Continuous microfluidic synthesis of zirconium-based UiO-67 using a coiled flow invertor reactor

MethodsX. 2021 Jan 23:8:101246. doi: 10.1016/j.mex.2021.101246. eCollection 2021.

Abstract

Metal-organic frameworks (MOFs), particularly Zirconium based, have a wide variety of potential applications, such as catalysis and separation. However, these are held back by traditionally only being synthesised in long batch reactions, which causes the process to be expensive and limit the amount of reaction control available, leading to potential batch to batch variation in the products, such as particle size distributions. Microfluidics allows for batch reactions to be performed with enhanced mass/heat transfer, with the coiled flow inverter reactor (CFIR) setup narrowing the residence time distribution, which is key in controlling the particle size and crystallinity. In this work, a Zirconium based MOF, UiO-67, has been synthesised continuously using a microfluidic CFIR, which has allowed for the product to be formed in 30 min, a fraction of the traditional batch heating time of 24 h. The microfluidicially synthesised UiO-67 is also smaller product with a narrower particle size distribution (≈200 nm to ≈400 nm) than its batch counterpart (~500 nm to over 3 µm).

Keywords: BPDC, biphenyl-4,4-dicarboxylic acid; CFIR, coiled flow inverter reactor; Coiled flow inverter reactor (CFIR); Continuous synthesis; DMF, dimethylformamide; MOFs, Metal organic frameworks; Metal-organic frameworks (MOFs); PXRD, powder X-Ray Diffraction; RTD, residence time distribution; SBU, secondary building unit; SEM, scanning electron microscopy; UiO, universitetet i Oslo.