Synthesis of metal-organic frameworks by continuous flow
Bayliss, Peter A. and Ibarra, I.A. and Perez, E. and Yang, S. and Tang, Chiu C. and Poliakoff, Martyn and Schröder, Martin (2014) Synthesis of metal-organic frameworks by continuous flow. Green Chemistry, 16 (8). pp. 3796-3802. ISSN 1463-9262
A continuous flow process for the synthesis of a metal-organic framework using only water as the reaction medium and requiring only short residence times is described. This affords a new route to scale-up of materials incorporating many of the principles of green chemistry. The process is demonstrated by the synthesis MIL-53(Al) via continuous flow reaction requiring only 5-6 minutes with a space time yield of 1300 kg m-3 d-1. We have demonstrated the synthesis of 500 g of MIL-53(Al) using this process, which can be scaled-up further by simply feeding further solutions of metal salt and ligand through the reactor. The product has a higher surface area and a better colour than a commercially produced sample of this MOF. In addition, a new and effective method for the extraction of terephthalic acid from within the pores of MIL-53(Al) using supercritical ethanol has been developed, representing a new methodology for activation and removal of substrates from porous hosts.
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