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formation of the relevant Ti-(hydro)peroxo species. We note that the original spectrum can be restored by a heat treatment at 90 °C, and may even partially be restored by extended scanning under the Raman beam. Figure 9. In situ UV-Raman (325 nm) spectra of (blue) TS-1 and (purple) TS-1 treated Figure 9. In situ UV-Raman (325 nm) spectra of (blue) TS-1 and (purple) TS-1 treated with H2O2. with H2O2. Similarly, the residual 960 and 1125 cm−1 stretches in TS-1B are also eliminated upon treatment with Similarly, the residual 960 and 1125 cm−1 stretches in TS-1B are also eliminated H2O2, confirming that at least some of the original active site remains following NH4HF2 treatment. upon treatment with H2O2, confirming that at least some of the original active site However, it is also notable that the 695 cm−1 band, which has been attributed to the −n1ew 270 nm remains following NH4HF2 treatment. However, it is also notable that the 695 cm UV-Vis absboarnbda,nwcehibcahnhda,sibseaenlsoatterliibmutiendatteodthfreonmewth2e70RnamaUnV-sVpiescatrbusmorbuapnocen bcaonodr,diisnaltsion of H2O2. eliminated from the Raman spectrum upon coordination of H O . The total loss of The total loss of this Raman band confirms (i) that this Raman mod2e a2rises from a species whose this Raman band confirms (i) that this Raman mode arises from a species whose vibrational signature is destroyed upon coordination of H2O2; and (ii) that the new active site formed vibrational signature is destroyed upon coordination of H2O2; and (ii) that the new following NH4HF2 treatment reacts with H2O2, indicating that this species also provides a route toward active site formed following NH4HF2 treatment reacts with H2O2, indicating that H2O2 activation. From the characterization data obtained thus far, we assign this change in Ti speciation this species also provides a route toward H2O2 activation. From the characterization to the extracdtaiotanobftafrinamedewthourskfa[Tr,i(wOeSai)s4s]igantotmhis,cahnadngtoe tinheTciospnceucirarteinotngteontehreateixotnraocftinoenwofactive sites. framework [Ti(OSi) ] atoms, and to the concurrent generation of new active sites. Given that a redistribution of4Ti from one T-site to another would not change the intensity of the Given that a redistribution of Ti from on−e1 T-site to another would not change the breathing mode of the [Ti(OSi)4] atoms at 1125 cm , it is likely that the new active sites are located in intensity of the breathing mode of the [Ti(OSi)4] atoms at 1125 cm−1, it is likely that extra-framework positions of the zeolite. the new active sites are located in extra-framework positions of the zeolite. At this time, we are not able to conclusively attribute the modified kinetic behaviour to the generation of extra-framework Ti species. Yet, the in situ UV-Raman data and the absence of any other contributing factors (see above) strongly suggest that these factors are related. We consider there to be two potential ways that the extraction of framework Ti could lead to such pronounced changes. The first possibility is that NH4HF2 treatment removes a particularly non-selective framework [Ti(OSi)4] site, responsible for both epoxidation and undesirable decomposition. Alternatively, the extraction of framework Ti could 111PDF Image | Zeolite Catalysis
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