The present study focuses on the aeration of aqueous triethanolamine acting as reaction medium for biocatalytic carboxylations. For enhancing mass transfer in a bubble column reactor, microbubble aeration is applied and compared to conventional macrobubble aeration. Application of a 0.5 μm porous sparger enables microbubble CO2 aeration with bubble size distributions below 150 μm in Sauter mean diameter, correlating with the highest measured mass transfer rates. During CO2 saturation of the aqueous triethanolamine, bubble size distributions changed according to the level of CO2 saturation. For microbubbles, less foaming was observed compared to macrobubble aeration by a 10 μm porous sparger. This microbubble effect is attributed to their accelerated dissolution assisted by the Laplace pressure lowering the amount of bubbles reaching the surface of the liquid. The experiments reveal that the rate of interfacial area generation, which is calculated based on measured bubble size distributions, influences the biocatalyst activity.