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Applications of the RC1e Calorimeter for Process Safety and Scale-Up
Aug 19, 2008
Allen M. Beard (Albemarle, USA) reported on the reaction modeling and process development of a fine chemical compound (4-Fluorobenzaldehyde). Kinetic data (ReactIR) and heat of reaction data (RC1e calorimetry) are key components of a safe and efficient scale-up to production.
Background
4-Fluorobnenzaldehyde is a fine chemical product used as an intermediate for pharmaceutical and agrochemical production. Production of this fine chemical involves a Gatterman-Koch Formylation requiring the dissolution and reaction of CO gas with the starting material in the presence of HCI catalyst. Characterization and optimization of the multiple-phase reaction mixture can benefit from in situ FTIR reaction monitoring, eliminating the need for offline sampling and analysis of highly reactive mixtures.
Approach
A series of experiments were performed to characterize the reaction operating space prior to scale-up. Experiments were carried out in a 1.8L RC1eTM pressure reactor, operating at 400 psig at various controlled temperatures. The RC1eTM reaction calorimeter was used to measure the heat of reaction, and ReactIRTM in situ FTIR reaction monitoring was used to track the concentration of reactants and product in solution.
An initial experiment was also carried out to measure the mass transfer rate of CO from the gas phase to the solution phase using ReactIRTM. This was used to determine that the reaction was not mass-transfer rate limited under normal operating conditions.
Results and Conclusions
In situ reaction monitoring (ReactIRTM) and modeling software (MATHCADTM) were used to determine reaction rate constants as a function of experimental operating conditions and to develop an overall kinetic model.
Heat of reaction was simultaneously measured with the RC1eTM Automated Lab Reactor for characterization of the process, which was used in conjunction with the kinetic model to ensure a safe and efficient scale-up to manufacturing.
4-Fluorobnenzaldehyde is a fine chemical product used as an intermediate for pharmaceutical and agrochemical production. Production of this fine chemical involves a Gatterman-Koch Formylation requiring the dissolution and reaction of CO gas with the starting material in the presence of HCI catalyst. Characterization and optimization of the multiple-phase reaction mixture can benefit from in situ FTIR reaction monitoring, eliminating the need for offline sampling and analysis of highly reactive mixtures.
Approach
A series of experiments were performed to characterize the reaction operating space prior to scale-up. Experiments were carried out in a 1.8L RC1eTM pressure reactor, operating at 400 psig at various controlled temperatures. The RC1eTM reaction calorimeter was used to measure the heat of reaction, and ReactIRTM in situ FTIR reaction monitoring was used to track the concentration of reactants and product in solution.
An initial experiment was also carried out to measure the mass transfer rate of CO from the gas phase to the solution phase using ReactIRTM. This was used to determine that the reaction was not mass-transfer rate limited under normal operating conditions.
Results and Conclusions
In situ reaction monitoring (ReactIRTM) and modeling software (MATHCADTM) were used to determine reaction rate constants as a function of experimental operating conditions and to develop an overall kinetic model.
Heat of reaction was simultaneously measured with the RC1eTM Automated Lab Reactor for characterization of the process, which was used in conjunction with the kinetic model to ensure a safe and efficient scale-up to manufacturing.
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