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 Huntsman 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 down 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
