ISBN 9783843953474

978-3-8439-5347-4, Reihe Apparatedesign

Timothy Aljoscha Frede
Automated Flow Calorimetry for Rapid Characterization of Exothermic Reactions

197 Seiten, Dissertation Technische Universität Dortmund (2023), Softcover, A5

Zusammenfassung / Abstract

Continuous processes and their development are essentially dependent on an optimized and adapted determination of the thermokinetic data of chemical reactions. Continuous flow reaction calorimetry represents a promising technique to quantify the heat release of exothermic reactions, features higher yield and selectivity, facilitates process automation, reduces the environmental footprint, and offers shorter process development times.

Two microscale reaction calorimeters are developed based on commercially available mircroreactors and thermoelectric modules. On the one hand, a reaction calorimeter based on a glass plate microreactor is developed and operated in isoperibolic operation mode to determine thermokinetic data. On the other hand, the calorimeter concept is integrated into an existing Hastelloy® plate microreactor. The setup allows for both isoperibolic and isothermal operation mode. In experimental feasibility studies, the application and limitations of the developed setups are demonstrated.

An essential feature of the developed reaction calorimeters is teh software-guided workflow. This includes automation of experimental planning, execution, and evaluation as well as data management using a commercial laboratory automation system, an open-source system, and a modular open-source IoT-platform. The developed reaction calorimeters and their digital workflow demonstrate the feasibility and future potential of microscale reaction calorimetry in chemical process development.