Rapid determination of reaction order and rate constants of an imine synthesis reaction using a mesoscale oscillatory baffled reactor

Intensification of carboxylic acid esterification using a solid catalyst in a mesoscale oscillatory baffled reactor platform

“…Steady states were achieved for the multi-steady states screening at all the ramped residence times of 2.5 -20min ( Figure 4). The results clearly showed that a step change occurred between residence times, similar to that reported elsewhere [34]. The flows inside the meso-OBR were therefore at a high degree of plug flow at these experimental conditions, resulting in a tight control of residence time and effective mixing, which allowed steady states to be achieved quickly with little variation in hexanoic acid conversion.…”

Passive isothermalisation of an exothermic reaction in flow using a novel “Heat Pipe Oscillatory Baffled Reactor (HPOBR)”

“…For process intensification, this means the reactor volume can also be reduced by the same margin to achieve the same throughput. Further, it was found that removing the large dilution otherwise created by the solvent, in combination with the elevated operating temperatures, caused the reaction rate to be approximately 13 times faster than the reaction when conducted at 0.25 M concentrations [21] (these data are not shown here). Therefore, the solventless synthesis of this imination reaction in the HPOBR provides a combined 260-fold intensification compared with the reaction performed in solvent whilst improving the conversion.…”

“…With no solvent or thermal control, this reaction reaches a temperature of ~90 °C, higher than the boiling point of butylamine (79 °C), and has an estimated reaction enthalpy of -20 kJ/mol based on average bond enthalpies [20]. Therefore, high solvent ratios (20:1) are typically used to minimise the impact of the temperature rise [21]. The benzaldehyde (99%) and n-butylamine (99.5%) reagents were both supplied by Sigma Aldrich and used as supplied.…”

“…The experiment design for the JOBR was implemented using the multi-steady state approach of previous works [21]. The JOBR was positioned with the FTIR probe at the outlet (Figure 1b) and the same start-up procedure as the HPOBR implemented.…”

“…The imination reaction under investigation here typically uses a high solvent excess (20:1) to avoid excessive heat release during the reaction [21]. In removing this solvent, the processing volume is reduced by a factor of 20.…”