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摘要
Hydrothermal synthesis is known as the most efficient method to prepare novel structural polyoxometalate (POM)-based materials, but controlled synthesis of a structure-directing POM is always challenging task. The experimental repeatability is usually one of the key topics. To explore a reliable hydrothermal synthesis approach for new POMs will be a meaningful work. Our previous work, which we have hydro thermally synthesized the first Cr-complexes-capped Keggin-type POM, [Hdma]3[H(2)phen] {[Cr(phen)](2)[Mo(8)(v)mo(4)(v1)0(36)(PO4)].nH(2)0 (n approximate to 2) (Chen et al., polyhedron, 2015, 85,117), afford us some commendable synthetic experiences, arouse us some introspections as well for its tricky preparation conditions and low experimental repeatability. Based on the aforementioned work, a new high-repetition rate and more steady heteropolyblue, [H(3)0](0).(5)(Hdma)(2.5)(dma)(0.25)(ICr(Phen)](2)[(Mo6Mo6O8)-Mo-V-O-v1(PO4)]}. 2H(2)0 (1) (dma = dimethylamine (C2H7N), phen = 1,10-phenanthroline (C12H8N2)), has been successfully obtained by virtue of reasonably adjusting synthetic strategy. The adjustment of synthetic strategy includes controlling ratio of reactants and aging time, reasonably using redoxes and stepwise self-assembly plans. Compound 1 is the second POM with Keggin-type polyanion capped by Cr-complexes. Experiments demonstrate that compound 1 has good catalytic activity in the both degradation reactions of rhodamine B (RHB) and methyl orange (MO) under ultraviolet (UV)-light and oxidant H2O2 conditions. Detailed structural characterizations include single-crystal X-ray diffraction (XRD) analyses, energy-dispersive X-ray spectrometry (EDS) analyses, elemental analyses, cerate oxidimetry, powder XRD, fourier transform infrared (FT-IR) spectroscopy, ultraviolet visible near-infrared (UV-Vis-NIR) solid diffuse reflection spectrum and X-ray photoelectron spectroscopy (XPS) analyses. The electrochemical property (cyclic voltammetry (CV)) of compound 1 has also been studied.
