In situ energy-dispersive X-ray diffraction for the synthesis optimization and scale-up of the porous zirconium terephthalate UiO-66.
Inorg Chem
; 53(5): 2491-500, 2014 Mar 03.
Article
en En
| MEDLINE
| ID: mdl-24527942
ABSTRACT
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.
Texto completo:
1
Colección:
01-internacional
Base de datos:
MEDLINE
Asunto principal:
Ácidos Ftálicos
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Difracción de Rayos X
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Circonio
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Cloruros
Idioma:
En
Revista:
Inorg Chem
Año:
2014
Tipo del documento:
Article
País de afiliación:
Francia