TY - JOUR A1 - Hieronymus, Hartmut A1 - Fischer, J. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Lange, T. A1 - Klemm, E. T1 - Sicherheitstechnische Untersuchungen zum Betrieb von Mikroreaktoren im Explosionsbereich N2 - Es wird eine Methode zur sicherheitstechnischen Untersuchung von Mikroreaktoren und mikrostrukturierten Komponenten, die im Explosionsbereich betrieben werden sollen, vorgestellt. Mikrostrukturierte Reaktoren sind nicht inhärent sicher, wenngleich der Bereich der sicheren Betriebsbedingungen gegenüber konventionellen Reaktoren erweitert ist. Der Explosionsbereich kann durch die Mikrostrukturen eingeengt werden. Am Beispiel von Ethylen/Sauerstoff-Gemischen und Ethylen/N2O-Gemischen wird hinsichtlich der Ausbreitung von Detonationen durch Kapillarrohre gezeigt, dass die sogenannte λ/3-Regel angewandt werden kann. Darüber hinaus werden erste Ergebnisse der Untersuchung der Ausbreitung von Explosionen durch einen Mikroreaktor mit rechteckigem Strömungskanal vorgestellt. KW - Detonationszellbreite KW - Explosionsgrenzen KW - Mikroreaktoren KW - Sicherheitstechnik KW - Detonation cell width KW - Explosion limit KW - Microreactor KW - Saftey engineering PY - 2011 DO - https://doi.org/10.1002/cite.201100112 SN - 0009-286X SN - 1522-2640 VL - 83 IS - 10 SP - 1742 EP - 1747 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-24486 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liebner, Christian A1 - Fischer, J. A1 - Heinrich, Sebastian A1 - Lange, T. A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Are micro reactors inherently safe? An investigation of gas phase explosion propagation limits on ethene mixtures N2 - A method for the determination of safety properties for micro reactors and micro structured components is presented. Micro structured reactors are not inherently safe but the range of safe operating conditions of micro reactors are extended since the explosion region is reduced. The λ/3 rule was demonstrated to be applicable to micro scale tubes for stoichiometric mixtures of ethane–oxygen and ethane–nitrous oxide. Furthermore first results from an investigation concerning detonation propagation through a micro reactor of non-ideal geometry are shown. Initial pressure investigated is ranging from low pressure up to 100 kPa. KW - Micro reactor KW - Explosion propagation limits KW - Chemical safety KW - Investigation method PY - 2012 DO - https://doi.org/10.1016/j.psep.2011.08.006 SN - 0957-5820 SN - 1744-3598 VL - 90 IS - 2 SP - 77 EP - 82 PB - Elsevier CY - Amsterdam AN - OPUS4-25594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Sebastian T1 - Safety aspects of heterogeneously catalysed oxidations inside the explosion region in micro reactors T2 - IMRET 12 The International Conferences on Microreaction Technology CY - Lyon, France DA - 2012-02-20 PY - 2012 AN - OPUS4-25585 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, T. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Reaction engineering investigations of the heterogeneously catalyzed partial oxidation of o-xylene in the explosion regime using a microfixed bed reactor N2 - The heterogeneously catalyzed selective gas phase oxidation of o-xylene was investigated, using a microstructured fixed bed reactor, inside of the explosion regime. The reaction was carried out with high amounts of o-xylene in air and stoichiometric with oxygen using a V2O5/TiO2-catalyst prepared through grafting. There were no significant losses in the selectivity to phthalic anhydride observable, during the measurements in the explosion regime, with feed compositions of up to 7 vol% o-xylene. Also the space-time yield was up to 2.3 times higher in comparison to conventional reaction conditions. An increase of the selectivity to total oxidation products was observed at higher o-xylene concentrations between 10 and 25 vol% o-xylene, which possibly was caused by the formation of a hotspot. The investigation of the used catalyst revealed a thermally induced deactivation due to phase transition of anatase into rutil and formation of crystalline vanadium oxide. Despite that expected hotspot at high oxylene concentrations, there was no ignition or explosion of the gas mixture observable. KW - O-xylene oxidation KW - Phthalic anhydride KW - V2O5/TiO2-catalyst KW - Microfixed bed reactor KW - Explosion regime KW - Hotspot PY - 2012 DO - https://doi.org/10.1016/j.ces.2011.10.072 SN - 0009-2509 VL - 69 IS - 1 SP - 440 EP - 448 PB - Elsevier CY - Amsterdam AN - OPUS4-25463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Sebastian A1 - Edeling, Florian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Lange, T. A1 - Klemm, E. T1 - Catalyst as ignition source of an explosion inside a microreactor N2 - The present issue reports on a specific aspect of safety engineering of the heterogeneously catalysed oxidation of ethene in a continuous-flow microreactor. Conversion of ethene and the corresponding surface temperature of the catalyst were monitored for different reactor temperatures and total flow rates with a stoichiometric ethene/oxygen mixture for total oxidation. Safe operation of the highly exothermic oxidation was possible, but not in the whole parameter range. At high reactor temperatures and flow rates, ignition of an explosion inside the microreactor caused by a hot spot on the surface of the catalyst was observed for the first time. KW - Catalyst KW - Ethene KW - Explosions KW - Hot spot KW - Microstructure KW - Safety PY - 2012 DO - https://doi.org/10.1016/j.ces.2012.08.049 SN - 0009-2509 VL - 84 SP - 540 EP - 543 PB - Elsevier CY - Amsterdam AN - OPUS4-26782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Liebner, Christian A1 - Heinrich, Sebastian A1 - Edeling, Florian A1 - Hieronymus, Hartmut A1 - Lange, T. A1 - Klemm, E. ED - Pierucci, S. ED - Klemes, J.J. ED - De Rademaeker, E. ED - Fabiano, B. ED - Buratti, S.S. T1 - Explosion initiation, propagation, and suppression inside a micro structured reactor N2 - The present contribution reports on specific aspects of safety engineering in heterogeneously catalysed oxidation reactions. Results for ethene-oxygen-mixtures in a continuous-flow micro reactor are reported related to the safety issues of the ethylene oxide process. Initial pressure is ranging from below 1 bar up to 10 bar at initial temperatures ranging from room temperature up to 673 K. Micro structured reactors offer an extended range of operating conditions. The key issue to be discussed in the present contribution is how to safely operate a micro reactor at conditions in conventional devices to be characterised as inside the explosion region. Within certain limits suppression of explosion inside a micro reactor can be achieved. This holds true for chain reactions as well as runaway reactions. Nevertheless it is not possible to safely operate micro structured reactors at any condition. Therefore, explosion propagation through a Micro structured reactor and initiation of gas phase explosions by hot spots inside the reactor were investigated. The investigation methods applied are subject to actual standardization. T2 - 14th International symposium on loss prevention and safety promotion in the process industries CY - Florence, Italy DA - 12.05.2013 KW - Micro reactor KW - Explosion KW - Safety PY - 2013 SN - 978-88-95608-22-8 DO - https://doi.org/10.3303/CET1331101 SN - 1974-9791 N1 - Serientitel: Chemical engineering transactions – Series title: Chemical engineering transactions IS - 31 SP - 601 EP - 606 PB - AIDIC, Associazione Italiana di Ingegneria Chimica CY - Milano AN - OPUS4-28583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Sebastian T1 - Hot Spots als Zündquelle in Mirkoreaktoren mit Wandkatalysator T2 - Jahrestreffen Reaktionstechnik 2013 CY - Würzburg, Germany DA - 2013-05-06 PY - 2013 AN - OPUS4-28593 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, T. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Partial oxidation of o-xylene to phthalic anhydride inside of the explosion regime using a micro structured reactor N2 - The heterogeneously catalyzed gas phase oxidation of o-xylene (oX) to phthalic anhydride (PA) was investigated above the lower explosion limit of appr. 2 vol.% oxylene in air using a micro structured reactor. For these investigations a V2O5/T1O2 grafting catalyst was applied as micro fixed bed and as wall catalyst. Up to 7 voL% 0-xylene, selectivities as well as space-time-yields to PA could be increased siginificantly. At o-xylene concentrations higher than 7 vol. %, the selectivity and space-time-yield to PSA decreased, probably due to a hotspot, which was predicted at high o-xylene concentrations with an approximation and could be indirectly approved by thermal deactivation of the used catalyst. T2 - 2012 AIChE Annual meeting CY - Pittsburgh, PA, USA DA - 28.10.2012 KW - O-xylene oxidation KW - V2O5/TiO2 catalyst KW - Micro structured reactor KW - Explosion regime KW - Micro reactor KW - Explosion KW - Phthalic anhydride KW - Partial oxidation PY - 2013 SN - 9781622767380 SP - 90 EP - 93 AN - OPUS4-28706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Dudzus, Thomas A1 - Meier, Klaus A1 - Recknagel, Sebastian A1 - Hedrich, Martina A1 - Matschat, Ralf T1 - Measurement of oxygen and nitrogen in high purity metals used as national standards for elemental analysis in Germany by classical carrier gas hot extraction (HE) and HE after activation with photons N2 - The special importance of the analysis of non-metals in high purity metals, which will serve as national standards for elemental analysis in Germany, is illustrated for oxygen and nitrogen. The typical range of the mass fraction of oxygen and nitrogen in these materials is below 10.MU.g/g, often close to 1.MU.g/g. The two methods applied at BAM for these measurements are classical carrier gas hot extraction (HE) and carrier gas hot extraction after activation with photons (PAA-HE). The approach, the methods and their advantages and limitations are discussed. Comparative results from the measurement of oxygen and nitrogen in Cu, Fe, Ga, Pb, Sn and W are presented. (author abst.) T2 - 8th International Conference on Ultra-High Purity Base Metals (UHPM-2001) CY - Berlin, Germany DA - 2001-06-25 KW - Oxygen determination KW - Nitrogen determination KW - High purity metals KW - Carrier gas hot extraction KW - Photon activation analysis PY - 2002 DO - https://doi.org/10.2320/matertrans.43.98 SN - 1345-9678 SN - 1347-5320 VL - 43 IS - 2 SP - 98 EP - 100 PB - Japan Institute of Metals CY - Sendai AN - OPUS4-1361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich A1 - Recknagel, Sebastian T1 - Measurement of Nitrogen in Steel by Carrier Gas Hot Extraction - a Challenge in Calibration T2 - 6th International Workshop on progress in analytical chemistry in the steel and metals industries CY - Luxembourg, Luxembourg DA - 2002-05-14 PY - 2002 SP - 1(?) AN - OPUS4-1629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -