Synthesis of Al – Fe/SiO2 and Al – Co/SiO2 catalysts by solid-phase method

V. Artyukh, V. Borshch, V. Yusupov, S. Zhuk, V. Zelensky, B. Belelyubsky
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Abstract

Powders of catalysts from aluminides Fe and Co on a SiO2 support (33.3 wt. %) were obtained by mechano-thermal synthesis. The formation of large powder fractions (> 100 μm) was experimentally established. The fractions of these fractions for Fe – Al – SiO2 and Co – Al – SiO2 respectively amounted to ~ 43 % and ~ 55 %, which is a positive result for further catalytic studies. After annealing the powders at 700 and 900 °C in vacuum, the SiO2 support and compounds: Co27Al73 (close in composition to CoAl3, Co4Al13 type intermetallic compounds), Fe3Al intermetallic compound with iron silicide type Fe0.9Si0.1 and compound Al0,3Fe3Si0.7 in small volumes. On the synthesis of cobalt aluminides, a conclusion has been made about more efficient annealing at 900 °C than at 700 °C. For Fe – Al – SiO2 powders, it is advisable to anneal in the temperature range 700 – 750 °C with the assumption that the SiO2 support influences the thermosynthesis of iron aluminides. An experimental analysis of the morphology and elemental composition of the surface of the obtained samples is presented. It was found that the catalyst powders have medium sphericity and angularity. Fe – Al – SiO2 powders have a more developed surface than Co – Al – SiO2. Lower intermetallics are predominantly formed on the surface of the Co – Al – SiO2 sample. The correction of the mechanical alloying modes by means of the fragmentation of the process, changes in the intensity of its parameters, and various annealing conditions for Co – Al – SiO2 and Fe – Al – SiO2 are proposed.
固相法合成Al - Fe/SiO2和Al - Co/SiO2催化剂
采用机械-热合成的方法,在SiO2载体(33.3% wt. %)上制备了Fe和Co铝化物催化剂粉末。实验结果表明,该材料可形成较大的粉末组分(> 100 μm)。这些馏分中Fe - Al - SiO2和Co - Al - SiO2的馏分分别达到~ 43%和~ 55%,为进一步的催化研究提供了积极的结果。粉末在700°C和900°C真空退火后,小体积的SiO2支持物和化合物:Co27Al73(成分接近于CoAl3, Co4Al13型金属间化合物),Fe3Al与硅化铁的金属间化合物Fe0.9Si0.1和化合物Al0,3Fe3Si0.7。在合成钴铝化物时,900℃退火比700℃退火更有效。对于Fe - Al - SiO2粉末,假设SiO2载体影响铁铝化物的热合成,建议在700 - 750℃的温度范围内退火。对所得样品的表面形貌和元素组成进行了实验分析。结果表明,该催化剂粉末具有中等的球形度和角度。Fe - Al - SiO2粉体比Co - Al - SiO2粉体具有更发达的表面。低金属间化合物主要形成于Co - Al - SiO2样品表面。提出了Co - Al - SiO2和Fe - Al - SiO2机械合金化过程的破碎化、参数强度的变化以及不同退火条件对机械合金化模式的修正。
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