Understanding the Mechanism of Nontraditional Zeolite Synthesis Using In Situ Nuclear Magnetic Resonance Spectroscopy and X‑ray Diffraction
Nicole L. Kelly, Emma A. L. Borthwick, Gaynor B. Lawrence, Paul S. Wheatley, Arosha A. K. Karunathilake, Oxana V. Magdysyuk, David C. Lloyd, Colan E. Hughes, Kenneth D. M. Harris, Russell E. Morris, Sharon E. Ashbrook
TL;DR
This study uses NMR and X-ray diffraction to understand how nontraditional zeolites form through the ADOR process.
Contribution
The study reveals new mechanistic details of zeolite synthesis using in situ NMR and XRD.
Findings
Local structural changes in water reactions are modeled as one disassembly process.
Acid reactions involve two processes: disassembly and interlayer rearrangement.
In situ methods show both local and long-range changes are needed to understand the reaction.
Abstract
In situ solid-state nuclear magnetic resonance (NMR) spectroscopy and in situ powder X-ray diffraction (PXRD) experiments are used to develop mechanistic insights into the disassembly and organization steps of nontraditional zeolite synthesis using the ADOR (Assembly, Disassembly, Organization, Reassembly) process. The work focuses on the reaction of the germanosilicate zeolite UTL to form two ADOR intermediates: IPC-1P on reaction with water and IPC-2P on reaction with aqueous HCl. The changes in the local structure on reaction with water can be modeled as one overall disassembly process, but the long-range changes, as measured by changes in interlayer spacing determined by XRD, indicate multiple stages of the reaction as the layer structure develops. For the reaction with aqueous acid, the local changes are modeled with two processes: a disassembly and an interlayer rearrangement…
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Taxonomy
TopicsZeolite Catalysis and Synthesis · Advanced NMR Techniques and Applications · Mesoporous Materials and Catalysis