The development of nanocomposite photocatalysts with high photocatalytic activity, cost-effectiveness, a simple preparation process, and scalability for practical applications is of great interest. In this study, nanocomposites of TiO
2 Degussa P25 nanoparticles/activated carbon (TiO
2/AC) were prepared at various mass ratios of (4:1), (3:2), (2:3), and (1:4) by a facile process involving manual mechanical pounding, ultrasonic-assisted mixing in an ethanol solution, paper filtration, and mild thermal annealing. The characterization methods included XRD, SEM-EDS, Raman, FTIR, XPS, and UV-Vis spectroscopies. The effects of TiO
2/AC mass ratios on the structural, morphological, and photocatalytic properties were systematically studied in comparison with bare TiO
2 and bare AC. TiO
2 nanoparticles exhibited dominant anatase and minor rutile phases and a crystallite size of approximately 21 nm, while AC had XRD peaks of graphite and carbon and a crystallite size of 49 nm. The composites exhibited tight decoration of TiO
2 nanoparticles on micron-/submicron AC particles, and uniform TiO
2/AC composites were obtained, as evidenced by the uniform distribution of Ti, O, and C in an EDS mapping. Moreover, Raman spectra show the typical vibration modes of anatase TiO
2 (e.g., E
1g(1), B
1g(1), E
g(3)) and carbon materials with D and G bands. The TiO
2/AC with (4:1), (3:2), and (2:3) possessed higher reaction rate constants (
k) in photocatalytic degradation of methylene blue (MB) than that of either TiO
2 or AC. Among the investigated materials, TiO
2/AC = 4:1 achieved the highest photocatalytic activity with a high
k of 55.2 × 10
−3 min
−1 and an MB removal efficiency of 96.6% after 30 min of treatment under UV-Vis irradiation (120 mW/cm
2). The enhanced photocatalytic activity for TiO
2/AC is due to the synergistic effect of the high adsorption capability of AC and the high photocatalytic activity of TiO
2. Furthermore, TiO
2/AC promotes the separation of photoexcited electron/hole (e
−/h
+) pairs to reduce their recombination rate and thus enhance photocatalytic activity. The optimal TiO
2/AC composite with a mass ratio of 4/1 is suggested for treating industrial or household wastewater with organic pollutants.
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