Static in-situ hydrothermal synthesis of small pore zeolite SSZ-16 (AFX) using heated and pre-aged synthesis mixtures

0458887 - ÚFCH JH 2017 RIV NL eng J - Journal Article
Hrabánek, Pavel - Zikánová, Arlette - Supiňková, Taťána - Drahokoupil, Jan - Fíla, V. - Lhotka, M. - Dragounová, H. - Laufek, František - Brabec, Libor - Jirka, Ivan - Bernauer, B. - Prokopová, Olga - Martin-Gil, V. - Kočiřík, Milan
Static in-situ hydrothermal synthesis of small pore zeolite SSZ-16 (AFX) using heated and pre-aged synthesis mixtures.
Microporous and Mesoporous Materials. Roč. 228, JUL 2016 (2016), s. 107-115. ISSN 1387-1811. E-ISSN 1873-3093
R&D Projects: GA ČR(CZ) GAP204/11/1206
Institutional support: RVO:61388955 ; RVO:68378271
Keywords : zeolite * synthesis * AFX
Subject RIV: CF - Physical ; Theoretical Chemistry
Impact factor: 3.615, year: 2016

The conditions of static in-situ hydrothermal synthesis were optimized to prepare crystalline, pure phase and template-free small pore zeolite SSZ-16 (AFX) particles. The type of silica source and prolonged ageing process at an elevated temperature were decisive in obtaining pure phase zeolite SSZ-16 particles under static conditions and conventional heating. Colloidal and fumed silica-based synthesis mixtures were successful in forming the zeolite SSZ-16. The zeolite particle size was reduced from 46 to 5 μm when the fumed silica was replaced by colloidal silica. Uniform, fine-grained and fully crystalline zeolite SSZ-16 particles were synthesized only from the colloidal silica-based mixtures that were aged at 80 °C for 7 days. The elevated temperature of the ageing stage is supposed to promote nucleation of viable nuclei leading to the reduction of the induction period. The two cycle calcination procedure with maximal temperature of 550 °C, ensured the removal of template molecules from the bulk phase of zeolite SSZ-16 particles. Carbonaceous residua were observed in zeolite subsurface region and mainly in the core shell morphology of zeolite SSZ-16 particles. The phase purity of zeolite SSZ-16 particles was checked by XRD and sorption properties were determined by N2 adsorption at −196 °C. Zeolite SSZ-16 particles showed the micropore volume of 0.24 cm3/g and BET surface area of 496 m2/g.
Permanent Link: http://hdl.handle.net/11104/0259103