钒锰基杂多酸制备方法的优化及其结构解析

Preparation of Vanadium and Manganese based POMs and the Analysis of its Structure and Properties

本文以钒酸钠和硫酸锰为主要原料,通过加入乙醇试剂,快速高效的制备了Keggin结构的钒锰基杂多酸(NaH[MnVO]),其质量收率从传统的25%增加至60%,质量收率显著增加。为了进一步探索本制备方法得到的杂多酸微观相貌和结构特性,文章采用显微镜、单晶衍射、XRD、FTIR和SEM表征手段研究了其结构特征,并考察了其热稳定性和水溶性。研究结果表明:本文制备的钒锰基杂多酸具有菱形四面体形貌,其微观结构由四面体和八面体组成,结晶度较高,每个钒锰基杂多酸分子中含有13个结晶水,分子中的钒元素由四价和五价组成,锰元素为6价,颗粒尺寸分布均匀,均大于500μm,且在0~50℃之间具有良好的水溶性。

In this paper, the polyoxometalate(NaH[MnVO]) with Keggin structure based on vanadium and manganese was prepared from NaVOand MnSO. Its structural characteristics were studied by microscope, single crystal diffraction, XRD, TG, FTIR and SEM. The electrochemical properties of its aqueous solution were studied by three electrode test system. The results show that the polyoxometalates based on vanadium and manganese prepared in this paper has a rhombic tetrahedron morphology, its microstructure is composed of tetrahedron and octahedron, and its crystallinity is high. Each polyoxometalate molecule contains 13 crystalline water, V in the molecule is composed of tetravalent and pentavalent, Mn is 6 valence, the particle size is large, the water solubility is good at 0~50 ℃.