The synthesis of zeolite ETS-10 is strongly influenced by factors such as pH, the amount of the structure-directing agent, hydrothermal temperature and duration, which collectively affect the material’s morphology and structure. This study thoroughly investigates the effects of these parameters on the synthesis of ETS-10 zeolite using TiCl 3 and a waterglass solution. Characterization of the materials was performed through X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), and nitrogen isotherm adsorption-desorption at 77 K (BET-BJH) techniques. The findings indicate that pH and the structure-directing agent significantly influenced the phase composition , while hydrothermal temperature predominantly determined the crystallization rate of ETS-10. Optimal synthesis conditions were established at an initial pH of 11, employing 0.3 g of the structure-directing agent and conducting hydrothermal crystallization at 230 °C for 24 h. Under these conditions, the ETS-10 zeolite produced exhibited a high surface area of 300.1 m 2 /g, making it effective in removing Pb 2+ ions from solution. In particular, when tested under optimal conditions (pH 5) for 600 min, Pb (II) adsorption by ETS-10 reached a maximum uptake capacity of 956.19 mg/g, as determined by the Langmuir isotherm model. This capacity surpasses that of as-synthesized ETS-10 prepared from alternative Ti sources and other materials used in previous studies on Pb(II) adsorption.
An imidazolium-based ionic liquid (IL) was employed and modified by sodium lignosulfonate (LnNa) to synthesize hierarchical ETS-10 zeolite with porous structure, morphology and surface properties effectively adjusted. The template and structure-directing effects of both IL and LnNa proved to be well maintained after modification. And more importantly, the unique molecular recognition of LnNa was preserved well, while the aggressiveness of LnNa implementing through interaction with other inorganic species can be efficiently suppressed. This led to the formation of hierarchical ETS-10 zeolite with not only high crystallinity and structure integrity but also enhanced catalytic performance in aqueous-phase biomass conversion. Thus, for guaiacol hydrodeoxygenation, a notable conversion (92.8%) and cyclohexane yield (89.7%) can be acquired. This remarkable catalytic reactivity should be owing to its distinguished analogous molecular recognition pattern, promoted crystallinity, modified morphology and porous structure, and what’s more, the strengthened acid property.
Three types of metal-doped ETS-10 zeolites including Ni-ETS-10, Al-ETS-10, and Ga-ETS-10 were successfully synthesized by one-pot template-free hydrothermal treatments. The effect of doping metals on the crystallinity, morphology, textural property, and basicity of the produced zeolites was systematically studied. It was found that doping with an appropriate amount of Ni could enhance the crystallinity and basicity of ETS-10 zeolites in comparison with Al and Ga, and the Ni species mainly existed in two forms of framework coordination and exchange site connection within Ni-ETS-10. The catalytic evaluation by the liquid Knoevenagel condensation reaction of benzaldehyde with ethyl cyanoacetate confirmed the superiority of ETS-10 and metal-doped ETS-10 in comparison with the contrast base zeolites of NaY and KY. And the 0.4Ni-ETS-10 catalyst exihibted the best performance with 75.6 % yield of ethyl ɑ-cyanocinnamate (ECC) among all the synthesized (metal-doped) ETS-10 zeolites. It is reasonable to expect that the demonstrated work has important implications for the design and facile synthesis of new-type high-performance base zeolite catalysts.
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