河南大学学报(自然科学版)
河南大學學報(自然科學版)
하남대학학보(자연과학판)
JOURNAL OF HENAN UNIVERSITY(NATURAL SCIENCE)
2008年
6期
575-579
,共5页
周朵%李继利%牛红雨%王伟%王敬平
週朵%李繼利%牛紅雨%王偉%王敬平
주타%리계리%우홍우%왕위%왕경평
多金属氧酸盐%水热合成%Keggin 结构%硅钨酸盐
多金屬氧痠鹽%水熱閤成%Keggin 結構%硅鎢痠鹽
다금속양산염%수열합성%Keggin 결구%규오산염
polyoxometalates%hydrothermal synthesis%keggin structure%silicotungstate
通过水热合成方法,合成了一种新型的硅钨酸盐担载的有机无机复合物[Zn(2,2'-bipy)3]1.5[SiW12O40Zn(2,2'-bipy)2(OH)]·0.25H2O,并对其进行了元素分析、红外光谱、热分析及X-射线单晶衍射等表征.结构分析表明,标题化合物结构单元中含有1个 [SiW12O40Zn(2,2'-bipy)2(OH)]3-杂多阴离子,1.5个[Zn(2,2'-bipy)3]2+ 阳离子和0.25个结晶水分子.在[SiW12O40Zn(2,2'-bipy)2(OH)]3-杂多阴离子中,Keggin阴离子[SiW12O40]4-通过一个端氧原子与[Zn(2,2'-bipy)2(OH)]+共价相连.TG-DTA 热分析曲线表明多阴离子的骨架在618 ℃分解.
通過水熱閤成方法,閤成瞭一種新型的硅鎢痠鹽擔載的有機無機複閤物[Zn(2,2'-bipy)3]1.5[SiW12O40Zn(2,2'-bipy)2(OH)]·0.25H2O,併對其進行瞭元素分析、紅外光譜、熱分析及X-射線單晶衍射等錶徵.結構分析錶明,標題化閤物結構單元中含有1箇 [SiW12O40Zn(2,2'-bipy)2(OH)]3-雜多陰離子,1.5箇[Zn(2,2'-bipy)3]2+ 暘離子和0.25箇結晶水分子.在[SiW12O40Zn(2,2'-bipy)2(OH)]3-雜多陰離子中,Keggin陰離子[SiW12O40]4-通過一箇耑氧原子與[Zn(2,2'-bipy)2(OH)]+共價相連.TG-DTA 熱分析麯線錶明多陰離子的骨架在618 ℃分解.
통과수열합성방법,합성료일충신형적규오산염담재적유궤무궤복합물[Zn(2,2'-bipy)3]1.5[SiW12O40Zn(2,2'-bipy)2(OH)]·0.25H2O,병대기진행료원소분석、홍외광보、열분석급X-사선단정연사등표정.결구분석표명,표제화합물결구단원중함유1개 [SiW12O40Zn(2,2'-bipy)2(OH)]3-잡다음리자,1.5개[Zn(2,2'-bipy)3]2+ 양리자화0.25개결정수분자.재[SiW12O40Zn(2,2'-bipy)2(OH)]3-잡다음리자중,Keggin음리자[SiW12O40]4-통과일개단양원자여[Zn(2,2'-bipy)2(OH)]+공개상련.TG-DTA 열분석곡선표명다음리자적골가재618 ℃분해.
A new Keggin-type silicotungstate anion-supported organic-inorganic hybrid transition metal complex [Zn(2,2'-bipy)3]1.5[SiW12O40Zn(2,2'-bipy)2(OH)]·0.25H2O (2,2'-bipy = 2,2'-bipyridine) has been synthesized by hydrothermal method and characterized by elemental analysis, IR spectrum, TG-DTA and single crystal X-ray diffraction. The analysis indicates that each structure unit of the title compound consists of a [SiW12O40Zn(2,2'-bipy)2(OH)]3- heteropolyanion, one and a half [Zn(2,2'-bipy)3]2+ cations, and a quarter of crystal water molecules. The [Zn(2,2'-bipy)2(OH)]+ unit is covalently bonded to one Keggin polyoxoanion [SiW12O40]4- through a terminal oxygen atom in the [SiW12O40Zn(2,2'-bipy)2(OH)]3- heteropolyanion. The TG-DTA analysis exhibits that the anion framework collapses at 618 ℃.