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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.
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Submitted on : Friday, February 22, 2019 - 3:36:33 PM
Last modification on : Wednesday, March 16, 2022 - 3:05:18 AM

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Thierry Durand, C. Henry, D. Bolien, D.C. Harrowven, S. Bloodworth, et al.. Thermolysis of 1,3-dioxin-4-ones: Fast generation of kinetic data using in-line analysis under flow. Reaction Chemistry & Engineering, Royal Society of Chemistry, 2016, 1 (1), pp.82-89. ⟨10.1039/C5RE00007F⟩. ⟨hal-02046204⟩



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