两个钒同多酸化合物的光谱测试  

Spectral Experimental Research of Two Novel Isopolyoxovanadates

作　　者：陈义平 孙瑞卿 杨珍 CHEN Yiping;SUN Ruiqing;YANG Zhen(College of Chemistry,Fuzhou University,Fuzhou 350116,China;State Key Laboratory of Structural Chemistry,Fuzhou University,Fuzhou 350002,China)

机构地区：[1]福州大学化学学院,福州350116 [2]福州大学结构化学国家重点实验室,福州350002

出　　处：《实验室研究与探索》2019年第12期4-9,共6页Research and Exploration In Laboratory

基　　金：国家自然科学基金项目(21473030,21371033)

摘　　要：水热法合成了两个新的钒同多酸化合物[H 2en]3n[V 6O 18]n(化合物1)和[Cu(en)2]3[V 10 O 28]·6H 2O(化合物2)。通过X射线单晶衍射确定化合物1属于三斜晶系,呈一维链状结构;化合物2属于单斜晶系,为孤立结构。二维红外相关光谱显示钒多酸阴离子骨架及N—H…O氢键对外界热微扰比较敏感,固体紫外漫反射光谱反映了结构中O→V的荷移跃迁,热重分析揭示多酸化合物热稳定性及结构变化,高温红外测试进一步验证随着温度变化,游离水、游离有机胺分子、胺合金属阳离子的脱除顺序。Two novel isopolyoxovanadates[H 2en]3n[V 6O 18]n(compound 1)and[Cu(en)2]3[V 10 O 28]·6H 2O(compound 2)were synthesized by hydrothermal method.Via X-ray single crystal diffraction,compound 1 belongs to triclinic system and has one-dimensional chain structure,while compound 2 belongs to monoclinic system and is isolated.2D-COS FTIR shows that the anion skeleton of polyoxovanadate and the hydrogen bond of N—H…O are sensitive to external thermal perturbation.UV-DRS reflects the charge transfer transition of O→V in the structure.TG analysis indicates the thermal stability and structural changes of polyoxovanadates.High temperature infrared measurements show that the decreasing order of small-molecule removal is free water,free organic amine molecule,amine metal cation.

关 键 词：钒同多酸化合物 二维红外相关光谱 高温红外光谱 固体紫外漫反射光谱 

分 类 号：O614.51[理学—无机化学] G642.0[理学—化学]