水热合成与表征
(1. 中南大学 冶金科学与工程学院，长沙 410083；
2. 中南大学 化学化工学院，长沙 410083)
摘 要: 在水热条件下合成了一种以低价过渡金属元素铬取代的高钒杂多化合物K13PV12Cr2O42·21.2H2O，并用元素分析、X射线衍射、红外光谱、紫外-可见光谱以及X射线光 电子能谱和热重分析等手段对其进行了表征。结果表明，该杂多化合物具有新奇的双帽Keggin型结构， 而两个低价的Cr(Ⅲ)原子可能取代了K9PV14O42中处于极位的两个帽上的V(Ⅴ)原子，这种取代可能导致该杂多化合物具有较好的催化性能。
关键字: 磷钒铬杂多酸盐；双帽Keggin结构；水热合成；表征
characterization of novel bi-capped Keggin
heteropolychromovanadophosphate
（1. School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China;
2. College of Chemistry and Chemical Engineering,
Central South University, Changsha 410083, China）
Abstract:The Cr3+-substituted vanadophosphate (K13PV12Cr2O42·21.2H2O) was synthesized by hydrothermal synthesis method for the first time and characterized by elementary analysis, IR and UV-Vis spectra, X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS) and TG analysis. The results show that the heteropolyanion (PV12Cr2O13-42) has a novel bi-capped Keggin structure and there is agreat possibility that the two vanadium(Ⅲ) atoms in the poles of PV14O9-42 are substituted by two low valence chromium (Ⅴ) atoms. In addition, the substitution may lead to better catalytic performances of the title compound.
Key words: heteropolychromovanadophosphate; bi-capped Keggin structure; hydrothermal synthesis; characterization
