Measurement and enhancement of gas–liquid mass transfer in milliliter-scale slurry reactors

Due to the limited availability of chemical reactants in the early process development of pharmaceuticals and fine chemicals, and sometimes the high-cost of catalyst, it is increasingly popular to use milliliter-scale slurry reactors with reaction volumes of 20 ml or less to screen catalyst candidates for three-phase reactions. To ensure the success of catalyst screening, it is advantageous to run reactions under kinetically controlled conditions so that the activities of different catalysts can be compared. Because catalysts with small particle sizes are used in slurry reactors, the reactions are susceptible to gas–liquid mass transfer limitations. This work presents an efficient way of enhancing gas–liquid mass transfer in milliliter-scale reactors through the use of magnetically driven agitation with complex motion. In the reactor described here, gas–liquid mass transfer coefficients can be doubled over those obtained with the agitation technique used in commercial milliliter-scale units. In addition, the reactor can achieve the top range of mass transfer coefficients obtained in a full-scale reactor. This work also presents the first measurements of gas–liquid mass transfer coefficients in milliliter-scale reactors, which are two orders-of-magnitude smaller than systems for which mass transfer coefficients have been reported earlier. Both physical and chemical absorption techniques are used.