Persulfates work effectively in a wide pH range and present great potential for wastewater purification. However, the development of efficient, cost-effective, and environmentally friendly heterogeneous catalysts is still challenging. In this study, an innovative catalyst for peroxymonosulfate (PMS) activation to degrade target contaminant atrazine is proposed. The catalyst is based on a combination of Cu-Fe spinel (CuFe2O4) and aluminium oxide (γ-Al2O3). The samples synthesised were fully characterised by X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy. The results show that all composite catalysts (CCs) had greater catalytic reactivity than spinel; the degradation of atrazine increased from 49%-94% when Cu-Fe spinel was replaced by a composite catalyst (CuFe2O4: γ-Al2O3 = 1:1; CC1). When the loading of Cu-Fe metals was equivalent, the pseudo-first-order rate constant with CC1 (0.37 min–1) was around 37 times that with Cu-Fe spinel (0.01 min–1). Both sulfate radicals and hydroxyl radicals were found to be the active species generated during the activation of PMS by CCs, and sulfate radicals were primarily responsible for the degradation of atrazine. The findings from this study will contribute to the advancement of wastewater treatment technology in Hong Kong and the rest of the world.