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首页> 外文期刊>Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics >Structure and Catalytic Activity of Cr-Doped BaTiO3 Nanocatalysts Synthesized by Conventional Oxalate and Microwave Assisted Hydrothermal Methods
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Structure and Catalytic Activity of Cr-Doped BaTiO3 Nanocatalysts Synthesized by Conventional Oxalate and Microwave Assisted Hydrothermal Methods

机译:常规草酸盐-微波辅助水热法合成Cr掺杂BaTiO3纳米催化剂的结构和催化活性

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摘要

In the present study synthesis of BaTi1-xCrxO3 nanocatalysts (x = 0.0 <= x <= 0.05) by conventional oxalate and microwave assisted hydrothermal synthesis methods was carried out to investigate the effect of synthesis methods on the physicochemical and catalytic properties of nanocatalysts. These catalysts were thoroughly characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), N-2 physisortion, and total acidity by pyridine adsorption Method. Their catalytic performance was evaluated for the reduction of nitrobenzene using hydrazine hydrate as the hydrogen source. Structural parameters refined by Rietveld analysis using XRD powder data indicate that BaT1-xCrxO3 conventional catalysts were crystallized in the tetragonal BaTiO3 structure with space group P4mm, and microwave catalysts crystallized in pure cubic BaTiO3 structure with space group Pm (3) over barm. TEM analysis of the catalysts reveal spherical morphology of the particles, and these are uniformly dispersed in microwave catalysts whereas agglomeration of the particles was observed in conventional catalysts. Particle size of the microwave catalysts is found to be 20-35 nm compared to conventional catalysts (30-48 nm). XPS studies reveal that Cr is present in the 3+ and 6+ mixed valence state in all the catalysts. Microwave synthesized catalysts showed a 4-10-fold increase in surface area and, pore volume compared to conventional catalysts. Acidity of the BaTiO3 catalysts improved with Cr dopant in the catalysts, and this could be due to an increase in the number of Lewis acid sites with an increase in Cr content of all the catalysts. Catalytic reduction of nitrobenzene, to aniline studies reveals that BaTiO3 synthesized by microwave is very active and showed 99.3% nitrobenzene conversion:with 98.2% aniline yield. The presence of Cr in the catalysts facilitates a faster reduction reaction in, all the catalysts, and its effect is particularly notable in conventional synthesized catalysts.
机译:在本研究中,通过常规草酸盐和微波辅助水热合成方法合成了BaTi1-xCrxO3纳米催化剂(x = 0.0 <= x <= 0.05),以研究合成方法对纳米催化剂的物理化学和催化性能的影响。通过X射线衍射(XRD),傅里叶变换红外光谱(FT-IR),透射电子显微镜(TEM),X射线光电子能谱(XPS),N-2物理形态以及吡啶的总酸度对这些催化剂进行了全面表征吸附法。使用水合肼作为氢源,评估了它们的催化性能,以还原硝基苯。使用XRD粉末数据通过Rietveld分析精炼的结构参数表明,BaT1-xCrxO3常规催化剂在空间基团为P4mm的四方BaTiO3结构中结晶,而微波催化剂在棒状表面上以空间基团为Pm(3)的纯立方BaTiO3结构结晶。催化剂的TEM分析揭示了颗粒的球形形态,并且它们均匀地分散在微波催化剂中,而在常规催化剂中观察到颗粒的团聚。与常规催化剂(30-48nm)相比,发现微波催化剂的粒度为20-35nm。 XPS研究表明,在所有催化剂中,Cr以3+和6+混合价态存在。与常规催化剂相比,微波合成的催化剂显示出表面积和孔体积增加了4-10倍。通过在催化剂中添加Cr掺杂剂,BaTiO3催化剂的酸度得以提高,这可能是由于路易斯酸位点数量的增加以及所有催化剂中Cr含量的增加所致。硝基苯催化还原为苯胺的研究表明,微波合成的BaTiO3活性很高,硝基苯转化率为99.3%:苯胺收率为98.2%。催化剂中Cr的存在促进了所有催化剂中更快的还原反应,并且其效果在常规合成催化剂中特别显着。

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