Keggin结构钼硅稀土杂多蓝的合成及性质研究

合成了钼硅稀土二电子、四电子杂多蓝ＬｎＨ３〔ＳｉＭｏ１０＾ＶＩＭｏ２＾ＶＯ４０〕·１２Ｈ２Ｏ和ＬｎＨ５〔ＳｉＭｏｇ＾ＶＩＭｏ４＾ＶＯ４０〕·１３Ｈ２Ｏ,其中Ｌｎ＝Ｌａ,Ｃｅ,Ｐｒ,Ｎｄ,Ｓｍ,Ｇｄ,通过ＩＲ,ＵＶ,ＴＧ－ＤＴＡ,ＸＰＳ,ＥＳＲ磁化率等对杂多蓝进行表征。结果表明,杂多酸盐还原为杂多蓝后,结构上发生了轻微的畸变。     

Keggin结构钨钼磷混配杂多酸盐的合成和性质研究

用复分解法首次合成了５种Ｋｅｇｇｉｎ结构钨钼磷混配杂多酸盐ＭｘＰＷ４Ｍｏ８Ｏ４０．ｎＨ２Ｏ（Ｍ＝Ｅｔ４Ｎ,Ｂｕ４Ｎ,Ｋ,Ｂａ,Ｚｎ）,通过ＩＲ,ＵＶ,ＤＴ－ＴＧＡ,极谱及循环伏安对它们进行了表征。     

Keggin结构过氧钛钨硅杂多配合物~(183)WNMR谱的研究

合成了Keggin结构一，三取代过氧铁钨硅杂多配合物，这两种化合物是：α－K6［SiW11（Tio2）O39］·12H2O和α－K9H［SiW9（TiO2）O39］·12H2O，并对183WNMR谱进行了指认，从而确定了2种过氧杂多配合物的基本结构．     

Keggin结构和Dawson结构稀土杂多配合物热稳定性研究

首次合成了十种具有Keggin结构的硅钨钒四元稀土杂多配合物和七种具有Dawson结构的磷钼钒稀土杂多配合物;并利用TG、DTA、IR光谱和x射线粉末衍射等手段研究了两系列稀土杂多配合物的热稳定性;总结并解释了近年来文献报道的Keggin结构和Dawson结构的稀土杂多配合物的热稳定性的变化规律。     

基于Keggin型同多钨酸盐稀土配合物的合成、晶体结构与表征

以Ln(NO_3)_3(Ln=Ce~(3+),Pr~(3+),Sm~(3+))、3,5-吡啶二甲酸和[H2W12O40]6-多阴离子为原料,用常规水溶液合成方法合成3个同构化合物,并用X射线单晶衍射对其结构进行表征.结果表明:[H2W12O40]6-多阴离子通过Ln—O键和Ln3+相连,形成了一维双链结构;Ln3+与吡啶二甲酸阴离子相连,Ln3+与有机配体阴离子相连,形成"方波"字形链;最终"方波"字形链与稀土-多阴离子双链相连,形成二维结构.     

2种Keggin型多金属氧酸盐化合物的合成和晶体结构

利用常规合成方法合成了2个由2,2′-联咪唑修饰的Keggin型多金属氧酸盐有机-无机杂化化合物:[H3(biim)2](C4H8O2)2[PW12O40].11H2O(1)和[H3(biim)2](C4H8O2)3[PMo12O40].3H2O(2)(H2biim=2,2′-联咪唑),并通过单晶X射线衍射、元素分析、IR光谱和电化学分析等进行了表征.结构分析表明化合物1属于单斜晶系,C2/c空间群,化合物2属于正交晶系,Pbca空间群.分子间通过静电引力作用和氢键作用形成了三维超分子网状结构.     

稀土金属锗钨杂多配合物的合成及表征

以稀土金属离子镝和多金属氧酸阴离子[GeW11O39]^8-为构筑块,通过分子设计与组装,与有机分子DMSO在一定条件下合成出一维链状化合物[Dy2（GeW11O39）（DMSO）（H2O）9]n^2-,该化合物晶体属单斜晶系,P21/c空间群,晶胞参数：a=23.537（5）,b=11.515（2）,c=23.418A,β=109.17（3）°,V=599 5（2）A^3,F（000）=601 4,Z=4,μ=24.712 mm^-1,对化合物进行了元素分析、IR、UV、CV及X-射线单晶衍射等谱学表征及结构、性质研究.     

具有Keggin结构—取代过氧型杂多配合物及其几何异构体的合成、表征及催化活性的研究

采用立体有择法合合成了具有 Kaggin结构的过氧型杂多配合物 :α-M6- m Hm[Si W11Ti O4 0 ]·x H2 O,α-M6- m Hm[Si W11( Ti O2 ) O3 9]· x H2 O和βi-M6- m Hm[Si W11( Ti O2 ) O3 9)· x H2 O.( m=K、TBA;i=1 ,2 ,3 ) ;用 IR、UV、极谱—循环伏安、183 WNMR等测试方法对其性质、结构进行研究 .结果表明 :它们都是具有 Keggin结构的过氧杂多配合物 ,它们对顺丁烯二酸的 H2 O2 环氧化反应具有显著的催化活性 .     

Synthesis, characterization and properties of ruthenium-substituted polyoxometallic acid H_6Ru(H_2O)FeW_(11)O_(39)·18H_2O with Keggin structure

The ruthenium-substituted polyoxometallic acid H6 [Ru(H2O)FeW 11O39 ]·18H2O was synthesized by stepwise acidification and stepwise addition of solutions of the component elements, and an ion-exchange-cooling method. The product was characterized using inductively coupled plasma spectrometry (ICP), Infrared Spectroscopy (IR), Ultraviolet Spectroscopy (UV), and X-ray diffraction (XRD). The results show that this complex has the Keggin structure. The determination of the thermal stability and proton conductivi...     

Effect of total aluminum concentration on the formation and transformation of nanosized Al13 and Al30 in hydrolytic polymeric aluminum aqueous solutions

Influence of total aluminum concentration （CAIT） on the generation and transformation of nanosized AI13 and AI30 in hydrolytic polyaluminum aqueous solutions was investigated using high field 27AI NMR and time-developed AI-Ferron complex colorimetry. When prepared at the optimal basicity （B） of Al13 generation and 80℃, the All3 species in polyaluminum solution tends to further polymerize and convert to AI30 and higher polymers when CAI; 〉0.2 mol· L^-1, but Al13 does not convert to AI30 quantificationally, as the formation of Alu from Al13 and AI30 is accelerated in the same way. The conversion rate of All3 is accelerated by the increase in CAIT. When CAlT 〉0.75 mol·.L^-1, Al13 content decreases rapidly, and AI30 content increases continuously and becomes the dominant nanometer polynuclear aluminum species. AIm is one of prerequisites of Al13 conversion to AI30. When CAI; increases and B reduces, the polymerization rate between Al13 and Aim increases, and at the same time, the dissociation reaction rate of All3 and AI30 by H^＋ also increases. The latter becomes the dominant reaction in polyaluminum solution with low B value, so AI30 decreases with the increasing CAlT. The hydrolytic polyaluminum solution with Al13 content beyond 80% can only be prepared under the condition of CAlT〈0.5 mol· L^-1 and optimal B value.