Journal
ACS SUSTAINABLE CHEMISTRY & ENGINEERING
Volume 6, Issue 11, Pages 15841-15849Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acssuschemeng.8b04458
Keywords
Zirconium MOFs; Zirconium acetate precursor; Mechanochemistry; Simple activation procedures; Twin-screw extrusion; Catalytic activity
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Funding
- Croatian Science foundation [4744]
- NSERC [RGPIN-2017-06467]
- NSERC E. W. R. Steacie Memorial Fellowship [SMFSU 507347-17]
- Defense Threat Reduction Agency [HDTRA1-18-1-0003]
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We present a solvent-free, green, and rapid mechanochemical route for the synthesis of a series of zirconium metal organic frameworks (MOFs) composed of Zr-6 cluster nodes, UiO-66, UiO-66-NH2, MOF-801, and MOF-804, both on a laboratory scale and by scalable and flow mechanochemical processing. The methodology, based on the use of a nonconventional zirconium dodecanuclear acetate cluster and a minute amount of water as an additive, affords high-quality MOFs in less than 1 h of milling, with minimal requirements for workup processing and eliminating the need for conventional hazardous solvents, such as dimethylformamide. Moreover, the use of a dodecanuclear zirconium acetate precursor circumvents the need for modulators resulting in acetic acid as the only byproduct of the reaction, which harm these acid-resistant materials. The porosity, thermal and chemical stability, as well as catalytic activity of mechanochemically prepared Zr-based MOFs are similar to those of solvothermally synthesized counterparts. Finally, the synthesis is readily applicable on a 10 g scale by using a planetary mill, and is also performed by solid-state flow synthesis using twin-screw extrusion (TSE), affording more than 100 g of catalytically active UiO-66-NH2 material in a continuous process at a rate of 1.4 kg/h.
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