Practical development of continuous supercritical fluid process using high pressure and high temperature micromixer

In the synthesis of metal oxide fine particles by continuous supercritical hydrothermal method, the particle characteristics are greatly affected by not only the reaction conditions (temperature, pressure, residence time, concentration, etc.), but also the heating rate from ambient to reaction temperature. Therefore, the heating method by direct mixing of starting solution at room temperature with supercritical water is a key technology for the particle production having smaller size and narrow distribution. In this paper, mixing engineering study through comparison between conventional T-shaped mixers and recently developed swirl mixers was carried out in the hydrothermal synthesis of NiO nanoparticles from Ni(NO3)2 aqueous solution at 400 °C and 30 MPa. Inner diameter in the mixers and total flow rates were varied. Furthermore, the heating rate was calculated by computational fluid dynamics (CFD) simulation. Relationship between the heating rate and the average particle size were discussed. It was clarified that the miniaturization of mixer inner diameter and the use of the swirl flow were effective for improving mixing performance and contributed to produce small and narrow distribution particle under same experimental condition of flow rate, temperature, pressure, residence time, and concentration of the starting materials. We have focused the mixer optimization due to a difference in fluid viscosity.