稀土锗钨钒酸根多元杂多配合物的合成和性质  

Synthesis and Properties of Heteropoly Tungstovanadogermanic Complexes with Rare Earth Elements

作　　者：马慧媛[1] 单永奎[1] 周百斌[1] 赵儒铭[2] 周宏立[1] 

机构地区：[1]哈尔滨师范大学化学系,黑龙江哈尔滨150080 [2]武汉大学化学系,湖北武汉430072

出　　处：《中国稀土学报》2000年第2期97-101,共5页Journal of the Chinese Society of Rare Earths

基　　金：国家自然科学基金!( 2 96710 0 9) ;黑龙江省自然科学基金!(B95 0 2 )

摘　　要：合成了通式为K1 3H2 [Ln(GeW1 0 VO39) 2 ]·nH2 O(Ln =La ,Ce ,Pr ,Nd ,Sm ,Eu ,Gd ,Tb ,Dy ,Yb)的 10种杂多配合物。利用IR ,UV ,ESR ,XPS ,X射线粉末衍射和磁化率对其结构进行了表征 ;循环伏安和极谱法研究了配合物的氧化还原性质 ,得出配合物经历了 3步还原 ,第一步为钒的双电子可逆还原 ,第二步和第三步均为钨的不可逆还原 ;借助变温IR、变温XRD和TG DTA研究了它们的热稳定性 ,表明配合物的热分解温度是 45 0～ 5 0 0℃ ;酸碱中和滴定法对配合物在水溶液中稳定性的研究表明 ,室温下配合物在水溶液中存在的pH范围为 3 3～ 7 6。Ten tungstovanadogermanic complexes K 13 H 2[Ln(GeW 10 VO 39 ) 2]·nH 2O(Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Yb) were synthesized. Their structure were characterized by IR, UV, ESR, XPS, XRD and magnetic susceptibility. The redox properties of them were studied by means of cyclic voctammetry and polargraphy. The results show that the complexes undergo three step reduction, of which the first step is the double electronic reversible reduction, and the second and the third steps are irreversible reduction. Their thermal stability studied by TG DTA, IR and XRD at various temperatures show that the range of temperature of pyrolysis is 450～500 ℃. The complexes stability in solution investigeted by the acid alkali titration indicates that the range of pH in which the heteropoly anions can exist stably is 3 3～7 6 at room temperature.

关 键 词：稀土 钨钒锗 杂多配合物 结构 杂多化合物 催化 

分 类 号：O614.33[理学—无机化学] TQ426.91[理学—化学]