Advances in Continuous Flow Calorimetry

Frede, Timothy Aljoscha; Maier, Manuel C.; Kockmann, Norbert; Gruber-Wölfler, Heidrun

doi:10.1021/acs.oprd.1c00437

Cited by 7 publications

(3 citation statements)

References 47 publications

(82 reference statements)

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“…Continuous flow calorimetry is receiving increasing attention in recent years. 28 The miniaturization of calorimeters that operate in a continuous flow fashion potentially enables the safe investigation of fast and highly exothermic reactions at high reactant concentrations along with minimal material consumption. 29 There are three types of flow calorimeters based on different calorimetric methods that have been reported:…”

Section: Introductionmentioning

confidence: 99%

Thermal characterization of highly exothermic flash chemistry in a continuous flow calorimeter

Fu¹,

Jiang²,

Hone³

et al. 2023

React. Chem. Eng.

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“…Recently, the combination of a continuous flow reactor and in-line thermal sensing, viz. continuous flow calorimetry (Figure c), has been attracting attention because it enables simpler, quicker, and safer screening of process conditions than batch calorimetry does. − Continuous flow calorimetry uses eq to calculate the enthalpy of reaction Δ H or fractional conversion X to determine the reaction kinetics by measuring the heat flux at a volumetric flow rate of F and initial reactant concentration of c 0 …”

Section: Introductionmentioning

confidence: 99%

Simultaneous Characterization of Reaction Kinetics and Enthalpy by Calorimetry Based on Spatially Resolved Temperature Profile in Flow Reactors

Imamura

Ogawa

Otake

et al. 2023

Org. Process Res. Dev.

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Characterizing the Gibbs energy of activation and the enthalpy of reactions typically requires repeated sampling. In this study, a new calorimetric reaction-characterization technique was developed for thermokinetic analysis in a flow reactor. The method was used to simultaneously determine the Gibbs energy of activation from the reaction kinetics and the enthalpy of reaction by fitting the thermal model equation to the spatially resolved temperature profile obtained on a flow reactor. This procedure was verified and comparatively assessed with conventional analytical methods using a family of peptide syntheses as model reactions. The thermal model equation closely fitted the acquired temperature profile. The calculated Gibbs energies of activation agreed closely with the values determined from product yield-time trends obtained using several reactants at different temperatures. The calculated reaction enthalpy was similar to the values obtained from quantum chemical calculations. The findings suggest that spatial regression calorimetry can simultaneously extract more reaction characteristics than conventional calorimetry.

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“…Recently, we have shown that the reaction enthalpy of a fast and selective reaction can be measured in the continuous flow calorimeter without extensive calibration of the heat transfer coefficient [12]. However, organometallic reactions, nitrations or polymerisations have half-lives in the range of seconds or minutes [13]. If full conversion is not achieved, the analysis of the exiting product is indispensable.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of enthalpy of mixing and reaction using milli-scale continuous flow calorimetry

Steinemann

Rütti²,

Moser³

et al. 2022

J Flow Chem

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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

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Advances in Continuous Flow Calorimetry

Cited by 7 publications

References 47 publications

Thermal characterization of highly exothermic flash chemistry in a continuous flow calorimeter

Simultaneous Characterization of Reaction Kinetics and Enthalpy by Calorimetry Based on Spatially Resolved Temperature Profile in Flow Reactors

Simultaneous determination of enthalpy of mixing and reaction using milli-scale continuous flow calorimetry

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