TY - CONF A1 - Fritzsche, Lutz A1 - Knorr, Annett T1 - Continuous synthesis of a high energetic substance using small scale reactors T2 - ICheaP11 - 11th International conference on chemical & process engineering (Proceedings) N2 - For the industrial production of chemicals a safe process design is required to avoid harm to people and environment. It becomes tremendous important if one or more of the following points are characteristic for the synthesis: high heat release, explosive atmosphere, presence of toxic and/or of thermal unstable substances. One substance group, known for being unstable, is the group of organic peroxides. They are potential high energetic substances. Many syntheses of organic peroxides are carried out in semi-batch mode to control the heat release in a good manner. With the aim to increase process control, the advantages of continuous reaction mode, combined with micro reaction technology, are used for the synthesis of one specific organic peroxide in this work. This approach is not only characterised by shorter residence time, good heat transfer, but also by smaller quantities of managed chemicals, and, therefore, by a lower hazard potential. Often yield and selectivity can be improved additionally. For the study a peroxyester, namely tert-Butyl peroxy-2-ethylhexanoate (TBPEH), with known thermal hazard potential was chosen. The two phase liquid/liquid reaction was carried out in three types of reactors. A small scale tubular reactor, stressed by ultrasound, and two different micro structured reactors were used. One of them had a meandering and the other a split-and-recombine channel structure. Synthesis temperature was also varied. From preliminary studies it was known that the side reaction of the involved carboxylic acid chloride to the corresponding acid can become more important in continuous mode compared to semi-batch mode. The effect of reactor type and temperature on selectivity and therefore yield of TBPEH was analysed and compared. In result the reaction could be carried out in a safe manner. The high heat-exchanging efficiency of the used reactors and the short residence time allowed synthesis temperature near the onset temperature of decomposition of TBPEH. In relation to the results of the capillary tube and of the reactor with meandering channel structure (MR), the results for the split-and-recombine reactor (SAR) showed the best trend line. Further studies have to underline the result. Compared to the traditional reaction path (the semi-batch mode), a higher space time yield could be achieved. This promising information is accompanied by the fact of low reaction volumes. In consequence the productivity is low without a numbering up of reaction channels or a scaling up of it. The nowadays existing philosophy of producing a specific quantity of product by a company, followed by the transport to the costumer may change. Just organic peroxides, used in small quantities, e.g. as initiators for polymerisation processes or as resin hardeners, provide the opportunity for an on-demand-production. T2 - ICheaP-11 - 11th International conference on chemical & process engineering CY - Milan, Italy DA - 2013-06-02 KW - Organic peroxide KW - Small scale reactor KW - Process safety KW - Continuous mode PY - 2013 SN - 978-88-95608-23-5 DO - https://doi.org/10.3303/CET1332115 SN - 1974-9791 N1 - Serientitel: Chemical engineering transactions – Series title: Chemical engineering transactions IS - 32 SP - 685 EP - 690 PB - AIDIC, Associazione Italiana di Ingegneria Chimica CY - Milan AN - OPUS4-28730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wehrstedt, Klaus-Dieter A1 - Knorr, Annett T1 - Miniautoclave - test results on organic peroxides and self-reactive substances T2 - IGUS - EOS working group 2001 T2 - Energetic and Oxidising Substances (EOS) working group meeting CY - Washington, DC, USA DA - 2001-03-12 PY - 2001 AN - OPUS4-1509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wehrstedt, Klaus-Dieter A1 - Knorr, Annett T1 - Miniautoclave - test results on organic peroxides and self-reactive substances T2 - IGUS - EOS working group (ad hoc) T2 - Energetic and Oxidising Substances (EOS) ad hoc group meeting CY - Tsukuba, Japan DA - 2000-11-13 PY - 2000 AN - OPUS4-1519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Knorr, Annett A1 - Rockland, Ulrike A1 - Steinbach, J. ED - Rockland, U. T1 - Sicherheitstechnische Bewertung nach der TRAS 410 am Beispiel einer Perestersynthese T2 - Tagungsband des 10. Kolloquiums zu Fragen der chemischen und physikalischen Sicherheitstechnik N2 - Die Technische Regel für Anlagensicherheit (TRAS) 410 mit dem Titel "Erkennen und Beherrschen exothermer Reaktionen" stellt im Rahmen der Betrachtung der thermischen Prozesssicherheit eine Anleitung zur systematischen Erarbeitung von Gefahren bei chemischen Stoffumwandlungen im Industriemaßstab dar. Sie unterstützt bei der Bewertung der Gefahren und bei der Erstellung von Maßnahmen, um Störfälle zu verhindern. Am Beispiel der exotherm ablaufenden Synthese von tert.-Butylperoxypivalat, einem organischen Peroxid, wird die Vorgehensweise dargestellt. Organische Peroxide sind als thermisch instabile Verbindungen bekannt und besitzen dadurch ein zusätzliches Gefahrenpotential. T2 - 10. Kolloquium zu Fragen der chemischen und physikalischen Sicherheitstechnik CY - Berlin, Deutschland DA - 2004-06-17 PY - 2004 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-48504 SP - 43 EP - 48 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-4850 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schreck, Andreas A1 - Knorr, Annett A1 - Wehrstedt, Klaus-Dieter A1 - Gmeinwieser, T. A1 - Steinbach, J. T1 - Sicherheitstechnische Untersuchungen zur Alkylierung von Wasserstoffperoxid mit verschiedenen Alkoholen T2 - Bericht der 34. Sitzung des DECHEMA-Arbeitsausschusses "Sicherheitstechnische Kenngrößen" T2 - 34. Sitzung des DECHEMA-Arbeitsausschusses "Sicherheitstechnische Kenngrößen" CY - Frankfurt am Main, Deutschland DA - 2001-05-17 PY - 2001 VL - 34 AN - OPUS4-1512 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fritzsche, Lutz A1 - Knorr, Annett ED - Cozzani, V. ED - de Rademaeker, E. T1 - Specification of the limit temperature Texo for a peroxide synthesis using different estimation methods T2 - CISAP-6 - Proceedings of the 6th International Conference on Safety and Environment N2 - A major item of thermal process safety, concerning the industrial realisation of exothermic reactions, is the determination of a temperature, where a reaction can be carried out without risk for humans, environment, and of economic loss. The so-called limit temperature Texo is a safety parameter for the reaction process and should not be mixed up with the Self Accelerating Decomposition Temperature (SADT). The last one refers to a temperature value for safe transportation including specific conditions like transport time and type of containment. In Germany a technical guide (Identification and Control of Exothermic Chemical Reactions, TRAS 410, 2012) specifies three approaches for determining Texo. In this work, all these approaches were applied to specify Texo for the synthesis of three tert-Butyl peroxycarboxylic esters. Peroxycarboxylic esters are a subdivision of organic peroxides, known for their high hazardous potential. Results differed partly significant. Anyhow, all of the used techniques and evaluation methods led to Texo values, which were on the safe side – taken the Texo value estimated by the heat release criterion as reference. This method is considered by the authors as a very accurate one. T2 - CISAP-6 - 6th International Conference on Safety and Environment CY - Bologna, Italy DA - 13.04.2014 KW - Peroxide KW - TRAS410 KW - Process safety PY - 2014 SN - 978-88-95608-27-3 DO - https://doi.org/10.3303/CET1436021 SN - 2283-9216 N1 - Serientitel: Chemical engineering transactions – Series title: Chemical engineering transactions IS - 36 SP - 121 EP - 126 PB - AIDIC, Associazione Italiana di Ingegneria Chimica CY - Milano AN - OPUS4-30618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wehrstedt, Klaus-Dieter A1 - Knorr, Annett A1 - Schreck, Andreas T1 - Test results on energetic substances using the Miniautoclave T2 - IGUS - EOS working group 2001 T2 - Energetic and Oxidising Substances (EOS) working group meeting CY - Buxton, England, UK DA - 2000-04-10 PY - 2000 AN - OPUS4-1518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -