Rh/SiO2 catalysts prepared by the sol-gel method

C.K. Lambert, R.D. Gonzalez
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引用次数: 12

Abstract

A series of Rh/SiO2 catalysts were prepared by the sol-gel method. The precursors used were tetraethoxysilane (TEOS) dissolved in ethanol and rhodium(III) acetylacetonate dissolved in acetone. Preparative variables include the amount of water added to the sol and the gelation temperature. Typical BET surface areas were 550–700 m2 g−1 with very narrow pore size distributions centered at approximately 4 nm. Sample characterization studies were performed using TGA-DTA-MS to determine the effect of O2 pretreatment and 29Si solid-state NMR to determine the extent to which silica was condensed. Sintering studies of Rh/SiO2 catalysts for which there was a reasonable match between metal particle size and pore diameter were performed. Catalysts prepared by ion-exchange having comparable dispersions to those prepared by the sol-gel method also showed considerable resistance to sintering in O2. Following heat treatment in O2 at 650°C, the particle size distribution of catalysts prepared by ion-exchange appear to broaden to a greater extent than catalysts prepared by the sol-gel method. This suggests that the sol-gel preparation is more effective in retaining the metal particles within the narrow pores of the support.

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溶胶-凝胶法制备Rh/SiO2催化剂
采用溶胶-凝胶法制备了一系列Rh/SiO2催化剂。前体是溶解在乙醇中的四乙氧基硅烷(TEOS)和溶解在丙酮中的乙酰丙酮铑。制备变量包括添加到溶胶中的水量和凝胶温度。典型的BET表面积为550-700 m2 g−1,孔径分布非常窄,以约4 nm为中心。使用TGA-DTA-MS进行样品表征研究,以确定O2预处理的影响,使用29Si固态NMR来确定二氧化硅的浓缩程度。对金属粒度和孔径相匹配的Rh/SiO2催化剂进行了烧结研究。离子交换制备的催化剂与溶胶-凝胶法制备的催化剂具有相当的分散性,也表现出相当的抗O2烧结性能。在650℃O2中热处理后,离子交换法制备的催化剂的粒径分布比溶胶-凝胶法制备的催化剂更宽。这表明溶胶-凝胶制备更有效地将金属颗粒保留在支架的窄孔内。
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Author index Subject index Contents Investigation of organosilanes as structure-directing agents in zeolite synthesis The influence of gel properties on the kinetics of crystallization and particulate properties of MFI-type zeolities. I. The influence of time and temperature of gel ageing on the particulate properties of silicalite-1 microcrystals
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