Synthesis of metal-organic frameworks by continuous flow

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Bayliss, Peter A. ; Ibarra, I.A. ; Perez, E. ; Yang, S. ; Tang, Chiu C. ; Poliakoff, Martyn ; Schröder, Martin (2014)

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.
  • References (1)

    1. K. S. Walton and R. Q. Snurr, J. Am. Chem. Soc., 2007, 129, 8552-8556. 2. Y.-S. Bae, A. O. z. r. Yazaydın and R. Q. Snurr, Langmuir, 2010, 26, 5475-5483.

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