Time-Dependent Ni2+-Ion Exchange in Zeolites Y (FAU, Si/AI=1.56) and Their Single-Crystal Structures
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2016 American Chemical Society. Seven single crystals of fully dehydrated Ni2+-exchanged zeolite Y (Si/Al = 1.56) were prepared via cation exchange of Na75Y (| Na75|[Si117Al75O384]-FAU) by flowing 0.05 M aqueous solutions of Ni(NO3)26H2O (pH 4.9 and 294 K) with various ion-exchange times. Their crystal structures were completely determined by single-crystal synchrotron X-ray diffraction techniques in cubic space group Fd3m at 100(1) K. In all seven structures, Ni2+ ions occupy sites I, I, and II, and sometimes site II or a second site II, or both, preferring site I; residual Na+ ions in crystals 1 and 2 are found at site III and/or a second site III. The level of Ni2+ exchange monotonically increased from 75.2 to 89.6% [from 28.2(2) to 33.6(8) Ni2+ ions per unit cell] with increasing exchange time until 18 h. The dealumination of the zeolite frameworks was observed in the center of sodalite cavities after 24 h, suggesting that this process occurs during ion exchange, or subsequent dehydration. H+ ions are present in all seven crystals for a charge balance. Both the unit cell constants and Na+ contents decreased with increasing levels of Ni2+ exchange and ion-exchange time.
