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Journal articles
Thermolysis of 1,3-dioxin-4-ones: Fast generation of kinetic data using in-line analysis under flow
Abstract : Rapid acquisition of kinetic data is demonstrated with a commercial meso-scale flow reactor, using a step-change in flow rate or ‘push-out’ from the flow line. For thermolysis of 1,3-dioxin-4-ones (1), we obtain excellent reproducibility in the activation energies measured from spectroscopic data collected by in-line UV or transmission FT-IR monitoring of the output during the transitional period between two flow rates (±3 kJ mol−1, 0.7 kcal mol−1). Analysis of multi-component UV and IR data is conducted using an orthogonal projection approach (multivariate curve resolution by alternating least squares) for complex spectra, or by calibration-less integration of non-overlapping peak absorbance. All analysis methods were validated using off-line 1H NMR analysis, and kinetic parameters obtained using the method of a flow rate step-change were validated against conventional steady-state measurements in which time-series data were acquired across multiple experiments. Thermal transfer and dispersion effects are addressed. The experimental methods described herein are valuable for accelerated reaction study and in process development.
https://hal-normandie-univ.archives-ouvertes.fr/hal-02046204
Contributor : Madeleine Roux-Merlin <>
Submitted on : Friday, February 22, 2019 - 3:36:33 PM
Last modification on : Thursday, July 2, 2020 - 3:30:12 AM
Contributor : Madeleine Roux-Merlin <>
Submitted on : Friday, February 22, 2019 - 3:36:33 PM
Last modification on : Thursday, July 2, 2020 - 3:30:12 AM
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