Zogg, Andreas
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Modeling-based approach towards quality by design for a telescoped process
A telescoped, two-step synthesis was investigated by applying Quality by Design principles. A kinetic model consisting of 12 individual reactions was successfully established to describe the synthesis and side reactions. The resulting model predicts the effects of changes in process parameters on total yield and quality. Contour plots were created by varying process parameters and displaying the model predicted process response. The areas in which the process response fulfils predetermined quality requirements are called design spaces. New ranges for process parameters were explored within these design spaces. New conditions were found that increased the robustness of the process and allowed for a considerable reduction of the used amounts of a reagent. Further optimizations, based on the newly generated knowledge, are expected. Improvements can either be direct process improvements or enhancements to control strategies. The developed strategies can also be applied to other processes, enhancing upcoming and preexisting research and development efforts.
Triphenylphosphanoxid Reduktion mit Silanen
Triphenylphosphan (TPP) ist ein häufig genutztes Reagenz bei der Wittig-Reaktion. Dabei wird es stöchiometrisch zu Triphenylphosphanoxid (TPPO) umgewandelt, welches zum heutigen Zeitpunkt entsorgt werden muss. Eine Rückführung zu TPP ist für die Industrie von grossem Nutzen. Deshalb wurde eine Reduktion mit Silanen für eine Implementierung untersucht. Es war möglich die grössten Hindernisse dieses Vorgehens für einen Prozess zu umgehen oder zu lösen. So wurde in diesem Zusammenhang die Aufarbeitung komplett neu entworfen und alle Abfallströme für eine Rückführung bzw. Weiterverarbeitung optimiert. Zudem konnten alle Reaktionsparameter und deren Einfluss quantifiziert und verbessert werden.
Development and evaluation of a new screening workflow for the determination of the self-accelerating decomposition temperature of solids
According to the UN (United Nations) recommendations for the transport of dangerous goods self reactive substances need to be identified and classified with a suitable temperature for transportation, the so-called self-accelerating decomposition temperature (SADT). Several test methods (H.1-H.4) are suggested by the UN for the determination of the SADT1. The suggested tests are inappropriate for many practical situations as they require a large amount of test substance, a significant experimental effort and the tests are hazardous with regard to laboratory safety2. Thus, the quantity of performed tests should be reduced to an absolute minimum. This is achievable if these tests could be limited to critical substances that are expected to have an SADT value below the 75 °C threshold for a 50 kg package, as defined by the UN. Hence, the development of a screening workflow, which is able to identify such critical substances is required. Such screening methods already exist, but they are often based on a single calorimetric principle and were not validated consequently. Here we present a new screening workflow to determine the SADT, by combining accelerating rate calorimetry (ARC) and differential scanning calorimetry (DSC). The experimental data were evaluated using nth-order kinetic combined with the Semenov model. The results of this screening workflow are validated for twelve solid compounds with data obtained from the H.2-adiabatic storage tests. The H.2-adiabatic storage tests were performed by an iso-certified reference laboratory. All of the twelve evaluated solid compounds were accurately categorized above or below the 75 °C threshold value. Furthermore, the new screening workflow identifies and flags substances with potentially autocatalytic decomposition kinetics. To our knowledge, we offer the first free, validated, standalone ready-to-use screening workflow for the categorization of solid compounds according to the 75 °C SADT threshold value. The workflow is implemented in MATLAB with an open source code. This enables further validation and development of this workflow towards a best practice method for the categorization of substances according to the 75 °C SADT threshold value.
Die Chemie Pilotanlage der FHNW Muttenz
Der Verein Miniplant 4.0 entwickelt im Process Technology Center an der FHNW neuartige Chemie-Pilotanlagen im Miniplant-Massstab. Der zentrale Scale-Down-Reaktor dient der präzisen Prozessentwicklung im Rührkessel. Insbesondere werden darin die lokalen thermischen Verhältnisse des Produktionsreaktors durch den Einsatz eines speziell designten Wärmetauschers exakt nachgebildet. Damit wird den Studenten und lokalen Unternehmen ein neuartiges Entwicklungswerkzeug zur Verfügung gestellt, welches einen schnelleren und präziseren Scale-Up von Produktionsverfahren direkt aus dem Labormassstab in den Produktionsreaktor erlaubt. Herr Prof. Dr. Andreas Zogg von der FHNW in Muttenz zeigt Ihnen den aktuellen Status der Anlage und die vielseitigen Schulungs- und Forschungsmöglichkeiten. Unterstützt wird er durch Herrn Dr. Jonas Asprion von der Firma Tool-Temp AG, welche die Kommerzialisierung der Temperierlösungen für Reaktormantel und Wärmetauscher anstrebt.
Development of a novel measurement setup to study and predict electrostatic discharges in agitated glass‐lined vessels
Two glass lined reactors in a launch platform facility operated by Syngenta have been damaged during the crystallization of an organic compound due to electrostatic discharges. The goal of this work was to design and commission a novel setup to measure charges and currents generated by this slurry in a laboratory‐scale reactor. An improved and more sophisticated setup was then proposed for possible implementation in Syngenta's own laboratories. With this novel setup, the electrostatic charging of stirred suspensions involving nonconductive solvents could be accurately measured in the context of a case study that involved the suspension that led to liner damages in the production facilities of Syngenta.
Modeling-Based Approach Towards Quality by Design for a Telescoped Process
A synthesis step, consisting of two sub-steps A and B was investigated by applying a model based approach. Deepening the process understanding was achieved through performed experiments, which also led to the generation of valuable knowledge for future improvements. A kinetic model consisting of 12 reactions and 15 components was successfully established. The model predicts the effects of changes in process parameters on quality. On this basis recommendations for process optimizations have been formulated.