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nn d ne e B o n n On g n e O d longer reaction times are required to induce substantial decomposition. Under reaction conditio entical to the epoxidation reaction, i.e., at 50 °C, neither catalyst decomposes more than 6% of th itial H2O2 present in the first 90 min, even in the absence of the olefin. Despite this, clear differenc tween the decomposition activities of each catalyst can be observed following NH4HF2 treatmen NH4HF2 treatment. Between 40 and 60 ◦C, TS-1 displays considerable decomposition etween 40 and 60 °C, TS-1 displays considerable decomposition activity, with conversion reachin activity, with conversion reaching a maximum of 53% over TS-1 after 270 min at maximum of 53% over TS-1 after 270 min at 60 °C (Figure 5). Whilst these values appear high, w 60 ◦C (Figure 5). Whilst these values appear high, we note that decomposition in general is substantially retarded by the co-presence of the olefin, particularly under te that decomposition in general is substantially retarded by the co-presence of the olefin, particularl the reaction conditions employed for epoxidation. The presence of an epoxidisable der the reaction conditions employed for epoxidation. The presence of an epoxidisable double bon double bond likely prohibits the Ti-(hydro)peroxo intermediate from liberating O2 via kely prohibits the Ti-(hydro)peroxo intermediate from liberating O2 via decomposition or oxidatio decomposition or oxidation. Over TS-1, an activation barrier for H2O2 decomposition ver TS-1, an activation barrier for H2O2 decomposition of 70.2 kJ·mol−1 was obtained, in excelle of 70.2 kJ·mol−1 was obtained, in excellent agreement to the values found in the open −1 literature (69–72 kJ·mol ) [14–16]. −1 ) [14–16]. reement to the values found in the open literature (69–72 kJ·mol Figure 5. Conversion versus time for H O decomposition at 60 ◦C over TS-1 22 Figure 5. Conversion versus time for H2O2 decomposition at 60 °C over TS-1 and TS-1B. and TS-1B. In contrast, H2O2 decomposition activity is almost completely suppressed following NH4HF2 treatmen In contrast, H2O2 decomposition activity is almost completely suppressed deed, even at 60 °C almost no decomposition is observed following the post-synthetic treatment, wit following NH4HF2 treatment. Indeed, even at 60 ◦C almost no decomposition is observed following the post-synthetic treatment, with a maximum conversion of 2.1% maximum conversion of 2.1% being observed under the same conditions. The suppression of H2 beingobservedunderthesameconditions.ThesuppressionofHO decomposition 22 composition is further exemplified by the Arrhenius plot in Figure 6, following calculation of th is further exemplified by the Arrhenius plot in Figure 6, following calculation of the initial rate constants over the linear region of the kinetic plot (ESI Figures S6 and S7). Due to the extremely low reactivity observed over TS-1B we were forced to work at slightly higher temperatures for experiments with this material. Nevertheless, an acceptable Arrhenius barrier of 140 kJ·mol−1 was obtained over TS-1B, a two-fold increase in kinetic barrier. 106PDF Image | Zeolite Catalysis
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