On-line polymerisation monitoring in scCO2: a reliable and inexpensive sampling method in high pressure applications

Kortsen, Kristoffer; Pacheco, Ana A.C.; Lentz, Joachim C; Taresco, Vincenzo; Howdle, Steven M.

Abstract

A versatile and reliable on-line sampling system for polymerisation reactions in supercritical fluids was developed. By withdrawing a small volume of a high-pressure reaction mixture and expanding it in a controlled volume, reliable kinetic data were obtained for a range of reactions in scCO2, avoiding the need for costly equipment or setup modifications. All experiments were carried out in a stainless-steel high-pressure autoclave with mechanical stirring and a volume of 60 ml. With the polymerisation of methyl methacrylate (MMA) in scCO2 being widely adopted for research in the past, the free-radical and RAFT controlled dispersion polymerisations of MMA were analysed in detail using the sampling system as a proof-of-concept. Additionally, initial implementation of the sampling system to a range of different reactions showed the facile applicability of the monitoring method.

Citation

Kortsen, K., Pacheco, A. A., Lentz, J. C., Taresco, V., & Howdle, S. M. (2021). On-line polymerisation monitoring in scCO2: a reliable and inexpensive sampling method in high pressure applications. Journal of Supercritical Fluids, 167, Article 105047. https://doi.org/10.1016/j.supflu.2020.105047

• Journal Article Type: Article
• Acceptance Date: Sep 14, 2020
• Online Publication Date: Sep 19, 2020
• Publication Date: Jan 1, 2021
• Deposit Date: Sep 24, 2020
• Publicly Available Date: Sep 20, 2021
• Journal: The Journal of Supercritical Fluids
• Print ISSN: 0896-8446
• Publisher: Elsevier
• Peer Reviewed: Peer Reviewed
• Volume: 167
• Article Number: 105047
• DOI: https://doi.org/10.1016/j.supflu.2020.105047
• Keywords: Physical and Theoretical Chemistry; General Chemical Engineering; Condensed Matter Physics
• Public URL: https://nottingham-repository.worktribe.com/output/4922657
• Publisher URL: https://www.sciencedirect.com/science/article/abs/pii/S0896844620302989