In Situ Energy-Dispersive X‑ray Diffraction for the Synthesis Optimization and Scale-up of the Porous Zirconium Terephthalate UiO-66

The synthesis optimization and scale-up of the benchmarked microporous zirconium terephthalate UiO-66(Zr) were investigated by evaluating the impact of several parameters (zirconium precursors, acidic conditions, addition of water, and temperature) over the kinetics of crystallization by time-resolv...

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Veröffentlicht in:Inorganic chemistry 2014-03, Vol.53 (5), p.2491-2500
Hauptverfasser: Ragon, Florence, Horcajada, Patricia, Chevreau, Hubert, Hwang, Young Kyu, Lee, U-Hwang, Miller, Stuart R, Devic, Thomas, Chang, Jong-San, Serre, Christian
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Sprache:eng
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Zusammenfassung:The synthesis optimization and scale-up of the benchmarked microporous zirconium terephthalate UiO-66(Zr) were investigated by evaluating the impact of several parameters (zirconium precursors, acidic conditions, addition of water, and temperature) over the kinetics of crystallization by time-resolved in situ energy-dispersive X-ray diffraction. Both the addition of hydrochloric acid and water were found to speed up the reaction. The use of the less acidic ZrOCl2·8H2O as the precursor seemed to be a suitable alternative to ZrCl4·xH2O, avoiding possible reproducibility issues as a consequence of the high hygroscopic character of ZrCl4. ZrOCl2·8H2O allowed the formation of smaller good quality UiO-66(Zr) submicronic particles, paving the way for their use within the nanotechnology domain, in addition to higher reaction yields, which makes this synthesis route suitable for the preparation of UiO-66(Zr) at a larger scale. In a final step, UiO-66(Zr) was prepared using conventional reflux conditions at the 0.5 kg scale, leading to a rather high space-time yield of 490 kg m–3 day–1, while keeping physicochemical properties similar to those obtained from smaller scale solvothermally prepared batches.
ISSN:0020-1669
1520-510X
DOI:10.1021/ic402514n