A novel nuclear magnetic resonance (NMR) probe head for monitoring fast chemical reactions is described. It combines micro-reaction technology with capillary flow NMR spectroscopy. Two reactants are fed separately into the probe head where they are effectively mixed in a micro-mixer. The mixed reactants then pass through a capillary NMR flow cell that is equipped with a solenoidal radiofrequency coil where the NMR signal is acquired. The whole flow path of the reactants is thermostatted using the liquid FC-43 (perfluorotributylamine) so that exothermic and endothermic reactions can be studied under almost isothermal conditions. The set-up enables kinetic investigation of reactions with time constants of only a few seconds. Non-reactive mixing experiments carried out with the new probe head demonstrate that it facilitates the acquisition of constant highly resolved NMR signals suitable for quantification of different species in technical mixtures. Reaction kinetic measurements on a test system are presented that prove the applicability of the novel NMR probe head for monitoring fast reactions.

Chemie Ingenieur TechnikVolume 84, Issue 8 p. 1365-1365 VortragFree Access Untersuchung schneller Reaktionskinetiken durch Kopplung von Mikro-Reaktionstechnologie und Online-NMR-Spektroskopie A. Brächer, Corresponding Author A. Brächer alexander.braecher@mv.uni-kl.de TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanyTU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorS. Hoch, S. Hoch TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorE. von Harbou, E. von Harbou TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorB. Werner, B. Werner Institut für Mikrotechnik, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorK. Albert, K. Albert Eberhard-Karls-Universität Tübingen, Institut für Organische Chemie, Auf der Morgenstelle 18, D-72076 Tübingen, GermanySearch for more papers by this authorH. Hasse, H. Hasse TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this author A. Brächer, Corresponding Author A. Brächer alexander.braecher@mv.uni-kl.de TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanyTU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorS. Hoch, S. Hoch TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorE. von Harbou, E. von Harbou TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this authorB. Werner, B. Werner Institut für Mikrotechnik, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorK. Albert, K. Albert Eberhard-Karls-Universität Tübingen, Institut für Organische Chemie, Auf der Morgenstelle 18, D-72076 Tübingen, GermanySearch for more papers by this authorH. Hasse, H. Hasse TU Kaiserslautern, Lehrstuhl für Thermodynamik, Erwin-Schrödinger-Straße 44, D-67663 Kaiserslautern, GermanySearch for more papers by this author First published: 25 July 2012 https://doi.org/10.1002/cite.201250044AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat No abstract is available for this article. Volume84, Issue8Special Issue: ProcessNet-Jahrestagung 2012 und 30. Jahrestagung der BiotechnologenAugust, 2012Pages 1365-1365 ReferencesRelatedInformation

Chemie Ingenieur TechnikVolume 82, Issue 9 p. 1589-1590 PosterFree Access Ringspalt-Elektrochromatographie als kontinuierliche Reinigungsmethode für die API-Produktion B. Werner Dr., B. Werner Dr. werner@imm-mainz.de Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorC. Hofmann, C. Hofmann Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorG. Menges Dr., G. Menges Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorP. Löb Dr., P. Löb Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorV. Hessel Dr., V. Hessel Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this author B. Werner Dr., B. Werner Dr. werner@imm-mainz.de Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorC. Hofmann, C. Hofmann Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorG. Menges Dr., G. Menges Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorP. Löb Dr., P. Löb Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this authorV. Hessel Dr., V. Hessel Dr. Institut für Mikrotechnik GmbH, Carl-Zeiss-Straße 18 – 20, D-55129 Mainz, GermanySearch for more papers by this author First published: 27 August 2010 https://doi.org/10.1002/cite.201050167Citations: 1AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article.Citing Literature Volume82, Issue9Special Issue: ProcessNet-Jahrestagung 2010 und 28. Jahrestagung der BiotechnologenSeptember, 2010Pages 1589-1590 RelatedInformation

The performance of the microstructured mixer Star-Laminator300 (StarLam300) with stacked star-shaped foils has been examined experimentally by the use of the adapted Villermaux/Dushman parallel-competitive iodide-iodate reaction system in continuous processes. The mixing efficiency was quantitatively determined by the segregation index derived from the UV absorption. The mixing performance of the microstructured mixer is analysed in terms of the total volume flow and turbulent energy dissipation rate. The influence of the geometry of the injection nozzles and the mixing chamber and the variation of foil number is also presented and discussed. The latter touches upon the numbering-up concept of microstructured devices. Since mixing efficiencies much better as for conventional equipment at throughputs up to 320 l h−1 were found (with pressure-loss curves showing further potential to 1000 l h−1), this microstructured mixer proved potential to act as process-intensification (PI) equipment.

Seit etwa 10 Jahren beschaftigt sich die Institut fur Mikrotechnik Mainz GmbH (IMM) mit der Nutzung von Mikrostrukturen im Bereich der Mikroverfahrenstechnik. Deren Vorteile – effizienterer Warmeaustausch und Massentransport – bewirken u. a. Steigerung von Ausbeute und Selektivitat bei gleichzeitiger Ressourcenschonung. Die Entwicklung von mikrostrukturierten Mischern war dabei ein Schlussel zu verbesserten Feinchemikaliensynthesen sowie zur Herstellung von Dispersionen, Cremes, Schaumen und Emulsionen. Bislang waren diese mikrostrukturierten Mischer im Wesentlichen auf Labor- oder bestenfalls Pilotanlagen-Masstab festgelegt – typische Maximalflussraten lagen bei 2 – 100 L/h fur wasserahnliche Fluidsysteme. Mit der Einfuhrung der StarLaminatoren StarLam300 und StarLam3000, konnte diese Grenze jetzt auf weit uber 300 L/h bis in den m3/h-Bereich angehoben werden. Beide Apparate zeigen gute Mischguten bei hohen Flussen, die durchaus an die sehr guten Werte von bisher bekannten Niederdurchsatz(L/h)-Mikromischer heranreichen. Damit ist eine Kontinuitat von „wirklichen” Mikromischern uber die hier beschriebenen Hochdurchsatz-Tools bis zu statischen Mischern mit noch hoheren Durchsatzen gegeben. Eine Klassifikation der Mischeffizienz nach dem Leistungseintrag bestatigt ebenso diese Kontinuitat. Mixers with Microstructured Foils for Chemical Production Purposes Since about 10 years the Institut fur Mikrotechnik Mainz GmbH (IMM) is engaged with the application of microstructures for chemical micro process engineering. Their advantages – more efficient heat exchange and mass transport – lead to, among other things, an increase in yield and selectivity even while saving resources. The development of microstructured mixers thereby played a key role for carrying out advanced syntheses of fine chemicals as well as for the generation of dispersions, creams, foams, and emulsions. So far, microstructured mixers were mainly limited for laboratory-scale or at best pilot plant-scale – typical maximum flow rates were from 2 – 100 L/h for watery fluid systems. With the introduction of the StarLaminators StarLam300 and StarLam3000 this barrier could be lifted far beyond 300 L/h up to the m3/h domain. Both apparatus yield at high flow rates a mixing efficiency which reaches the high performance of today's low-capacity (L/h) micro mixers. Therefore, continuity from the ”real” micro mixers over the herein described high-throughput tools to conventionally manufactured static mixers with even higher flow rates is given.

An industrial production-scale process currently conducted at Clariant site/Frankfurt, termed Phenyl Boronic Acid Process from here on, was investigated at laboratory-scale using two micromixer/tubular reactor configurations, being equipped with either a glass interdigital (for details see (1) Ehrfeld, W.; Golbig, K., Hessel, V.: Lowe, H.; Richter, T. Characterization of mixing in micromixers by a test reaction: single mixing units and mixer arrays. Ind. Eng. Chem. Res. 1999, 38, (3), 1075-1082; (2) Hessel, V., Hardt, S.; Lowe, H.; Schonfeld, F. Laminar mixing in different interdigital micromixers - Part 1: Experimental characterization. AIChE J. 2003, 49, 566-577; (3) Hardt, S.; Schonfeld, F. Laminar Mixing in Different Interdigital Micro-mixers - Part 2: Numerical Simulations. AIChE J. 2003, 49, 578-584; (4) Herweck T.; Hardt, S.; Hessel, V.; Lowe, H.; Hofmann, C.; Weise, F., Dietrich, T.; Freitag, A. Visualization of Flow Patterns and Chemical Synthesis in Transparent Micromixers. In Topical Conference Proceedings; IMRET 5, 5th International Conference on Microreaction Technology, AIChE Spring National Meeting; Matlosz, M., Ehrfeld, W., Baselt, J. P., Eds., Springer-Verlag: Berlin, 2001; pp 215-229) or a steel split-recombine mixer (for details see Schonfeld, F.; Hessel, V.; Hofmann, C. An Optimised Split-and-Recombine Micro Mixer with Uniform 'Chaotic' Mixing. Lab Chip 2004,4,65-69). The best yield of the microreactor investigations was 89%, exceeding the performance of the industrially employed stirred-tank process by nearly 25%. Moreover, the total amount of side and consecutive products was decreased from 10-15% to 5-10%. In addition to these yield improvements, the energy expenditure of the microreactor processing was also notably reduced, first of all because of carrying out the reaction at favorable ambient temperature. In contrast, the former batch process had to be carried out at cryogenic temperatures of -35 degreesC. Even at temperatures as high as 50 degreesC, a high selectivity was maintained when using the microreactor. As a further cause for energy savings, the higher purity of the product eliminated the need for distillation; in total therefore, only one heating-cooling cycle with reduced temperature difference was required for the microreactor process in contrast to the three cycles with large temperature differences used in conventional processing. Facing production and process liability issues, a specially made pilot-scale configuration was constructed entirely out of stainless steel components, among them a split-recombine caterpillar mixer having larger internal fluid channels than the interdigital glass mixer. The new configuration allowed one to perform scale-up studies at throughputs as high as 10 L/h.

Very fast mixing in the range of milliseconds as well as deliberately slow mixing was realized by specially adjusted interdigital micro mixers made of glass or stainless steel. The corresponding micro mixers are presented including experimental and theoretical investigations of the respective mixing process. Fast mixing was realized by combination of flow multilamination by interdigital microstructured feeding structures with geometric focusing. Details on the microfabrication, achievable throughputs and hydrodynamics are discussed. To prevent clogging of microsized feeding structures in the case of precipitation reactions, mixing was deliberately slowed down by separating the reactant solutions at the outlet by additional layers of inert liquids.