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.
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)
出处
《实验室研究与探索》
CAS
北大核心
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)
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
isopolyoxovanadates
two-dimensional infrared correlation spectroscopy(2D-COS FTIR)
high temperature infrared spectroscopy
solid ultraviolet diffuse reflectance spectroscopy(UV-DRS)