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In situ IR spectroscopic study to reveal the impact of the synthesis conditions of zeolite β nanoparticles on the acidic properties of the resulting zeolite

机译:原位红外光谱研究揭示了沸石β纳米粒子的合成条件对所得沸石酸性的影响

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摘要

Zeolite p has been synthesised by hydrothermally ageing zeolite p nanoparticles. The influence of a small variation in the synthesis conditions of the zeolite nanoparticles solution, i.e. a hydrothermal synthesis temperature of 373 K versus 423 K, on the structural and acidic properties is examined. The structural characteristics, as determined via N2-sorption, DRIFT, XRD and SEM, do not show clear discrepancies: However, an extensive study of the aluminium coordination (~(27)Al MAS NMR) and the acidic characteristics (in situ FT-IR with NH3 and CO as probe) reveal a difference between the two nanoparticles based zeolites. Although both zeolites exhibit a similar total acid site concentration, a clear impact of the synthesis temperature on the protonic bridging hydroxyls (Si(OH)Al) concentration has been detected. Hence, even though both nanoparticles solutions have been submitted to a further hydrothermal synthesis period of several days, the differences induced by the variation in temperature during the formation of the nanoparticles (first 24 h) remain in the final structure. This knowledge not only allows the tailoring of the material characteristics of the full-grown zeolites, but also reveals important aspects to be taken into account in f.e. the up-scaling of zeolite synthesis for catalytic applications, in which the acidity characteristics play a key role.
机译:通过水热老化沸石p纳米颗粒来合成沸石p。研究了沸石纳米颗粒溶液的合成条件的小变化,即373 K对423 K的水热合成温度,对结构和酸性的影响。通过N2吸附,DRIFT,XRD和SEM确定的结构特征没有显示明显的差异:但是,对铝的配位(〜(27)Al MAS NMR)和酸性特征(原位FT-以NH3和CO为探针的IR揭示了两种基于纳米颗粒的沸石之间的差异。尽管两种沸石都具有相似的总酸位点浓度,但已检测到合成温度对质子桥联羟基(Si(OH)Al)浓度的明显影响。因此,即使两种纳米颗粒溶液都已经经历了几天的进一步水热合成阶段,由纳米颗粒形成过程中(最初的24小时)温度变化所引起的差异仍保留在最终结构中。这种知识不仅可以定制成年沸石的材料特性,而且还揭示了在成型工艺中要考虑的重要方面。催化应用中合成沸石的规模扩大,其中酸性特征起着关键作用。

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