background and overview[1-2]
2,2′-bipyridyl-4,4′-bisphosphonate is an organic intermediate vulcanizing agent, which can be synthesized from [2,2′-bipyridyl]-4,4′-diylbis(phosphonate) ) tetraethyl ester is prepared in one step. 2,2′-bipyridyl-4,4′-bisphosphate can be used to prepare two-dimensional proton-conducting mofs materials.
preparation[1]
under an argon atmosphere, dissolve [2,2′-bipyridyl]-4,4′-diyl bis(phosphonate) tetraethyl ester (1.0 g, 2.33 mmol) in anhydrous ch2cl2 (~ 50 ml). to this solution was added bromotrimethylsilane (2.15 ml, 12.1 mmol) and the reaction was stirred at room temperature under an argon atmosphere for 3 days. the solvent was removed under vacuum and dry methanol (~30 ml) was added. the solution was stirred at room temperature for 30 min, the methanol was removed under vacuum, and diethyl ether (~60 ml) was added to the white solid. the suspension was stirred for 2 h and the white solid (0.74 g, 87%) was collected by suction filtration. 1 h nmr (mhz, d 6 -dmso): δ (ppm) 8.85 (t, 2h), 8.66 (d, 2h), 7.75 (dd, 2h).
apply[2]
2,2′-bipyridyl-4,4′-bisphosphate can be used to prepare two-dimensional proton-conducting mofs materials with good thermal and chemical stability and good proton conductivity. by introducing bisphosphate groups, the synthesized two-dimensional proton-conducting mofs material has good crystallization ability, high thermal stability and chemical stability, good proton conductivity at medium and low temperatures, and good stability in a variety of solvents. dissolution provides the possibility for its material application, showing attractive application prospects in proton conduction. here’s how:
put 0.05mmol of 2,2′-bipyridyl-4,4′-diphosphate and 05mmol of cucl2 and polyetheramine in a bottle, and then add concentrated hydrochloric acid: water (mass ratio) = 1 : 8 add a total of 1.5ml of the mixture into the bottle, heat at 200 degrees celsius for 5 hours, and cool n naturally to obtain green crystals. unit cell parameters: the compound crystallizes in the monoclinic crystal system, c2/c space group, β=100.391°, f(000)=1656.0, z=8.
references
[1] dennis l. ashford, m. kyle brennaman, robert j. brown, shahar keinan, javier j. concepcion, john m. papanikolas, joseph l. templeton, and thomas j. meyer, inorganic chemistry 2015 54 ( 2), 460-469
[2] [chinese invention] cn201811431284.4 a two-dimensional mofs material with proton conductivity and its preparation method