水熱合成與表征
(1. 中南大學(xué) 冶金科學(xué)與工程學(xué)院，長沙 410083；
2. 中南大學(xué) 化學(xué)化工學(xué)院，長沙 410083)
摘 要: 在水熱條件下合成了一種以低價(jià)過渡金屬元素鉻取代的高釩雜多化合物K13PV12Cr2O42·21.2H2O，并用元素分析、X射線衍射、紅外光譜、紫外-可見光譜以及X射線光 電子能譜和熱重分析等手段對其進(jìn)行了表征。結(jié)果表明，該雜多化合物具有新奇的雙帽Keggin型結(jié)構(gòu)， 而兩個(gè)低價(jià)的Cr(Ⅲ)原子可能取代了K9PV14O42中處于極位的兩個(gè)帽上的V(Ⅴ)原子，這種取代可能導(dǎo)致該雜多化合物具有較好的催化性能。
關(guān)鍵字: 磷釩鉻雜多酸鹽；雙帽Keggin結(jié)構(gòu)；水熱合成；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
