps:
[0090] (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;
[0091] (2) dissolving amino group-containing hyperbranched benzimidazole polymers, side chain carboxyl-containing partially phosphonated olefin polymers and carboxyl-containing phosphonic acids in an organic solvent, reacting under heating conditions to prepare the described graft copolymer.
[0092] 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), carboxylated polystyrene at least one of .
[0093] In a specific embodiment of the ...
Embodiment 1
[0128] (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.
[0129] (2) Dissolve 0.3 g of polyacrylic acid (PAA) in DMAc, then add 0.986 g of alendronic acid (accounting for 95% of the carboxyl moles), react at 150° C. for 12 h under the protection of ...
Embodiment 2
[0134] (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.
[0135] (2) Dissolve 0.45g of PAA in DMAc, then add 1.090g of alendronic acid (accounting for 70% of the carboxyl moles), react at 150°C for 12h under the protection of nitrogen, and then dry by rotary evaporation of the solvent to obtain partially phosphonated PAA (LPAA).
[0136] (3) According to the mass ratio of 1.75:1, the total mass of 4.01 g of HBPBI in (1) and LPAA in (2) were dissolved in DMAc to obtain solution a. 1.502 g of phosphonoacetic acid was dissolved in DMF to obtain solut...
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