Control of Hazardous Processes in Flow: Synthesis of 2-Nitroethanol

• Published in: Journal of flow chemistry Vol. 4; no. 1; pp. 26 - 34
• Main Authors: Roberge, Dominique M., Noti, Christian, Irle, Eberhard, Eyholzer, Markus, Rittiner, Bruno, Penn, Gerhard, Sedelmeier, Gottfried, Schenkel, Berthold
• Format: Journal Article
• Language: English
• Published: Cham Springer International Publishing 2014
• Subjects: Chemistry; Chemistry and Materials Science; Chemistry/Food Science; Green Chemistry; Industrial Chemistry/Chemical Engineering; Inorganic Chemistry; Nanochemistry; Organic Chemistry; continuous flow; hazardous chemistry; formaldehyde; energetic compound; 2-nitroethanol; paraformaldehyde; microreactor technology; nitromethane; Henry reaction
• ISSN: 2062-249X; 2063-0212
• DOI: 10.1556/JFC-D-13-00016

After a short section of safety aspects related to 2-nitroethanol, the paper describes a powerful methodology for developing flow processes based on a proof of concept (1), an optimization and modeling analysis (2), and a long run study in a mini-plant (3). The proof of concept is the initial stage where the solubilities and concentrations are fixed, taking into account the rough kinetics with a mass transfer understanding. It is followed by a complete kinetic analysis including activation energy to model the reaction under various conditions to optimize different targets (yield not being the only driver!). The last section shows the operation of a mini-plant including a microreactor and work-up unit operations. The approach is extremely powerful as it enables the study at laboratory scale of all the features that are usually associated with a pilot plant namely: stability over time on stream, solvent recirculation, model prediction, and robustness.