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o 2 we s u b ne o lg h ob o i r na ns HT s e a xtremely low reactivity observed over TS-1B we were forced to work at slightly higher temperatur or experiments with this material. Nevertheless, an acceptable Arrhenius barrier of 140 kJ·mol−1 w btained over TS-1B, a two-fold increase in kinetic barrier. Figure 6. Arrhenius expression for H O decomposition over (blue squares) TS-1 22 Figure 6. Arrhenius expression for H2O2 decomposition over (blue squares) TS-1 and and (hollow red squares) TS-1B. Reaction conditions: [H2O2] = 0.25 M, mass of (hollow red squares) TS-1B. Reaction conditions: [H2O2] = 0.25 M, mass of catalyst = 50 mg, catalyst = 50 mg, various temperatures. various temperatures. 2.4. Spectroscopic Studies with in Situ Raman .4. Spectroscopic Studies with in Situ Raman To account for these interesting effects, particularly the suppression of H2O2 decomposition, we considered several possibilities. Although the treatment To accounotf vfoariotuhseszeeoilnitesrewstiitnhgNeHffeHcFts, hpaasrtbiceeunlarfloyuntdhetosuinpdpurecesssionmeofmeHso2Opo2redsecompositio 42 e considered several possibilities. Although the treatment of various zeolites with NH4HF2 has be formation [17], the impact of this was ruled out given the negligible changes observed in the porosimetry data (Table S1). Similarly, changes to the potential acid/base ound to induce some mesopores formation [17], the impact of this was ruled out given the negligib character of TS-1—an important factor in H2O2 decomposition chemistry [18]—were hanges observed in the porosimetry data (Table S1). Similarly, changes to the potential acid/ba also ruled out, based on previous observations that NH4HF2 treatment does not haracter of TchSa-n1g—e asunrfiamcepoarctiadnityf(ancetoitrheirnLHew2Ois2 ndoercBormøpnsotseidti)otno cahneymexistternyt [178]].—Flwuoerienealso ruled o analysis of TS-1B revealed that no residual fluorine remained after treatment ased on previous observations that NH4HF2 treatment does not change surface acidity (neither Lew (Table S2), and thus changes to the hydrophilicity or polarity of the catalyst based or Brønsted) to any extent [17]. Fluorine analysis of TS-1B revealed that no residual fluorine remain on fluorine are unlikely. Further indication of this was provided through FTIR fter treatment (Table S2), and thus changes to the hydrophilicity or polarity of the catalyst based spectroscopy: Although additional defect sites are indeed observed in TS-1B (ESI uorineareuFnigliukrelyS8.)F,tuhretsherdoindoitcoabtivoinouosflytchhisanwgeasthperobvsiedrevdedthdreohuygdhraFtiTonIR/reshpyedctrraotisocnopy:Althou rate compared to TS-1. The potential role of defect sites can also be ruled out dditional defect sites are indeed observed in TS-1B (ESI Figure S8), these do not obviously change t given that theoretical studies indicate these would decrease the activation barrier bserved dehydration/rehydration rate compared to TS-1. The potential role of defect sites can also for epoxidation [13], in contrast to our observed kinetics. Whilst ICP analysis also uled out given that theoretical studies indicate these would decrease the activation barrier f revealed a decrease in trace Fe content following etching (Fe content decreased from 326 to 254 ppm), control measurements investigating the ability of Fe-silicalite-1 to poxidation [13], in contrast to our observed kinetics. Whilst ICP analysis also revealed a decrease decomposeHO revealedthattheimpurityFecontentwasnotresponsibleforHO 22 22 ace Fe content following etching (Fe content decreased from 326 to 254 ppm), control measuremen vestigating the ability of Fe-silicalite-1 to decompose H2O2 revealed that the impurity Fe content w 107 ot responsible for H2O2 decomposition (ESI Table S3). The inability of this MFI material to cataly 2O2 decomposition at a similar Fe loading to that found in TS-1 as impurities clearly indicates that required for decomposition to proceed, in good agreement with previous studies [18].PDF Image | Zeolite Catalysis
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