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以12-钼磷酸和吡啶为原料合成了一种电荷转移盐。通过C,N,Mo和P元素分析和热重分析确定其组成为[C5H5NH]3[PMo12O40].4.5H2O,各元素的质量分数分别为(括号内为理论值)C 8.82%(8.42%),N 1.69%(1.96%),P 1.40%(1.45%)和Mo 52.98%(53.78%);采用红外光谱、紫外-可见漫反射光谱、X射线粉末衍射和循环伏安法等分析手段对该化合物进行了表征。结果表明:所合成的新型电荷转移化合物的杂多阴离子保持Keggin结构特征;相对于H3PMo12O40.xH2O,[C5H5NH]3[PMo12O40].4.5H2O中由于离域π键的存在,对紫外-可见光的吸收从紫外区拓展到可见光区,并且在波长为370 nm处出现新的吸收峰;其还原电位为0.21 V,较H3PMo12O40.xH2O的还原电位(0.32 V)低,故其还原能力增强。
A kind of charge transfer salt was synthesized from 12-molybdophosphoric acid and pyridine. The composition of [C5H5NH] 3 [PMo12O40] .4.5H2O was determined by elemental analysis of C, N, Mo and P and TG analysis. The mass fractions of each element were respectively (theoretical value in parentheses) C 8.82% (8.42% , N 1.69% (1.96%), P 1.40% (1.45%) and Mo 52.98% (53.78%), respectively. The results of IR, UV-Vis, XRD and cyclic voltammetry Compounds were characterized. The results showed that the heteropolyanions of the new charge-transfer compounds retained the Keggin structure. Compared with H3PMo12O40.xH2O, [C5H5NH] 3 [PMo12O40] .4.5H2O, due to the delocalized π bond, the UV-Vis absorption From ultraviolet to visible region, new absorption peak appears at 370 nm. The reduction potential is 0.21 V, which is lower than that of H3PM12O40.xH2O (0.32 V), so its reduction ability is enhanced.