H_2O-DMSO体系中联吡啶甲基化及其钨硅酸盐的形成

N-methylation of dipyridyl in H_2O-DMSO and the formation of its tungstosilicate

以Keggin型钨硅酸H_4[SiW_(12)O_(40)]·24H_2O和MN^(2+)为原料,4,4′-联吡啶(4,4′-bipy)为有机前驱体,水和二甲基亚砜(DMSO)为混合溶剂,在水热条件下,4,4′-bipy发生N-甲基化,并与DMSO共同修饰[SiW_(12)O_(40)]^(4-)阴离子,形成了1个钨硅酸盐基无机-有机杂化化合物(CH_3)_2bipy)((CH_3)_2SOH)_2[SiW_(12)O_(40)].通过元素分析、红外光谱(IR)、热重(TG)及X-射线单晶衍射分析对该化合物进行了表征,初步探讨了该化合物的形成条件,并研究了其在水溶液中的电化学性质及其对H_2O_2还原的电催化活性.

A new tungstosilicate-based inorganic-organic hybrid compound constructed by Keggin-type tungstosilicic acid H4[SiW（12）O（40）]·24 H2O,MN（2＋）and organic precursor 4,4′-dipyridyl（4,4′-bipy）,namely（C（12）H（14）N2）（C2H6SOH）2[SiW（12）O（40）],was synthesized under hydrothermal conditions in dimethyl sulfoxide（DMSO）and water mixed solvent.In title compound,the N-methylated 4,4′-bipy and DMSO co-modified the[SiW（12）O（40）]（4-）anion.Title compound was characterized by elemental analysis,infrared spectroscopy（IR）,thermogravimetry（TG）and X-ray single crystal diffraction.In addition,the synthetic condition of title compound was also discussed,and the electrochemical properties in aqueous solution and the electrocatalytic activity of title compound for H2O2 reduction were also studied.