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作 者:李国清[1,2] 唐晓梅[1] 周百斌[1] 徐学勤[1] 张旭[1]
机构地区:[1]哈尔滨师范大学化学系,哈尔滨150080 [2]哈尔滨学院生命科学与化学学院,哈尔滨150086
出 处:《应用化学》2009年第1期67-71,共5页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金(20371014,20671026);黑龙江省自然科学基金(ZTB2005-33);黑龙江省高校骨干教师创新基金(1055G016);黑龙江省教育厅科研基金(10543071)资助项目
摘 要:用直接法和降解法制备了3种含锂的多金属氧酸盐,采用ICP和TG曲线确定其化学式为K11-n[XLi(OH2)W11O39].xH2O(X为B3+、Si4+、P5+),并用IR、UV、XRD、XPS及183W NMR等测试技术对合成配合物的结构进行了表征。结果表明,所合成的配合物均为典型的Keggin结构,其阴离子骨架上的1个W原子已被1个Li原子取代。热分析结果表明,合成配合物具有较高的热稳定性。循环伏安的测定指出,3种配合物的氧化还原过程为不可逆过程。电导率测试显示,在室温下的各配合物均具有导电性,其电导率分别为:K7[SiLi(OH2)W11O39].xH2O 2.4×10-6S/cm,K6[PLi(OH2)W11O39].xH2O 3.8×10-6S/cm,K8[BLi(OH2)W11O39].xH2O 7.3×10-7S/cm。Three heteropolyoxometalates containing lithium were prepared by means of direct method and degradation for the first time. The chemical formulas were confirmed as Kn [ XLi( OH2 )Wl1O39 ] · xH2O( X = Si,P,B) by ICP and TG and their structures were characterized by IR, UV, XRD, XPS and ^183W NMR. The results show that the new materials are all of Keggin-type structure, in which one W atom has been substituted by one Li atom. The results of DTA indicate that the new materials have good thermostability. The redox cesses are irreversible . The determination results of conductivity show they all have conductivity and the conductivities are 2.4 × 10^-6 S/cm for K7 [ SiLi ( OH2 ) W11O39]· xH2O , 3.8 × 10^ -6 S/cm for K6 [ PLi ( OH2 ) W11O39 ]· xH2O, 7. 3 × 10^-7 S/cm for Ks [ BLi( OH2)W11O39 ] · xH20, respectively.
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