微波辅助溶剂热合成的各种参数对MgF纳米颗粒比表面积和催化性能的影响
The Effects of Various Parameters of the Microwave-Assisted Solvothermal Synthesis on the Specific Surface Area and Catalytic Performance of MgF Nanoparticles.
作者信息
Wang Yawen, Bajestani Zahra Gohari, Lhoste Jérôme, Auguste Sandy, Hémon-Ribaud Annie, Body Monique, Legein Christophe, Maisonneuve Vincent, Guiet Amandine, Brunet Sylvette
机构信息
Institut de Chimie et Matériaux de Poitiers UMR 7285, University of Poitiers, Cedex 9, 86073 Poitiers, France .
Institut des Molécules et Matériaux du Mans (IMMM), UMR 6283 CNRS, Le Mans Université, Cedex 9, 72085 Le Mans, France.
出版信息
Materials (Basel). 2020 Aug 12;13(16):3566. doi: 10.3390/ma13163566.
High-specific-surface-area MgF was prepared by microwave-assisted solvothermal synthesis. The influences of the solvent and the magnesium precursors, and the calcination atmospheres, on the nanoparticle sizes and specific surface areas, estimated by X-Ray Powder Diffraction, N sorption and TEM analyses, were investigated. Nanocrystallized (~7 nm) magnesium partially hydroxylated fluorides (MgF(OH)) with significant specific surface areas between 290 and 330 m∙g were obtained. After activation under gaseous HF, MgF(OH) catalysts underwent a large decrease of both their surface area and their hydroxide, rates as shown by their F and H solid-state NMR spectra. Expect for MgF prepared from the acetate precursor, an activity of 30-32 mmol/h∙g was obtained which was about 40% higher compared with that of MgF prepared using Trifluoroacetate method (21.6 mmol/h∙g).
通过微波辅助溶剂热合成法制备了高比表面积的MgF。通过X射线粉末衍射、N吸附和透射电子显微镜分析，研究了溶剂、镁前驱体以及煅烧气氛对纳米颗粒尺寸和比表面积的影响。获得了纳米晶化（约7nm）的部分羟基化氟化镁（MgF(OH)），其比表面积在290至330m²/g之间。在气态HF下活化后，MgF(OH)催化剂的表面积和氢氧化物含量均大幅下降，其F和H固态核磁共振光谱表明了这一点。除了由乙酸盐前驱体制备的MgF外，获得了30-32 mmol/h∙g的活性，与使用三氟乙酸盐法制备的MgF（21.6 mmol/h∙g）相比，活性提高了约40%。
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