A compact 3D printed magnetically stirred tank reactor cascade coupled with a free impinging jet for continuous production of colloidal nanoparticles

Abstract

Most colloidal nanoparticle production processes involve more than one step, such as particle nucleation, growth and stabilisation, that often take place at different time scales. Flow chemistry offers an attractive platform for nanoparticle synthesis, as it can provide excellent control of conditions for each individual step. In this work, a free impinging jet reactor (FIJR), known for its rapid mixing capability and fouling-proof operation, is followed by a cascade of 5 miniaturised (3 ml) continuous stirred tank reactors (mCSTR) that provides longer residence time and efficient temperature control for subsequent synthesis steps, while still being resistant to clogging due to active mixing. The small (0.1 mm) diameter nozzle design allowed the FIJR to provide excellent mixing even at relatively low flowrates (2 ml/min/jet). The mCSTR cascade was arranged in a vertical configuration (one tank on top of another), offering a compact design that is simple to use and requiring only one magnetic stirrer. It provided excellent mixing characteristics with limited dead volumes and interconnections, as reflected by a residence time distribution comparable with the theoretical one for a CSTR cascade. Most parts of the reactor system were 3D printed with features that facilitated the assembly. The proposed FIJR design overcomes the accuracy limitations of 3D printing by combining it with micromilling to achieve one of the smallest FIJR reported and by allowing for rotation of the nozzles to easily resolve issues with jet alignment. The reactor system was employed for the synthesis of colloidal (∼10 nm size) silver nanoparticles via NaBH4 reduction of AgNO3, in a 0.06 g/day scale for 50 min continuous operation and (∼6 nm core size) iron oxide nanoparticles via co-precipitation of Fe3+/Fe2+, producing colloidally stable nanoparticles in a 16.1 g/day scale for over 2 h continuous operation.