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Improved Synthesis of a Zirconium(IV) Muconate Metal–Organic Framework: Characterization, Stability and Gas Sorption Properties
Author(s) -
Buragohain Amlan,
Biswas Shyam
Publication year - 2015
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.201500133
Subject(s) - thermogravimetric analysis , chemistry , crystallinity , sorption , powder diffraction , zirconium , isostructural , thermal stability , bet theory , fourier transform infrared spectroscopy , metal organic framework , inorganic chemistry , nuclear chemistry , chemical engineering , organic chemistry , crystallography , crystal structure , catalysis , adsorption , engineering
The formerly reported Zr IV trans , trans ‐muconate framework material ( 1 ) was synthesized by using an improved synthetic protocol. Instead of using the noncommercial Zr 6 ‐methacrylate oxido cluster as the metal source, the same MOF was successfully synthesized by using commercially available ZrCl 4 as the Zr source. Small amounts of H 2 O ( 1 ‐H 2 O‐AS; AS = as‐synthesized) or concd. aqueous HCl ( 1 ‐HCl‐AS) were used as additives in N , N ‐dimethylformamide (DMF) in order to enhance the crystallinity of the compounds. The guest molecules were removed from the pores by heating the as‐synthesized compounds under vacuum, resulting in the empty‐pore forms of the compounds. The as‐synthesized and thermally activated compounds were characterized by X‐ray powder diffraction (XRPD), Fourier transform infrared (FTIR), thermogravimetric (TG) and elemental analyses. Thermogravimetric analyses suggest that the two compounds are stable up to ca. 250 °C in an air atmosphere. As verified by the XRPD experiments, the 1 ‐HCl compounds gradually lose their crystallinity when exposed to water and moisture. As confirmed by the N 2 sorption analyses, the optimally activated 1 ‐HCl compound displayed a BET surface area of 557 m 2 g –1 , which is lower than the isostructural UiO‐66 (950 m 2 g –1 ) but it is close to the literature value (705 m 2 g –1 ). The moderate physiochemical stability paired with considerable porosity renders the material a promising candidate for gas storage and separation.