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Dry impregnation in fluidized bed: Drying and calcination effect on nanoparticles dispersion and location in a porous support

机译:流化床中的干浸渍:干燥和煅烧对纳米颗粒分散和在多孔载体中的位置的影响

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摘要

The synthesis of metal nanoparticles dispersed inside the grains of a porous inorganic support was carried out by ‘‘dry impregnation’’ in a fluidized bed. The principle of this technique consists in the spraying of a solution containing a metal source into a hot fluidized bed of porous particles. The metal source can be of different nature such as metal salts, organometallic precursors or colloidal solutions. The experimental results obtained from iron oxide deposition on a porous silica gel as support, constitute the core of this article but others results concerning the deposition of rhodium from a colloidal suspension containing preformed rhodium nanoparticles are also described. More precisely, this study aims to understand the effect of the bed temperature during the impregnation step, the initial particle porosity and the calcination operating protocol on the metallic nanoparticles dispersion and location in the silica porous particles. The so-obtained products were characterized by various techniques in order to determine their morphology, their surface properties and the dispersion of the nanoparticles inside the support. The results showed that, under the chosen operating conditions, the deposit efficiency is close to 100% and the competition between the drying rate, depending on the process-related variables, and the capillary penetration rate, depending on the physicochemical-related variables, controls the deposit location. A quasi uniform deposit inside the support particles is observed for soft drying. The metal nanoparticles size is controlled by the pore mean diameter of the support as well as the calcination operating protocol.
机译:分散在多孔无机载体颗粒内部的金属纳米颗粒的合成是通过在流化床中进行“干浸渍”来进行的。该技术的原理在于将包含金属源的溶液喷涂到多孔颗粒的热流化床中。金属源可以具有不同的性质,例如金属盐,有机金属前体或胶体溶液。从氧化铁沉积在作为载体的多孔硅胶上获得的实验结果构成了本文的核心,但同时也描述了其他有关从含预制铑纳米粒子的胶体悬浮液中沉积铑的结果。更准确地说,本研究旨在了解浸渍步骤中床温,初始颗粒孔隙率和煅烧操作规程对金属纳米颗粒在二氧化硅多孔颗粒中的分散和位置的影响。通过各种技术对如此获得的产物进行表征,以确定其形态,表面性质以及纳米颗粒在载体内的分散性。结果表明,在所选的操作条件下,沉积效率接近100%,取决于工艺相关变量的干燥速率与取决于理化相关变量的毛细管渗透速率之间的竞争存款地点。观察到在载体颗粒内部的准均匀沉积,以进行软干燥。金属纳米粒子的大小由载体的平均孔径以及煅烧操作规程控制。

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