Synthesis of metal-organic frameworks by continuous flow

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 demonstrat...

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Bibliographic Details
Main Authors: Bayliss, Peter A., Ibarra, I.A., Perez, E., Yang, S., Tang, Chiu C., Poliakoff, Martyn, Schröder, Martin
Format: Article
Published: Royal Society of Chemistry 2014
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Online Access:https://eprints.nottingham.ac.uk/29698/
Description
Summary: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.