SiO₂@TiO₂ core-shell nanoparticles were successfully synthesized via a simple, reproducible, and low-cost method and tested for methylene blue adsorption and UV photodegradation, with a view to their application in wastewater treatment. The monodisperse SiO₂ core was obtained by the classical Stöber method and then coated with a thin layer of TiO₂, followed by calcination or hydrothermal treatments. The properties of SiO₂@TiO₂ core-shell NPs resulted from the synergy between the photocatalytic properties of TiO₂ and the adsorptive properties of SiO₂. The synthesized NPs were characterized using FT-IR spectroscopy, HR-TEM, FE–SEM, and EDS. Zeta potential, specific surface area, and porosity were also determined. The results show that the synthesized SiO₂@TiO₂ NPs that are hydrothermally treated have similar behaviors and properties regardless of the hydrothermal treatment type and synthesis scale and better performance compared to the SiO₂@TiO₂ calcined and TiO₂ reference samples. The generation of reactive species was determined by EPR, and the photocatalytic activity was evaluated by the methylene blue (MB) removal in aqueous solution under UV light. Hydrothermally treated SiO₂@TiO₂ showed the highest adsorption capacity and photocatalytic removal of almost 100% of MB after 15 min in UV light, 55 and 89% higher compared to SiO₂ and TiO₂ reference samples, respectively, while the SiO₂@TiO₂ calcined sample showed 80%. It was also observed that the SiO₂-containing samples showed a considerable adsorption capacity compared to the TiO₂ reference sample, which improved the MB removal. These results demonstrate the efficient synergy effect between SiO₂ and TiO₂, which enhances both the adsorption and photocatalytic properties of the nanomaterial. A possible photocatalytic mechanism was also proposed. Also noteworthy is that the performance of the upscaled HT1 sample was similar to one of the lab-scale synthesized samples, demonstrating the potentiality of this synthesis methodology in producing candidate nanomaterials for the removal of contaminants from wastewater.

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