Amination of Cyclohexane by Dielectric Barrier Discharge Processing in a Continuous Flow Microreactor: Experimental and
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Amination of Cyclohexane by Dielectric Barrier Discharge Processing in a Continuous Flow Microreactor: Experimental and Simulation Studies Aurélien Lepoetre1 · Stéphanie Ognier1 · Mengxue Zhang1 · Julien Wengler1 · Safwan Al Ayoubi1 · Cyril Ollivier2 · Louis Fensterbank2 · Xavier Duten3 · Michael Tatoulian1 Received: 7 August 2020 / Accepted: 2 November 2020 © Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract A miniaturized flow device has been developed to combine microfluidics technology and plasma process. In this microreactor, atmospheric pressure dielectric barrier discharges are generated in a gas in contact with a liquid phase. This study was conducted with plasma generated in ammonia in contact with a flow of liquid cyclohexane. Cyclohexylamine was synthesized with a good selectivity, and the process can be implemented to improve conversion and effectiveness. Numerical simulations confirmed that N H2 radicals are generated in the plasma and react with cyclohexyls radicals to achieve the reaction, giving a selectivity of 50% and a total molar conversion of 20% of cyclohexane. The effects of voltage and frequency on the selectivity and the experimental conversion rate were studied and discussed. Keywords Amination · Ammonia discharges · Dielectric barrier discharges (DBD) · Microreactor · Radicals · Flow chemistry
Electronic supplementary material The online version of this article (https://doi.org/10.1007/s1109 0-020-10140-9) contains supplementary material, which is available to authorized users. * Stéphanie Ognier [email protected] 1
Chimie ParisTech-PSL, PSL Université Paris, CNRS, Institut de Recherche de Chimie Paris, UMR 8247, 2PM Group, 11 rue Pierre et Marie Curie, 75005 Paris, France
2
MACO Group, Sorbonne Université, CNRS, Institut Parisien de Chimie Moléculaire, UMR 8232, 4 place Jussieu, 75005 Paris, France
3
LSPM – CNRS UPR 3407 – Université Sorbonne Paris Nord, 99 Avenue J.B. Clément, 93430 Villetaneuse, France
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Plasma Chemistry and Plasma Processing
Introduction Microplasmas have become a promising technique over the years, since the first ones created by G. Demhelt and W. Paul more than 30 years ago [1]. It was seen as a technique for the future, with a high potential in terms of good reactivity coupled with low energy consumption. Plasma generation in micro channels would control chemical reaction very accurately, while reducing energetic wastes to the minimum [1]. Plasmas are already used to graft chemical groups, generally on thin polymers films, or directly to create the thin polymer films [2–5]. Among the plasma parameters, the nature of the gas plasma is crucial to control the type of surface modification (i.e. etching, grafting, plasma deposition of organic/inorganic films). Nitrogen plasma jets in particular are often used to create amine function on thin polymer films [6], specially to improve specificities like water soaking or wettability, lifetime, or flexibility. However, they are not used
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