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New sterically hindered tin(IV) siloxane precursors to tinsilicate materials: synthesis, spectral, structural and photocatalytic studies

机译:新的空间阻碍锡(IV)硅氧烷前体溶硅酸盐材料:合成,光谱,结构和光催化研究

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摘要

A series of sterically hindered tin(IV) siloxanes were synthesized by the reaction between tris(tert-butoxy) silanol/tri-phenylsilanol and organotin chlorides {[(Bu-t)(2)Sn(OSi((OBu)-Bu-t)(3))(2)] (1), [(Bu-t)(2)Sn(OSi((OBu)-Bu-t)(3)) Cl] (2), [(n-Bu)(2)Sn(OSi((OBu)-Bu-t)(3))(2)] (3), [(n-Bu)(2)Sn(OSi((OBu)-Bu-t)(3))Cl] (4), [(Me)(2)Sn(OSi((OBu)-Bu-t)(3))(2)] (5), [(Me)(2)Sn(OSi((OBu)-Bu-t)(3)) Cl] (6), [(Bu-t)(2)Sn(OSiPh3)(2)] (7), [(Bu-t)(2)Sn(OSiPh3) Cl] (8) whereas Bu-t = tertiary butyl; n-Bu = butyl; Me = methyl}. All the compounds were characterized by analytical and spectroscopic (FT-IR and H-1, C-13, Si-29, Sn-119 NMR) methods. Compounds 1 and 7 were structurally characterized by single-crystal X-ray crystallography. The coordination geometry of tin (SnO2C2) is slightly distorted from tetrahedral due to sterically crowded ligands around the tin atom. In order to convert tinsilicate materials, compounds 1 and 3 were selected for thermolysis to give identical SnO2 center dot 2SiO(2) materials at low temperature (similar to 350 degrees C). The degradation was investigated by thermal analysis (TGA/DTA), both compounds having butyl groups which facile eliminate to butene gas via a beta-hydride elimination process (similar to 250 degrees C). The molecular route to oxide materials at low temperature described here represents an alternative to the sol-gel technique. The tinsilicate material was examined by several techniques including infrared, powder X-ray diffraction analysis (PXRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX). The optical band gap of the material has been studied by UV-vis-NIR spectroscopy and the result is a low band gap value (E-g = 2.549 eV) due to the silicon oxide mixed with tin oxide. The prepared material acts as photocatalyst for the degradation of methylene blue (MB).
机译:一系列的空间位阻的锡(IV)的硅氧烷是由三(叔丁氧基)硅烷醇/三phenylsilanol和有机锡氯化物之间的反应合成的{[(BU-T)(2)的Sn(OSI((OBU)-Bu-吨)(3))(2)](1),[(BU-T)(2)的Sn(OSI((OBU)-Bu-T)(3))CL](2),[(正丁基)(2)的Sn(OSI((OBU)-Bu-T)(3))(2)](3),[(正丁基)(2)的Sn(OSI((OBU)-Bu-T)( 3))CL](4),[(Me)的(2)的Sn(OSI((OBU)-Bu-T)(3))(2)](5),[(Me)的(2)的Sn(OSI ((OBU)-Bu-T)(3))CL](6),[(BU-T)(2)的Sn(OSiPh3)(2)](7),[(BU-T)(2)的Sn (OSiPh3)CL](8),而卜叔=叔丁基;正Bu =丁基; Me =甲基}。通过分析和光谱(FT-IR和H-1,C-13,的Si-29系,Sn-119 NMR)方法的所有化合物进行表征。化合物1和7结构特征在于单晶X射线晶体学。锡的配位几何形状(SnO2C2)稍微从四面体由于周围的锡原子在空间上拥挤的配体扭曲。为了tinsilicate物质转化,将化合物中的1和3为热解,得到相同的SnO2中心点2SiO(2)在低温下(类似350摄氏度)的材料。降解通过热重分析(TGA / DTA)研究中,具有丁基基团经由β-氢消除反应过程(类似于250℃),其容易消除丁烯气体两种化合物。在这里描述的低温氧化物材料的分子路线表示到溶胶 - 凝胶技术的替代方案。所述tinsilicate物质通过几种技术包括红外,粉末X射线衍射分析(PXRD),扫描电子显微镜(SEM)和能量色散X射线(EDX)检测。该材料的光学带隙已研究通过UV-vis-NIR光谱,结果是低带隙值(E-G = 2.549 eV)的因氧化硅与氧化锡混合。所制备的材料作为光催化剂对亚甲基蓝(MB)的降解。

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  • 来源
    《RSC Advances》 |2016年第3期|共9页
  • 作者单位

    VIT Univ Sch Adv Sci Mat Chem Div Vellore 632014 Tamil Nadu India;

    VIT Univ Sch Adv Sci Mat Chem Div Vellore 632014 Tamil Nadu India;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
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