title: In situ energy-dispersive X-ray diffraction for the synthesis optimization and scale-up of the porous zirconium terephthalate UiO-66.
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.
authors: Institut Lavoisier, UMR CNRS 8180, Université de Versailles Saint-Quentin-en-Yvelines , 45 avenue des États-Unis, 78035 Versailles cedex, France.
authors: Florence
authors: F
authors: Ragon
authors: Patricia
authors: P
authors: Horcajada
authors: Hubert
authors: H
authors: Chevreau
authors: Young Kyu
authors: YK
authors: Hwang
authors: U-Hwang
authors: UH
authors: Lee
authors: Stuart R
authors: SR
authors: Miller
authors: Thomas
authors: T
authors: Devic
authors: Jong-San
authors: JS
authors: Chang
authors: Christian
authors: C
authors: Serre
mesh_terms: D002712:Chlorides / Q000737:chemistry*; D008958:Models, Molecular; D010795:Phthalic Acids / Q000138:chemical synthesis* / Q000737:chemistry; D016062:Porosity; D014961:X-Ray Diffraction; D015040:Zirconium / Q000737:chemistry*
chemical_list: D002712:Chlorides; D010795:Phthalic Acids; C011363:terephthalic acid; D015040:Zirconium; C429984:zirconium chloride