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A sol–gel synthesis technique was employed for the preparation of anatase phase {001}-TiO2/Au hybrid nanocomposites (NCs). The scalable, schematic, and cost-efficient method was successfully modified using HF and NH4OH capping agents. The photocatalytic activity of the as-synthesized {001}-TiO2/Au NCs were tested over 2-cycle degradation of methylene blue (MB) dye and pharmaceutical active compounds (PhACs) of ibuprofen and naproxen under direct sunlight illumination at 35 °C and 44,000 lx. Transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), fast Fourier transform (FFT), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDS), and ultraviolet–visible diffuse reflectance spectroscopy (UV–Vis DRS) were employed for the characterization of the as-prepared sample. The characterization results from the TEM, XPS, and XRD studies established both the distribution of Au colloids on the surface of TiO2 material, and the presence of the highly crystalline structure of anatase {001}-TiO2/Au NCs. Photodegradation results from the visible light irradiation of MB indicate an enhanced photocatalytic performance of Au/TiO2 NCs over TiO2. The results from the photocatalytic activity test performed under direct sunlight exposure exhibited promising photodegradation efficiencies. In the first cycle, the sol–gel synthesized material exhibited relatively better efficiencies (91%) with the MB dye and ibuprofen, while the highest degradation efficiency for the second cycle was 79% for the MB dye. Pseudo first-order photodegradation rates from the first cycle were determined to be comparatively slower than those from the second degradation cycle.

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