TY - JOUR
T1 - Monitoring Heterogeneously Catalyzed Hydrogenation Reactions at Elevated Pressures Using In-Line Flow NMR
AU - Tijssen, Koen C.H.
AU - Van Weerdenburg, Bram J.A.
AU - Zhang, Hainan
AU - Janssen, J. W.G.
AU - Feiters, Martin C.
AU - Van Bentum, P. Jan M.
AU - Kentgens, Arno P.M.
N1 - Funding Information:
We thank Renée Ripken and Robin Burgers for their contributions in the early stages of this project, Professor Floris Rutjes (Radboud University Nijmegen) and Professor Han Gardeniers (Twente University) for discussions, and the staff of Future Chemistry for their help with the experimental setup. We also acknowledge the technical support provided by Gerrit Janssen and Ruud Aspers. We thank The Netherlands Organization for Scientific Research (NWO) and the Institute for Molecules and Materials for their support of the NMR facility. We are grateful to the European Union and the provinces of Gelderland and Overijssel for their support of the EFRO (Europees Fonds voor Regionale Ontwikkeling) Ultrasense NMR project.
Publisher Copyright:
© 2019 American Chemical Society.
PY - 2019/10/15
Y1 - 2019/10/15
N2 - 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.
AB - 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.
UR - http://www.scopus.com/inward/record.url?scp=85073097698&partnerID=8YFLogxK
U2 - 10.1021/acs.analchem.9b00895
DO - 10.1021/acs.analchem.9b00895
M3 - Article
C2 - 31508941
AN - SCOPUS:85073097698
SN - 0003-2700
VL - 91
SP - 12636
EP - 12643
JO - Analytical chemistry
JF - Analytical chemistry
IS - 20
ER -