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Switching off H2O2 Decomposition during TS-1 Catalysed Epoxidation via Post-Synthetic Active Site Modification Ceri Hammond and Giulia Tarantino Abstract: Despite its widespread use, the Lewis acidic zeolite, TS-1, still exhibits several unfavourable properties, such as excessive H2O2 decomposition, which decrease its overall performance. In this manuscript, we demonstrate that post-synthetic modification of TS-1 with aqueous NH4HF2 leads to modifications in epoxidation catalysis, which both improves the levels of epoxide selectivity obtained, and drastically minimises undesirable H2O2 decomposition. Through in situ spectroscopic study with UV-resonance enhanced Raman spectroscopy, we also observe a change in Ti site speciation, which occurs via the extraction of mononuclear [Ti(OSi)4] atoms, and which may be responsible for the changes in observed activity. 1. Introduction Over recent decades, remarkable achievements have been observed in the design of Lewis acidic zeolites [1–3]. The biggest breakthrough in this context is titanium silicalite-1 (TS-1), which is a crystalline, porous, MFI-type zeolite doped with a low quantity of framework TiIV atoms [4]. Possessing active Lewis acid sites, TS-1 has been shown to be an exceptional catalyst for a wide range of oxidation challenges, including olefin epoxidation, aromatic hydroxylation and ketone ammoxidation, amongst others. The unique reactivity of TS-1 is attained when it is reacted at relatively mild conditions with hydrogen peroxide (H2O2), an oxidant with high potential in the area of sustainable chemistry. A pertinent example of this catalysis is the recently commercialised “hydrogen peroxide to propylene oxide” (HPPO) process [5,6]. Despite its industrial exploitation, conventional TS-1 catalyst still exhibits some unfavourable properties. Particularly when employed to perform epoxidation reactions, decreases in epoxide selectivity at high levels of conversion, and the undesirable decomposition of H2O2, yielding O2, are two of its major disadvantages. The second is especially problematic, as unnecessary H2O2 decomposition leads both to decreased economic performance through loss of a relative expensive oxidant, and safety concerns associated with the generation of O2 in the system. Reprinted from Catalysts. Cite as: Hammond, C.; Tarantino, G. Switching off H2O2 Decomposition during TS-1 Catalysed Epoxidation via Post-Synthetic Active Site Modification. Catalysts 2015, 5, 2309–2323. 100PDF Image | Zeolite Catalysis
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