Design and characterization of a flow reaction calorimeter based on FlowPlate® Lab and Peltier elements

Abstract

Continuous manurfacturing and development of flow processes depend significantly on an optimized and adapted determination of thermokinetic data of chemical reations. Reaction calorimetry represents a prominent technique to quantify the...

Continuous Synthesis of Diazo Acetonitrile: From Experiments to Physical and Grey‐Box Modeling

“…Due to the high number of model parameters in the greybox PFR model, we use k-fold cross-validation to check overfitting is not occurring [51]. This works as follows: given a total of k data sets (in our case experimental data for the mixer and calorimeter setups), we exclude one data set from the identification and solve (23) with the remaining k − 1 data sets. The excluded data set is then used as test set, i.e., we evaluate the model prediction and compare it with the actual data.…”

“…For the sake of brevity, we refer the reader to [47,48], where cashocs is presented, and to [41], where it is used to solve a similar parameter identification problem in the context of a gas phase reaction. The grey-box model is implemented in the dynamic programming language Julia [49] and IPOPT [50] is used to solve the parameter identification problem (23).…”

“…Additionally, reaction calorimetry can help in optimizing reaction conditions, identifying potential hazards, and designing safe and efficient processes. In recent years, a new generation of reaction calorimeters based on micro structured flow reactors and microreactors has emerged [23–26]. The flow reactors used therein provide excellent heat transfer capabilities due to their high specific surface area, which enables precise temperature control.…”

Thermokinetic analyses of metal-sensitive reactions in a ceramic flow calorimeter

“…While the comprehensive review of Frede et al 6 provides a detailed overview on state-of-the-art continuous flow calorimeters, such as the ones from Ladosz, 11 Reichmann 12 and Zhang, 13 even more recent work has seen the integration of a FlowPlate® Lab microreactor into a calorimeter setup. 14 Furthermore, while most flow calorimeters described in literature are set in micro-scale, [11][12][13] scalable milli-scale calorimeters have also been described. 10,15 As for the origin of the used reactors, different predesigned microreactors can be purchased from various manufacturers, typically made from materials such as glass, stainless steel or Hastelloy, and silicon carbide ceramics.…”

Dynamic Spinning Disc Reactor Technology to Enable In Situ Solid Product Formation in a Diazotization and Azo Coupling Sequence

“…The experiment revealed a heat of reaction (Δ H rxn ) of −127 kJ mol –1 for the first step, thus demonstrating its exothermic nature, which corresponds to an adiabatic temperature rise of 18.5 °C. This result highlights the importance of controlling the exotherm through careful dosing of reagents and good heat transfer given the thermal instability of diazonium salts, which then can result in the evolution of nitrogen gas on decomposition. ,, For the second step, an exotherm was also observed, which is a combination of the exothermic neutralization of HCl and NaOH (between −56 and −58 kJ/mol based on literature references) − and the endothermic azo coupling (35.6 kJ/mol).…”