Synthesis and Spectral Study of Amine Salt of Tungstovanadophosphoric Heteropolyacid with Dawson Structure
LIU Xia1,ZHAO Jun2,FENG Chang-gen2*,LI Hong-zhen3
1. College of Science,China Agriculture University,Beijing 100094,China 2. Research and Development Center of New Medication,Beijing Institute of Technology,Beijing 100081,China 3. Institute of Chemical Materials,China Academy of Engineering Physics,Mianyang 621900,China
Abstract:Parent heteropoly salt was prepared by the method of stepwise addition of materials-stepwise acidification and distillation. Firstly,tungstovanadophosphoric heteropolyacid with tri-wanadium-substituted Dawson structure was synthesized with ammonium metavanadate,sodium dihydrogen phosphate and sodium tungstate as materials under the conditions of pH 4 and reaction time of 10 h. Secondly,parent heteropoly salt K9P2W15V3O62·41H2O was prepared by adding counterion K+ 5 times as much as determined by stoichiometric relation of reaction to the solution of tungstovanadophosphoric heteropolyacid. The acid solution of the parent heteropoly salt was slowly added to the solution of hexadecyltrimethylammonium bromide with continually stirring,then amine salt of tungstovanadophosphoric heteropolyacid,(C19H42N)6H3[P2W15V3O62] was synthesized. The target compound was characterized by elemental analysis,IR,XRD powder diffraction and TG-DTA,and the results indicated that it was a new heteropoly compound retaining Dawson structure.
刘霞1,赵军2,冯长根2*,李洪珍3. Dawson结构磷钨钒杂多酸有机铵盐的合成及光谱研究[J]. 光谱学与光谱分析, 2007, 27(08): 1584-1586.
LIU Xia1,ZHAO Jun2,FENG Chang-gen2*,LI Hong-zhen3. Synthesis and Spectral Study of Amine Salt of Tungstovanadophosphoric Heteropolyacid with Dawson Structure . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2007, 27(08): 1584-1586.