Chemical Process Engineering (CVT), Faculty of Production Engineering (FB 4), University of Bremen, Leobener Straße 6, 28359 Bremen, Germany.
Faculty of Chemistry (FB 2), Institute of Applied Physical and Chemistry (IAPC), University of Bremen, Leobener Straße 6, 28359 Bremen, Germany.
Rev Sci Instrum. 2021 Apr 1;92(4):043711. doi: 10.1063/5.0044795.
Recently, in situ studies using nuclear magnetic resonance (NMR) have shown the possibility to monitor local transport phenomena of gas-phase reactions inside opaque structures. Their application to heterogeneously catalyzed reactions remains challenging due to inherent temperature and pressure constraints. In this work, an NMR-compatible reactor was designed, manufactured, and tested, which can endure high temperatures and increased pressure. In temperature and pressure tests, the reactor withstood pressures up to 28 bars at room temperature and temperatures over 400 °C and exhibited only little magnetic shielding. Its applicability was demonstrated by performing the CO methanation reaction, which was measured operando for the first time by using a 3D magnetic resonance spectroscopic imaging sequence. The reactor design is described in detail, allowing its easy adaptation for different chemical reactions and other NMR measurements under challenging conditions.
最近,使用核磁共振(NMR)的原位研究表明有可能监测不透明结构内气相反应的局部传输现象。由于固有的温度和压力限制,它们在多相催化反应中的应用仍然具有挑战性。在这项工作中,设计、制造和测试了一种 NMR 兼容的反应器,该反应器能够承受高温和高压。在温度和压力测试中,该反应器在室温下可承受高达 28 巴的压力,在 400°C 以上的温度下可承受压力,并且仅表现出很小的磁屏蔽。通过进行 CO 甲烷化反应证明了其适用性,这是首次使用 3D 磁共振波谱成像序列对其进行原位测量。详细描述了该反应器的设计,允许其在具有挑战性的条件下轻松适应不同的化学反应和其他 NMR 测量。