Combining continuous flow oscillatory baffled reactors and microwave heating: Process intensification and accelerated synthesis of metal-organic frameworks

We have constructed a continuous flow oscillatory baffled reactor (CF-OBR) equipped with a homogeneous and controllable microwave applicator in an entirely novel design. This affords a new route to chemical production incorporating many of the principles of process intensification and allows, for the first time, investigation of the synergistic benefits of microwave heating and CF-OBRs such as; faster and continuous processing; improved product properties and purity; improved control over the processing parameters; and reduced energy consumption. The process is demonstrated by the production of a metal-organic framework (MOF), HKUST-1, a highly porous crystalline material with potential applications in gas storage and separation, catalysis, and sensing. Our reactor enabled the production of HKUST-1 at the 97.42 g/h scale, with a space time yield (STY) of 6.32 × 105 kg/m3/day and surface area production rate (SAPR) of 1.12 × 1012 m2/m3/day. This represents the highest reported STY and fastest reported synthesis (2.2 seconds) for any MOF produced via any method to-date and is an improvement on the current SAPR for HKUST-1 by two orders of magnitude owing to the superior porosity exhibited by HKUST-1 produced using our rig (Langmuir surface area of 1772 compared to 600 m2/g)