一个铜掺杂的缺位Keggin型链状杂化材料的合成与表征

Hydrothermal Synthesis and Characterization of A Hybrid Material with Copper Doped Keggin-type Lacunary Polyoxometalates

对过渡金属掺杂的缺位Keggin型簇基杂化材料的合成方法及表征手段进行了研究。采用水热合成技术制备了一个具有新颖结构的无机-有机杂化材料{K(H2O)2[Cu0.5(en)][CuSiW11O39]}(H2en)2(1,en=乙二胺),利用元素分析、红外光谱、X射线光电子能谱、TG及X射线单晶衍射等技术对晶体结构进行了分析,并对化合物1的光催化性能进行了研究。结构分析显示,簇基杂化材料是由过渡金属掺杂的缺位Keggin型簇阴离子[SiCuW11O39]6-通过(μ-O)单桥氧原子连接成以簇阴离子为结构单元的1-D链,两个相邻的1-D簇阴离子链再经K(H2O)2[Cu0.5(en)]配合物阳离子通过共价键连接成新颖的1-D"梯子"状双链,质子化的乙二胺填充于网络之中。

In this paper, the crystal synthesis and performance of inorganic organic hybrid materials with metallic oxy gen cluster were studied. A new hybrid material {K（H2O）2[Cu0.5（en）][CuSiW11O39]}（H2en）2 （1, en ethylenediamine） has been hydrothermally synthesized and characterized by elemental analysis, IR, XPS, TG and single crystal X-ray diffraction analysis, and the photucatalytic property of 1 has been investigated. Compound 1 is possessed of 1D chain like structure {[CuSiW11039] 6- }n which was built up Keggin type lacunary polyoxoanions with copper doped [CuSiW11O39]6-, two neighbor 1-D chains are linked by {K（H2O）2[Cu0.5（en）]}2＋ cations to build a ladder like chain structure, which is further interconnected into a 3ID supramolecular framework via hydrogen bonding interactions. Two protonated H2en2＋ is located in the holes of the network.