This paper reports investigations in the mineralization of industrial wastewater (COD = 3246 mg/L, TOC = 2500 mg/L) using a ternary (ultrasound + Fenton + adsorption) hybrid advanced oxidation process. Fe 3 O 4 decorated activated charcoal (Fe 3 O 4 @AC) nanocomposites (surface area = 538.88 m 2 /g; adsorption capacity = 294.31 mg/g) were synthesized using coprecipitation. The wastewater treatment process was optimized using central composite statistical design. At optimum conditions, viz. pH = 4.2, H 2 O 2 loading = 0.71 M, adsorbent dose = 0.34 g/L, reduction in COD and TOC of wastewater were 94.75% and 89%, respectively. These results are attributed to synergistic interactions between the adsorption of pollutants on Fe 3 O 4 @AC, surface Fenton reactions, and enhanced mass transfer due to sonication. This synergism boosted the interactions among • OH radicals and pollutant molecules, leading to effective degradation and mineralization. The Fe 3 O 4 @AC showed excellent recovery (>90 wt %) and reusability (>90% COD removal) in 5 successive cycles of treatment.