Research output: Contribution to journal › Article › peer-review
In-Line NMR Diagnostics of Hydroformylation Provided by the Segmented-Flow Microfluidic Regime. / Eid, Mahmoud E.A.; Nenasheva, Maria V.; Bulgakov, Aleksei N. et al.
In: Analytical Chemistry, Vol. 97, No. 50, 23.12.2025, p. 27879-27884.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - In-Line NMR Diagnostics of Hydroformylation Provided by the Segmented-Flow Microfluidic Regime
AU - Eid, Mahmoud E.A.
AU - Nenasheva, Maria V.
AU - Bulgakov, Aleksei N.
AU - Soldatov, Alexander V.
AU - Burueva, Dudari B.
AU - Kononenko, Elizaveta S.
AU - Skovpin, Ivan V.
AU - Koptyug, Igor V.
AU - Gorbunov, Dmitry N.
AU - Guda, Alexander A.
N1 - AAG, DNG, and MEA acknowledge financial support from the Russian Science Foundation (project RSF no. 25-12-00424) for developing the microfluidic setup and performing experiments. DBB, IVS, and IVK thank the Russian Ministry of Science and Higher Education for access to NMR equipment. ESK and IVK acknowledge the Russian Science Foundation for the support of NMR experiments (grant no. 25-13-00053).
PY - 2025/12/23
Y1 - 2025/12/23
N2 - Hydroformylation is an industrial method for the conversion of olefins to aldehydes, which are further transformed to other valuable products, including primary alcohols. In industry, it is catalyzed by Rh and Co complexes, mostly under homogeneous catalysis conditions and in batch mode. The microfluidic regime offers improved mass and heat transfer efficiency due to a large gas–liquid interfacial area in the segmented-flow regime that accelerates conversion and shows increased yields of the products. However, the existing in situ spectroscopic characterization methods either lack sensitivity or require complex preparation steps to separate signals from olefin isomers, aldehydes, and other products formed in the reaction mixture. We employed 1H NMR spectroscopy for fast in-line monitoring of hydroformylation products directly within the segmented flow. This approach avoids the replacement of organic solvents by expensive deuterated analogues as well as sample probing and preparation for ex situ NMR spectroscopy. Our work opens wide perspectives for screening and optimization of hydroformylation under microfluidic conditions.
AB - Hydroformylation is an industrial method for the conversion of olefins to aldehydes, which are further transformed to other valuable products, including primary alcohols. In industry, it is catalyzed by Rh and Co complexes, mostly under homogeneous catalysis conditions and in batch mode. The microfluidic regime offers improved mass and heat transfer efficiency due to a large gas–liquid interfacial area in the segmented-flow regime that accelerates conversion and shows increased yields of the products. However, the existing in situ spectroscopic characterization methods either lack sensitivity or require complex preparation steps to separate signals from olefin isomers, aldehydes, and other products formed in the reaction mixture. We employed 1H NMR spectroscopy for fast in-line monitoring of hydroformylation products directly within the segmented flow. This approach avoids the replacement of organic solvents by expensive deuterated analogues as well as sample probing and preparation for ex situ NMR spectroscopy. Our work opens wide perspectives for screening and optimization of hydroformylation under microfluidic conditions.
UR - https://www.scopus.com/pages/publications/105025210663
UR - https://www.mendeley.com/catalogue/0ff3daf9-fa83-340e-8492-988eb3edefa6/
U2 - 10.1021/acs.analchem.5c05154
DO - 10.1021/acs.analchem.5c05154
M3 - Article
C2 - 41391006
VL - 97
SP - 27879
EP - 27884
JO - Analytical Chemistry
JF - Analytical Chemistry
SN - 0003-2700
IS - 50
ER -
ID: 73871893