Influence of Water, Vacuum, and Temperature on Surface Conditions of a Zeolite‐based Molecular Sieve

Molecular sieves such as zeolite-based materials are ubiquitous in industrial separation processes. However, there is a significant gap in understanding the surface properties and adsorption mechanisms for commercial zeolites, as most research focuses on pure zeolite powders rather than industrially relevant forms. Here, this work addresses this gap in understanding by employing advanced characterization techniques, including positron annihilation spectroscopy, X-ray diffraction, scanning electron microscopy, X-ray fluorescence spectroscopy, X-ray photoelectron spectroscopy, liquid nitrogen sorption, and Fourier-transform infrared spectroscopy, to investigate the adsorption and desorption behavior of water in commercial zeolite 13X. Our research reveals insights into the pore-filling mechanisms, the impact of material binders on adsorption properties, and the dynamics of hydration and drying processes for zeolites. Monitoring changes on a minute scale allowed the distinction between fast and slow processes leading to sample drying. The identification of positronium bound to Na⁺ ions indicated that water molecules remain in the vicinity of Na⁺ ions after air-drying zeolite 13X. These findings highlight the importance of various environmental conditions in restoring zeolite properties to baseline after hydration, with significant implications for optimizing industrial processes. This work sets the direction for further research aimed at developing more efficient and robust separation techniques.. Authors: Zaleski, Radosław [Maria Curie-Sklodowska Univ., Lublin (Poland)] (ORCID:0000000272278189); Evans, George Steven [Idaho National Laboratory (INL), Idaho Falls, ID (United States)] (ORCID:0000000176129490); Kierys, Agnieszka [Maria Curie-Sklodowska Univ., Lublin (Poland)]; Kochel, Mateusz [Institute of Energy and Fuel Processing Technology (ITPE), Zabrze (Poland)] (ORCID:0000000277638374); Kuśmierz, Marcin [Maria Curie-Sklodowska Univ., Lublin (Poland)]. DOE Contract: AC07-05ID14517. Subjects: Beads Binder; Coincidence Doppler Broadening Spectroscopy; Commercial Molecular Sieves; Drying; Positron Annihilation; Positron Annihilation Lifetime Spectroscopy; Positron Annihilation Spectroscopy; Water Adsorption; Zeolites; Zeolites X