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3. ExperimentalSection 3.1. Catalyst Synthesis and Pre-Treatment TS-1 was prepared according to a method described elsewhere [29]. TS-1B was prepared as follows. TS-1 (4 g) was suspended in an aqueous solution (80 mL) containing NH4HF2 (120 mg) and H2O2 (50 wt. %, 3.2 mL). The slurry was stirred for 4 h at 80 ◦C, prior to filtration. The sample was finally dried overnight (110 ◦C, 16 h). 3.2. Catalyst Characterization Powder X-ray diffraction was performed on a PANalytical X’PertPRO X-ray diffractometer (PANalytical, Almelo, the Netherlands), with a CuKα radiation source (40 kV and 30 mA). Diffraction patterns were recorded between 6◦ and 55◦. FTIR spectroscopy was performed on a Bruker Tensor spectrometer (Bruker Corporation, MA, USA) over a range of 4000–650 cm−1 at a resolution of 2 cm−1. UV-Vis analysis was performed on an Agilent Cary 4000 UV-Visible Spectrophotometer (Agilent Technologies, CA, USA) in Diffuse Reflectance mode. Samples were measured between 190 and 800 nm at 600 nm·min−1 scan rate. Ti content and Si/Ti molar ratios were determined by EDX. Specific surface area was determined from nitrogen adsorption using the BET equation, and microporous volume was determined from nitrogen adsorption isotherms using the t-plot method. Porosimetry measurements were performed on a Quantachrome Autosorb (Quantachrome, FL, USA), and samples were degassed prior to use (275 ◦C, 3h). Adsorption isotherms were obtained at 77 K. UV-Raman spectroscopy was performed on a Renishaw inVia spectrometer (Renishaw plc, Gloucestershire, UK) equipped with laser lines at 785, 514, 325 and 266 nm. Laser power was kept at or below 10 mW for solid powders, and at or below 2 mW for in situ measurements with H2O2. 3.3. Kinetic Evaluation and Analytical Methods Allyl alcohol epoxidation was performed in a 100 mL round bottom flask equipped with a reflux condenser, thermostatically controlled by immersion in a silicon oil bath. The vessel was first charged with a 10 mL solution of allyl alcohol in methanol (0.5 M), which also contained an internal standard (biphenyl, 0.025M). The desired amount of catalyst (50 mg) was also added. The mixture was subsequently heated to the desired temperature (stated in the manuscript, all temperatures correspond to the oil temperature outside the reactor), and the reaction was initiated by addition of an appropriate amount of H2O2 (0.25 M, corresponding to a 1:2 H2O2:olefin ratio). The solution was stirred at ±750 rpm with an oval magnetic stirrer bar. Aliquots of reaction solution were taken periodically for analysis, and were centrifuged prior to injection into a GC (Agilent 7820 (Agilent Technologies, CA, USA), 25 m CP-Wax 52 CB column). Reactants were quantified against the 113PDF Image | Zeolite Catalysis
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