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and zeolite ZSM-5 (Figure 1d). At low TiO2 contents in both the materials from sol-gel synthesis and mechanical mixing, i.e., TZSG (25/75) and HZMM (25/75), the reflexes for anatase are scarcely observed and the zeolite reflexes dominate the XRD patterns (Figure 1c,d). Although the anatase reflexes are similarly broad for pure Hombikat and TiO2 from sol-gel synthesis (Figure 1a), they are much broader in the composite prepared by the sol-gel route when compared to the mechanical mixture (Figure 1d). This points at a higher dispersion of small TiO2 particles over the crystallites of zeolite ZSM-5 in the sol-gel-derived composites. It is also consistent with earlier literature reports showing that zeolite ZSM-5 can suppress the crystal growth of anatase during sol-gel synthesis [45]. Note also that the XRD patterns of the composites from solid-state dispersion of Hombikat and zeolite ZSM-5 are identical to those of the mechanical mixture (Figure S1). The particle size distribution in the composite from solid-state dispersion can, therefore, be assumed to be comparable to that in the mechanical mixture. Due to the overlap of the most intense anatase reflex at 2θ = 25.4 ̋ (101), the crystal size of TiO2 in the composites could, however, not be accurately determined. The differences in the textural properties of the composites from solid-state dispersion, mechanical mixing and sol-gel synthesis become clear from the N2 sorption isotherms shown in Figure 2a–c. Only minor differences are observed in the sorption isotherms for the composites from mechanical mixing and solid-state dispersion (Figure 2a,b). The composite isotherms can be described as a superposition of the isotherms of the individual components, i.e., Hombikat and zeolite ZSM-5, taking into account the corresponding mass fractions. Thus, all textural properties show additivity. This means that in all cases of these material series, the two components do not affect each other within the composite with respect to the accessibility of their pore systems. This is in accordance with the similar XRD patterns found for the HZMM and HZSSD materials with the same mass fractions. A different behavior is observed for the materials from sol-gel synthesis (TZSG-series, Figure 2c). Distinct hysteresis loops in the desorption isotherms of the H1 type [46] occur at relative pressures of P/P0 = 0.4 to 0.8 caused by the formation of mesopores during the sol-gel process. With increasing content of TiO2 in the material, the hysteresis loop shifts to higher relative pressures. Correspondingly larger mesopores are formed with increasing mass fraction of TiO2 in the TZSG-composites. 158PDF Image | Zeolite Catalysis
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