We present a 3D-printed continuous flow platform for controllable synthesis of isobutylaluminoxanes (IBAO), an effective olefin polymerization co-catalyst, via highly exothermic hydrolytic reaction of triisobutylaluminum (TIBA). This platform encompasses modules of mixing and reaction, in-line separation, and in situ UV-vis characterization. In addition, two NMR protocols are established to validate the results of in-line UV-vis analysis (31P NMR) and reveal product structures (1H NMR). Measured temperature profiles over the reactor indicate essentially fast heat removal, ensuring inherent safety. Subsequently, co-catalytic activity of IBAO is obtained by ethylene oligomerization experiments using an iron-based catalyst system at atmospheric pressure. Furthermore, we investigate the influence of key operating parameters including initial molar ratio between water and TIBA, initial TIBA concentration, and residence time. High IBAO yield over 98% and superior co-catalytic activity of ~5000 kg·(mol Fe)–1·h–1 are achieved with optimized parameters in this single-pass platform, demonstrating the advantages of process.

Based on a cold-flow experimental device, the transition between trickle flow and pulse flow in a 3D cocurrent downflow three-phase moving bed is investigated by the standard deviation of pressure drop and visual observations. Results show that at a constant gas flow rate, the trickle-to-pulse transition shifts to a higher liquid flow rate with the increasing solid flow rate because the particle moving inhibits the formation of local liquid blockage. Furthermore, an empirical model is proposed to fit the trickle-to-pulse transition boundary by correlating the dynamic liquid holdup at the boundary with the gas Reynolds number and the particle velocity. Finally, the effects of the particle moving on the liquid distribution is investigated, which show that the particle moving makes the liquid distribution more uniform when the solid flow rate is smaller than a certain value. But further increasing the solid flow rate, the liquid distribution becomes uneven