Study on the Transport Phenomena in Complex Micro-Reactors

Title: Study on the Transport Phenomena in Complex Micro-Reactors
Authors: Mielke, Eric
Date: 2017
Abstract: Continuous processing in the pharmaceutical and fine chemical industries, particularly in micro/milli-scale reactors, has been a topic of interest in literature in recent years due to the advantages offered over batch reactions. One such advantage is the enhanced transport properties of operating at smaller scales, although the quantification of the transport phenomena is not straightforward when wall and entrance effects cannot be neglected. In the first study presented, various micro-mixer geometries and scales were considered to increase the mixing efficiency in liquid-liquid systems of diverse interfacial tensions for fast reactions. The conditions were varied over different flow regimes; including slug flow, parallel flow, and drop flow. A mass-transfer-limited test reaction was used to evaluate the overall volumetric mass transfer coefficients (Korga) as a function of the average rate of energy dissipation (ε) for each mixer design. The onset of drop flow occurred at a lower ε for the LL-Triangle mixer when compared with the Sickle or LL-Rhombus mixers for low interfacial-tension systems (i.e., n-butanol-water). In the drop flow regime for energy dissipation rates of around 20 to 500 W/kg, Korga values ranged from approximatively 0.14 to 0.35 s-1 and 0.004 to 0.015 s-1 for the relatively low and high interfacial-tension (i.e., toluene-water) systems, respectively. The second investigation explored the heat transfer properties of a FlowPlate® system by Ehrfeld Mikrotechnik BTS. First, in a non-reactive system with rectangular serpentine channels (d_h<1mm, 400<Re<2000), a Gnielinski-type model was fit to the internal Nusselt number. Using a silver-based thermal paste between the reactor and heat transfer fluid plates proved to reduce the external resistance to heat transfer by ~70%, yielding overall heat transfer coefficients of ~2200 [W/(m^2 K)]. Secondly, a Grignard reaction was highlighted as a test reaction to compare different reactors’ localized heat transfer characteristics (i.e., hotspot formation) with various micro-mixer geometries, materials, injection ports, and channel scales. Lastly, a case study of four reactions utilized the fourth Damköhler number to determine a maximum channel diameter that would remove sufficient heat to avoid hotspot formation. Each of these studies provides insight to aid in the proper selection of a reactor for a given set of physical properties and reaction kinetics/enthalpies.
CollectionThèses, 2011 - // Theses, 2011 -