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两个新的Dowson结构硫钼多酸盐合成,表征以及催化性质
引用本文:孙月霞,张志斌,孙 琪,许 岩.两个新的Dowson结构硫钼多酸盐合成,表征以及催化性质[J].无机化学学报,2011,27(3):556-560.
作者姓名:孙月霞  张志斌  孙 琪  许 岩
作者单位:1. 辽宁师范大学化学化工学院,化学功能材料研究所,大连,116029
2. 南京工业大学化学化工学院,材料化学工程国家重点实验室,南京,210009
3. 辽宁师范大学化学化工学院,化学功能材料研究所,大连,116029;南京工业大学化学化工学院,材料化学工程国家重点实验室,南京,210009
基金项目:国家自然科学基金(No.20771050、20971068); 辽宁省教育厅基金(No.2008T106)资助项目
摘    要:通过水热技术合成了两种新的Dowson结构硫钼多酸盐C5N2H14]2S2MoⅥ18O62].8H2O(1)和C5N2H14]8(H3O)2S2MoⅤ2MoⅥ16O62]3.(C5H5N)2(2),并通过X射线分析、红外光谱和元素分析其进行了表征。X射线晶体结果分析,化合物1结晶于正交晶系,Pmmn空间群,a=1.79929(17)nm,b=1.35804(13)nm,c=1.41926(13)nm,V=3.4680(6)nm3,Z=2。化合物2结晶于单斜晶系,C2/m空间群,a=2.266 5(3)nm,b=1.374 9(2)nm,c=3.291 2(5)nm,β=104.31(0)°,V=9.938(2)nm3,Z=4。化合物1和2都含有Dawson结构的硫钼多酸阴离子和质子化的N-甲基哌嗪阳离子。并且由苯乙烯的氧化催化结果中看出混价钼的化合物2的催化活性要比化合物1略高。

关 键 词:硫钼酸盐  晶体结构  水热合成  催化

Syntheses, Characterization and Catalytic Properties of Two New Wells-Dawson Molybdosulfates
SUN Yue-Xi,ZHANG Zhi-Bin,SUN Qi and XU Yan.Syntheses, Characterization and Catalytic Properties of Two New Wells-Dawson Molybdosulfates[J].Chinese Journal of Inorganic Chemistry,2011,27(3):556-560.
Authors:SUN Yue-Xi  ZHANG Zhi-Bin  SUN Qi and XU Yan
Institution:Institute of Functionalized Chemistry Materials, Faculty of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian, Liaoning 116029, China,College of Chemistry and Chemical Engineering, State Key Laboratory of Materials-oriented Chemical Engineering, Nanjing University of Technology, Nanjing 210009, China,Institute of Functionalized Chemistry Materials, Faculty of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian, Liaoning 116029, China and Institute of Functionalized Chemistry Materials, Faculty of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian, Liaoning 116029, China; College of Chemistry and Chemical Engineering, State Key Laboratory of Materials-oriented Chemical
Abstract:Two new wells-Dawson compounds C5N2H14]2S2MoⅥ18O62]· 8H2O (1) and C5N2H14]8(H3O)2S2MoⅤ2MoⅥ16O62]3·(C5H5N)2 (2) have been synthesized and characterized by single crystal X-ray analysis, IR spectra and elemental analysis. Single crystal X-ray diffraction confirms that compound 1 crystallizes in orthorhombic, a=1.799 29(17)nm, b=1.358 04(13) nm, c=1.419 26(13) nm, V=3.468 0(6) nm3, Z=2. Compound 2, monoclinic, a=2.266 5(3) nm,b=1.3749(2) nm, c=3.291 2(5) nm, β=104.31(0)°, V=9.938(2) nm3, Z=4. Both compound 1 and 2 are built up of the Dawson-type molybdosulfate anions, full protonated N-methylpiperazine cations. The catalytic result in the oxidation of styrene indicates that the mixed MoⅤ/MoⅥ compound 2 has higher catalytic activity than 1. CCDC:783378, 1; 783379, 2.
Keywords:molybdosulfate  crystal structure  hydrothermal synthesis  catalysis
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