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Abstract
During the early stages of research and development chemical industry needs flexible and versatile tools to investigate chemical reaction systems. An important part of the optimisation of a process considering economic factors, risk analysis and environmental impacts is the determination of a reaction mechanism and its associated parameters (i.e. activation energies, rates and heat of reactions).
We present here a new fully automated small-scale reaction calorimeter combining a power-compensation heater and a thermoelectrically regulated metal surrounding. This dual temperature control makes the reactor highly suitable for fast and exothermic reactions and eliminates the need for time-consuming calibration of heat transfer coefficients. With a working volume from 25 to 45ml the device is particularly suited for the fine and pharmaceutical chemical industries where only small amounts of test substances are available.
An integrated ATR-IR probe coupled to an FT-IR spectrometer allows the investigation of complex reaction mechanisms. Moreover, the new reactor design allows the simultaneous use of various additional in-situ analytics such as UV-Vis, gas intake/uptake and particle size analysis. The performance of the new reaction calorimeter has already been successfully demonstrated based on several reactions [1, 2, 3].
Different analytical techniques may point to different optimum reaction parameters. Algorithms and mathematical tools, such as multi-objective multivariate kinetic modelling, become an important research area in data oriented process development. Only a short introduction into these methods will be given here.
[1] Zogg, A., Fischer, U., & Hungerbühler, K. (2003). A new small-scale reaction calorimeter that combines the principles of power compensation and heat balance. Industrial & Engineering Chemistry Research, 42, 767-776.
[2] Visentin, F., Gianoli, S. I., Zogg, A., Kut, O. M., & Hungerbühler, K. (2004). Pressure-resistant smallscale reaction calorimeter that combines the principles of power compensation and heat balance (CRC.v4). Organic Process Research & Development, 8(5), 725-737.
[3] Visentin, F., Puxty, G., Kut, O. M., & Hungerbühler, K. (2006). Study of the hydrogenation of selected nitro compounds by simultaneous measurements of calorimetric, FT-IR, and gas-uptake signals. Industrial & Engineering Chemistry Research, 45(13), 4544-4553.
We present here a new fully automated small-scale reaction calorimeter combining a power-compensation heater and a thermoelectrically regulated metal surrounding. This dual temperature control makes the reactor highly suitable for fast and exothermic reactions and eliminates the need for time-consuming calibration of heat transfer coefficients. With a working volume from 25 to 45ml the device is particularly suited for the fine and pharmaceutical chemical industries where only small amounts of test substances are available.
An integrated ATR-IR probe coupled to an FT-IR spectrometer allows the investigation of complex reaction mechanisms. Moreover, the new reactor design allows the simultaneous use of various additional in-situ analytics such as UV-Vis, gas intake/uptake and particle size analysis. The performance of the new reaction calorimeter has already been successfully demonstrated based on several reactions [1, 2, 3].
Different analytical techniques may point to different optimum reaction parameters. Algorithms and mathematical tools, such as multi-objective multivariate kinetic modelling, become an important research area in data oriented process development. Only a short introduction into these methods will be given here.
[1] Zogg, A., Fischer, U., & Hungerbühler, K. (2003). A new small-scale reaction calorimeter that combines the principles of power compensation and heat balance. Industrial & Engineering Chemistry Research, 42, 767-776.
[2] Visentin, F., Gianoli, S. I., Zogg, A., Kut, O. M., & Hungerbühler, K. (2004). Pressure-resistant smallscale reaction calorimeter that combines the principles of power compensation and heat balance (CRC.v4). Organic Process Research & Development, 8(5), 725-737.
[3] Visentin, F., Puxty, G., Kut, O. M., & Hungerbühler, K. (2006). Study of the hydrogenation of selected nitro compounds by simultaneous measurements of calorimetric, FT-IR, and gas-uptake signals. Industrial & Engineering Chemistry Research, 45(13), 4544-4553.