Activated carbon (AC) is a porous, amorphous form of carbon known for its strong adsorption capacity, making it highly effective for use in wastewater treatment. In this investigation, AC-based nanocomposites (NCs) loaded with zirconium dioxide and cerium dioxide nanoparticles (ZrO2/CeO2 NPs) were successfully synthesized for the effective elimination of methylene blue (MB) and tetracycline hydrochloride (TCH). The AC-ZrO2/CeO2 NCs have a size of 231.83 nm, a zeta potential of -20.07 mV, and a PDI value of 0.160. The adsorption capacities of AC-ZrO2/CeO2 NCs for MB and TCH were proved in agreement with the Langmuir isotherm and pseudo 1st-order kinetic model, respectively. The maximum adsorption capacities were determined to be 75.54 mg/g for MB and 26.75 mg/g for TCH. Notably, AC-ZrO2/CeO2 NCs exhibited superior photocatalytic degradation efficiency for MB and TCH under sunlight irradiation with removal efficiencies reaching up to 95% and 79% within 90 min, respectively. The t1/2 for the photo-degradation process of MB and TCH were 11.55 min and 44.37 min. Analysis of active species trapping confirmed the involvement of hole (h+), superoxide anion (•O2−), and hydroxyl radical (•OH) in the degradation mechanism. Furthermore, the residual solution post-contaminant removal exhibited minimal toxicity towards Artemia salina and NIH3T3 cells. Importantly, the NCs did not exhibit antibacterial activity against tested pathogens post-absorption/degradation of TCH. Thus, AC-ZrO2/CeO2 NCs could be a promising nanomaterial for wastewater treatment applications.