Synthesis and Characterization of Vanadium Substituted Dawson-Type Heteropoly Acid (Mo, As)  

作　　者：张静 李娟 余立琼 魏先印 刘丽萍 黄如丹 

机构地区：[1]School of Science, Beijing Institute of Technology, Beijing 100081, China [2]Key Laboratory of Rare Earth Chemistry and Physics, Changehun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022, China [3]Department of Chemistry, Normal College, Beihua University, Jilin 132013, China

出　　处：《Journal of Beijing Institute of Technology》2006年第3期336-339,共4页北京理工大学学报（英文版）

基　　金：SponsoredbytheNationalNaturalScienceFoundationofChina(20371007)

摘　　要：Five novel vanadium substituted series of Dawson-type heteropoly acid H7 [As2Mo17VO62 ]·10H2O （1）, H8 [ As2Mo16 V2O62 ]· 7H2O（2）, Ha [ As2MO15 V3O62 ]·8H2O（3）, H8 [ As2Mo14 V4O62 H2 ]·7H2O（ 4 ）, H9[As2Mo13V5O62H2] ·10H2O（5） were prepared respectively in aqueous solution. When magnetic stirring and pH meter monitoring, all reactants mixed and controled different pH, then the mixture was refluxed for 10 h, later extracted by aether when it cooled, finally, it could be recrystaled by 0.5 % sulphuic acid solution, then yielded productions that we need. Compounds （ 1 ） - （5） were characterized by elemental analysis, thermogravimetic analysis （TGA）, infrared spectroscopy （IR）, ultraviolet and visible spectroscopy（UV-Vis）, X-ray powder diffraction analysis, ^51V nuclear magnetic resonance （SIV NMR） structure analysis. The study indicates that these compounds possess Dawson structures, ^51V NMR spectra reveals that V atom is polar-site substituted indeed.Five novel vanadium substituted series of Dawson-type heteropoly acid H7 [As2Mo17VO62 ]·10H2O （1）, H8 [ As2Mo16 V2O62 ]· 7H2O（2）, Ha [ As2MO15 V3O62 ]·8H2O（3）, H8 [ As2Mo14 V4O62 H2 ]·7H2O（ 4 ）, H9[As2Mo13V5O62H2] ·10H2O（5） were prepared respectively in aqueous solution. When magnetic stirring and pH meter monitoring, all reactants mixed and controled different pH, then the mixture was refluxed for 10 h, later extracted by aether when it cooled, finally, it could be recrystaled by 0.5 % sulphuic acid solution, then yielded productions that we need. Compounds （ 1 ） - （5） were characterized by elemental analysis, thermogravimetic analysis （TGA）, infrared spectroscopy （IR）, ultraviolet and visible spectroscopy（UV-Vis）, X-ray powder diffraction analysis, ^51V nuclear magnetic resonance （SIV NMR） structure analysis. The study indicates that these compounds possess Dawson structures, ^51V NMR spectra reveals that V atom is polar-site substituted indeed.

关 键 词：heteropoly acid Dawson-type ^51V nuclear magnetic resonance （^51V NMR） 

分 类 号：O611.4[理学—无机化学] O614.511[理学—化学]