Fluitec mixing + reaction solutions AGSeuzachstrasse 40

A simultaneous determination of the enthalpy of mixing and reaction in a scalable continuous milli-scale flow calorimeter is investigated. As obtained calorimetric data is pivotal for the safety assessment of chemical reactions and processes. The acid-catalysed selective, homogeneous hydrolysis of acetic anhydride with half-lives from a few seconds to a few minutes is investigated as a model reaction. For the enthalpy of mixing 7.2 ± 2.8 kJ/mol and for the enthalpy of reaction −60.8 ± 2.5 kJ/mol were determined. For reactions that show complete conversion in the continuous reactor, a technique is introduced to further improve the accuracy of the reaction enthalpy determination. Thereby, the resolution of the observed temperature profile is increased by measuring the profile at different flow rates. Applying this procedure, the reaction enthalpy of −62.5 kJ/mol was determined which is in good agreement with literature values for this model reaction. Graphical abstract

Process engineering is based on models, which are preferably established at laboratory scale under near-service conditions. Here, for the first time, a kinetic study of the basic hydrolysis of ethyl acetate was performed with a small volume liquidliquid loop reactor satisfying these criteria. The activation energy and pre-exponential factor were determined that agreed with data from the literature. Acquired data could be successfully transferred to well-established ideal reactor models such as continuous stirred tank or plug flow reactors. It was, thus, possible to show that a simply scalable loop reactor, requiring only small amounts of substrate and producing minimum waste, can serve as a tool for kinetic studies of continuous processes.