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a second mesopore into TS-1 zeolite crystals to form hierarchical structured TS-1 is an efficient strategy [15–21]. While significant achievements have been realized in this approach, the methods employed usually involved either cost-intensive mesostructured templates [15,19–21] or complex synthetic procedures [17,18]. In this regard, synthesis of TS-1 zeolite-based composites is an alternative approach. Recently, hierarchical core-shell structured composites with a microporous zeolite crystal core and a mesoporous silica/carbon shell have received much attention [22–27] and have been widely applied in the some important catalytic reactions, such as epoxidation of alkene [23], cyclohexanone ammoximation [24], methanol to propylene (MTP) conversion [22] and catalytic cracking of large molecules [25]. Owing to the unique structural properties and the bimodal pore structure with open junction and retainable diffusion efficiency, these zeolite-based core-shell composite materials exhibit superior catalytic activity and selectivity. Moreover, multifunctional core-shell composites with various catalytic sites have been also designed to catalyze one pot cascade reactions. For-example, Rh(OH)3 species were supported on the core-shell structured TS-1@KCC-1 composite for one-pot synthesis of benzamide from benzaldehyde, ammonia and hydrogen peroxide [28]. However, TS-1 zeolite-based yolk/core-shell composites have been rarely reported for application in hydroxylation of phenol. In the current work, we devoted our efforts to study the catalytic properties of TS-1 zeolite-based yolk/core-shell composites in the hydroxylation of phenol and determine the relationship between the mircostructure of the material and its catalytic performance. To study the catalyzed hydroxylation of phenol, specifically we prepared yolk/core-shell structured TS-1@mesosilica composites and used H2O2 as the oxidant. The core-shell structured TS-1@mesosilica composite was prepared via a uniform coating process, whereas the yolk-shell structured TS-1@mesosilica composite was prepared, for the first time, using a resorcinol-formaldehyde resin (RF) middle-layer as the sacrificial template. The obtained materials were characterized by X-ray diffraction (XRD), N2 sorption, FT-IR, UV-Visible spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). 2. ResultsandDiscussion 2.1. Synthesis and Characterization of CS-TS-1@mSiO2 The micro-sized TS-1 single crystal was prepared by hydrothermal method. The SEM image (Figure 1a) and TEM image (Figure 2a,b) indicate that the TS-1 sample consist of uniform monodisperse nanocrystals with a particle size of 290–350 nm. Core-shell structured TS-1@mesosilica composites (designated as CS-TS-1@mSiO2−x, x is the thickness of mSiO2 layer) were obtained through a uniform coating process using water-ethanol (2:1), ammonia aqueous, CTAB (hexadecyltrimethylammonium 141PDF Image | Zeolite Catalysis
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