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biphenyl internal standard. Conversion was calculated as follows: Conversion = Σ[products, M]/[H2O2]0 × 100. All chemicals were purchased from Sigma-Aldrich (St. Louis, MO, USA). 4. Conclusions Titanium silicalite-1 is a uniquely active catalyst for a range of commercial scale oxidation reactions. In this manuscript, we demonstrate that treatment of TS-1 with NH4HF2 leads to a change in Ti site speciation. Through UV-Vis, FTIR and UV-resonance enhanced Raman spectroscopy, we interpret this change as being related to the extraction of mononuclear [Ti(OSi)4] atoms from the zeolite framework, and the generation of new active Ti species that are present in extra-framework sites of the structure. These new active sites may be responsible both for the changes in epoxidation catalysis observed (increased selectivity, modified temperature dependence), and also for significant improvements in H2O2-based selectivity, as non-selective H2O2 decomposition is found to be drastically decreased following post-synthetic treatment of TS-1 with NH4HF2. Acknowledgments: C.H. gratefully appreciates the support of The Royal Society for the provision of a University Research Fellowship (UF140207) and additional research funding (RG140754). Author Contributions: C.H. Conceived and designed the experiments and guided the research. G.T. and C.H. performed characterization and catalytic studies. C.H. performed the Raman measurements. Both authors contributed to the writing of the manuscript. Conflicts of Interest: The authors declare no conflict of interest. References 1. Corma, A.; Garcia, H. Lewis Acids as Catalysts in Oxidation Reactions: From Homogeneous to Heterogeneous Systems. Chem. Rev. 2002, 102, 3837–3892. 2. Moliner, M. State of the Art of Lewis Acid-Containing Zeolites: Lessons From Fine Chemistry to New Biomass Transformation Processes. Dalton Trans. 2014, 43, 4197–4208. 3. Dapsens, P.Y.; Mondelli, C.; Perez-Ramirez, J. Design of Lewis-acid centres in zeolitic matrices for the conversion of renewables. Chem. Soc. Rev. 2015, 44, 7025–7043. 4. Ratnasamy, P.; Srinivas, D.; Knözinger, H. Active Sites and Reactive Intermediates in Titanium Silicate Molecular Sieves. Adv. Catal. 2004, 48, 1–169. 5. Cavani, F.; Teles, J.H. Sustainability in Catalytic Oxidation: An Alternative Approach or Structural Evolution? ChemSusChem 2009, 2, 508–534. 6. Cavani, F. Catalytic Selective Oxidation: The Forefront in the Challenge for a More Sustainable Chemical Industry. Catal. Today 2010, 157, 8–15. 114PDF Image | Zeolite Catalysis
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