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作 者:朱传高[1] 王凤武[1] 徐迈[1] 方文彦[1]
出 处:《吉林大学学报(理学版)》2013年第5期955-960,共6页Journal of Jilin University:Science Edition
基 金:国家自然科学基金(批准号:21176099);安徽省教育厅自然科学基金重点项目(批准号:KJ2010A309)
摘 要:用电解法在乙二醇溶液中制备铅和钛醇盐配合物PbTi2(OCH2CH2OH)12-x,将其电解液水解、真空干燥后于450℃煅烧2 h,得到纳米级PbO2/TiO2粉体,通过溶胶-凝胶法在钛丝表面得到纳米PbO2/TiO2电极.电解产物通过红外光谱(FT-IR)和Raman光谱表征,纳米PbO2/TiO2粉体使用X射线衍射(XRD)和扫描电子显微镜(SEM)表征,并采用循环伏安法在盐酸和己二醛溶液中考察电极的氧化还原行为及电催化活性.实验结果表明:有机体系电解法得到的纳米PbO2/TiO2粉体颗粒分散较理想,粒径为100-150 nm;纳米TiO2掺杂PbO2电极的氧化峰电流密度为157 mA/cm2,氧化还原峰电位差明显减小,具有较高的电催化活性,催化合成己二酸的电流效率和产率分别为89.2%和97.4%.Precursor PbTi2 (OCH2CH2OH)12-x was synthesized by electrolysis of titanium and lead in glycol solution. Nano-crystalline PbO2/TiO2 powder was prepared by direct sol-gel method from the precursor and then calcined for 2 h at 450 ℃. The metal alkoxide was characterized by FT-IR and Raman spectra. The mono-disperse structure and the diameter of nano-PbO2/TiO2 were observed by XRD and SEM. The results show that PbO2/TiO2 of 100--150 nm was obtained. The highly active nano-PbO2/TiO2 electrode was prepared via electro-synthesis and sol-gel method. The cyclic voltammetry was used to study the redox behavior of the nano-PbO2/TiO2 electrode in HC1 4- OHC(CH2)4CHO solution. The current density of the electrode increased] obviously and reached to 157 mA/cm2. The electrode potential difference of the redox peaks decreased obviously. The PbO2/TiO2 electrode had the high electro-catalytic activities for the oxidation of OHC-(CH2)4CHO, and the average current efficiency and yield were 89.2% and 97.4% respectively.
关 键 词:电解 纳米PbO2/TiO2 电极 电催化 己二醛
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