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Influence of Calcination Conditions on Structural and Solid-State Kinetic Properties of Iron Oxidic Species Supported on SBA-15.
ChemistryOpen ( IF 2.3 ) Pub Date : 2019-10-17 , DOI: 10.1002/open.201900236
Nina Sharmen Genz 1 , Thorsten Ressler 1
Affiliation  

Iron oxidic species supported on silica SBA‐15 were synthesized with various iron loadings using two different FeIII precursors. The effect of varying powder layer thickness during calcination on structural and solid‐state kinetic properties of FexOy/SBA‐15 samples was investigated. Calcination was conducted in thin (0.3 cm) or thick (1.3 cm) powder layer. Structural characterization of resulting FexOy/SBA‐15 samples was performed by nitrogen physisorption, X‐ray diffraction, and DR‐UV/Vis spectroscopy. Thick powder layer during calcination induced an increased species size independent of the precursor. However, a significantly more pronounced influence of calcination mode on species size was observed for the FeIII nitrate precursor compared to the FeIII citrate precursor. Temperature‐programmed reduction (TPR) experiments revealed distinct differences in reducibility and reduction mechanism dependent on calcination mode. Thick layer calcination of the samples obtained from FeIII nitrate precursor resulted in more pronounced changes in TPR profiles compared to samples obtained from FeIII citrate precursor. TPR traces were analyzed by model‐dependent Coats‐Redfern method and model‐independent Kissinger method. Differences in solid‐state kinetic properties of FexOy/SBA‐15 samples dependent on powder layer thickness during calcination correlated with differences in iron oxidic species size.

中文翻译:

煅烧条件对 SBA-15 负载的氧化铁物质的结构和固态动力学性质的影响。

使用两种不同的 Fe III前体合成了具有不同铁负载量的二氧化硅 SBA-15 负载的氧化铁物质。研究了煅烧过程中不同粉末层厚度对 Fe x O y /SBA-15 样品的结构和固态动力学性质的影响。煅烧在薄(0.3 cm)或厚(1.3 cm)粉末层中进行。通过氮物理吸附、X 射线衍射和 DR-UV/Vis 光谱对所得 Fe x O y /SBA-15 样品进行结构表征。煅烧过程中厚的粉末层导致物质尺寸增加,与前体无关。然而,与柠檬酸三价铁前体相比,硝酸价铁前体的煅烧模式对物质尺寸的影响明显更显着。程序升温还原(TPR)实验揭示了取决于煅烧模式的还原性和还原机制的明显差异。与从柠檬酸三价铁前体获得的样品相比,从硝酸价铁前体获得的样品的厚层煅烧导致 TPR 曲线发生更显着的变化。TPR 迹线通过模型相关的 Coats-Redfern 方法和模型无关的 Kissinger 方法进行分析。Fe x O y /SBA-15 样品的固态动力学特性的差异取决于煅烧过程中粉末层的厚度,并且与氧化铁物质尺寸的差异相关。
更新日期:2019-10-17
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