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Ultrasound-Assisted Hydrazine Reduction Method for the Preparation of Nickel Nanoparticles Physicochemical Characterization and Catalytic Application in Suzuki-Miyaura Cross-Coupling Reaction

机译:超声辅助肼还原法制备镍纳米粒子的理化表征及其在铃木宫浦交叉偶联反应中的催化应用

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摘要

In the experimental work leading to this contribution, the parameters of the ultrasound treatment (temperature, output power, emission periodicity) were varied to learn about the effects of the sonication on the crystallization of Ni nanoparticles during the hydrazine reduction technique. The solids were studied in detail by X-ray diffractometry, dynamic light scattering, thermogravimetry, specific surface area, pore size analysis, temperature-programmed CO /NH desorption and scanning electron microscopy. It was found that the thermal behaviour, specific surface area, total pore volume and the acid-base character of the solids were mainly determined by the amount of the nickel hydroxide residues. The highest total acidity was recorded over the solid under low-power (30 W) continuous ultrasonic treatment. The catalytic behaviour of the nanoparticles was tested in a Suzuki-Miyaura cross-coupling reaction over five samples prepared in the conventional as well as the ultrasonic ways. The ultrasonically prepared catalysts usually performed better, and the highest catalytic activity was measured over the nanoparticles prepared under low-power (30 W) continuous sonication.
机译:在做出这一贡献的实验工作中,改变了超声处理的参数(温度,输出功率,发射周期),以了解在肼还原技术中超声处理对镍纳米颗粒结晶的影响。通过X射线衍射,动态光散射,热重分析,比表面积,孔径分析,程序升温的CO / NH解吸和扫描电子显微镜对固体进行了详细研究。发现固体的热行为,比表面积,总孔体积和酸碱特性主要由氢氧化镍残余物的量决定。在低功率(30 W)连续超声处理下,固体上的总酸度最高。在Suzuki-Miyaura交叉偶联反应中,以常规方法和超声方法对五个样品进行了测试,测试了纳米颗粒的催化行为。超声制备的催化剂通常表现更好,在低功率(30 W)连续超声处理下制备的纳米颗粒上,催化活性最高。

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