Coal fly ash (CFA) based-copper ferrite nanocomposites were fabricated, characterized, and applied for the photocatalytic degradation of Methyl Orange (MO) dye. The hydrothermal synthesis route was opted for the fabrication of pristine copper ferrite nanoparticles and its CFA nanocomposites. The prepared photocatalysts were analyzed in terms of structural, surface morphology, chemical state analysis, elemental composition, and optical response. The photocatalytic activity of nanocomposites was investigated sequentially under ultraviolet light (254 nm) and influencing parameters (pH, H 2 O 2 dose, photocatalyst content, dye initial concentration, irradiation time) were studied. The optimized conditions for photocatalytic degradation were found at pH= 5, composite dose= 100 mg/L, H 2 O 2= 10 mM using CFA nanocomposite and the dye was efficiently degraded within 60 min. The best degradation efficiency of~ 98% was achieved using CFA-CuFe 2 O 4 (1: 1) under the optimized conditions. The key reactive species (radical dot OH, h+, and e−) for photocatalytic degradation were determined by a radical scavenging experiment and radical dot O H radicals were found to be the most effective ones. The kinetic study of Fenton oxidation processes was conducted using Behnajady-Modirshahla-Ghanbery (BMG) kinetic model. Response surface methodology was the statistical tool for the assessment of interaction effect among experimental variables.