Monitoring Heterogeneously Catalyzed Hydrogenation Reactions at Elevated Pressures Using In-Line Flow NMR

We present a novel setup that can be used for the in-line monitoring of solid-catalyzed gas–liquid reactions. The method combines the high sensitivity and resolution of a stripline NMR detector with a microfluidic network that can withstand elevated pressures. In our setup we dissolve hydrogen gas i...

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Bibliographic Details
Published in:Analytical chemistry (Washington) 2019-10, Vol.91 (20), p.12636-12643
Main Authors: Tijssen, Koen C. H, van Weerdenburg, Bram J. A, Zhang, Hainan, Janssen, J. W. G, Feiters, Martin C, van Bentum, P. Jan M, Kentgens, Arno P. M
Format: Article
Language:English
Subjects:
Analytical chemistry
Cartridges
Catalysts
Chemical reactions
Chemistry
Cyclohexene
Gas-liquid reactions
Hydrogen storage
Hydrogenation
Microfluidics
Monitoring
NMR
Nuclear magnetic resonance
Optimization
Phenylacetylene
Reaction kinetics
Styrene
Substrates
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Summary:We present a novel setup that can be used for the in-line monitoring of solid-catalyzed gas–liquid reactions. The method combines the high sensitivity and resolution of a stripline NMR detector with a microfluidic network that can withstand elevated pressures. In our setup we dissolve hydrogen gas in the solvent, then flow it with the added substrate through a catalyst cartridge, and finally flow the reaction mixture directly through the stripline NMR detector. The method is quantitative and can be used to determine the solubility of hydrogen gas in liquids; it allows in-line monitoring of hydrogenation reactions and can be used to determine the reaction kinetics of these reactions. In this work, as proof of concept we demonstrate the optimization of the Pd-catalyzed hydrogenation reactions of styrene, phenylacetylene, cyclohexene, and hex-5-en-2-one in a microfluidic context.
ISSN:0003-2700
1520-6882
DOI:10.1021/acs.analchem.9b00895