NMR of petrochemical-type chemical reactions

• Published in: Journal of magnetic resonance (1997) 2020-02, Vol.311, p.106665-106665, Article 106665
• Main Authors: Fabich, Hilary T., Nandi, Partha, Thomann, Hans, Altobelli, Stephen A., Bunnelle, William, Conradi, Mark S.
• Format: Article
• Language: English
• Subjects: Chemical species; High pressure; High temperature; Hydrogenation; Methanol synthesis; Reaction; Refinery reactions
• ISSN: 1090-7807; 1096-0856
• DOI: 10.1016/j.jmr.2019.106665

[Display omitted] •We report a simple technique for monitoring chemical reactions at high temperature and pressure with NMR.•Our technique uses a simple sealed glass capillary sample holder.•We report several reactions that have been monitored. A simple technique is presented for NMR of chemically reacting systems at conditions of high temperature and pressure. The method can follow reactions that are typical of refinery operations – hydrogenation, transfer dehydrogenation, methanol synthesis, and isomerization. All of the reacting materials are flame-sealed into a glass capillary. Gaseous agents such as O2 and CO are loaded into the capillary by condensation at liquid N2 temperature. H2 is provided by loading LiAlH4. The capillary holds the high pressure, up to 7 MPa, so the NMR probe can be a simple design with hot air flowing over the sample tube, up to 350 °C. Example reaction results are presented, including hydrogenation of benzene, hydrogenation/dehydrogenation of cyclohexene to benzene and cyclohexane (a disproportionation), and synthesis of methane, methanol and dimethyl ether from CO and H2. In this work we present a simple, inexpensive method with rapid temperature response for tracking chemical reactions in real-time at high temperature and high pressure.