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A Facile “Green” Route for Scalable Batch Production and Continuous Synthesis of Zirconium MOFs
Author(s) -
Reinsch Helge,
Waitschat Steve,
Chavan Sachin M.,
Lillerud Karl Petter,
Stock Norbert
Publication year - 2016
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201600295
Subject(s) - zirconium , chemistry , aqueous solution , metal organic framework , sorption , chemical engineering , cubic zirconia , inorganic chemistry , organic chemistry , ceramic , adsorption , engineering
Considering the requirements for the commercial production of metal–organic frameworks (MOFs), we investigated the aqueous synthesis of zirconium MOFs. A highly versatile route was identified employing ZrOCl 2 · 8H 2 O, H 2 O, acetic acid and the respective linker molecule as starting materials. These synthesis conditions are suitable to obtain zirconium MOFs with different topologies like UiO‐66‐(OH) 2 , zirconium fumarate, zirconium mesaconate, DUT‐67 or MOF‐808 with synthesis times of 1 to 5 h under microwave irradiation. The scalability of the synthesis of zirconium fumarate was demonstrated at multigram scale under reflux conditions using conventional dielectric heating. To ease the recovery of this MOF which bypasses filter paper as a pure product, we identified sodium polyacrylate as a suitable additive to induce aggregation of the particles. Moreover, a custom‐made prototype flow reactor was developed which allows for the continuous synthesis of zirconium fumarate and UiO‐66‐NH 2 starting from a slurry of the starting materials. The commonly employed toxic organic solvents needed for activation/purification of the MOFs could be successfully replaced by a basic aqueous solution.