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Sulfamethazine (SMZ) is one of the most widely used sulfonamides and is frequently detected in water resources, posing threats to human and ecological health. To address this concern, SMZ degradation was investigated using nanoscale zero-valent iron (nZVI) supported on an organo-montmorillonite (OMt) composite (nZVI/OMt), which was synthesized by reduction of Fe²⁺ with NaBH₄, to activate persulfate (PS). Up to 97% degradation of 20 mg/L SMZ was achieved within 10 min using 1.5 mM nZVI/OMt (mass/mass, 3/1) and 4 mM persulfate at pH 6.8 and 25 °C. Experimental results indicated that SMZ degradation obeyed pseudo-first-order reaction kinetics, and the observed pseudo-first-order rate constant (k_obs) in the nZVI/OMt-activated PS process was 1.5 times that for the nZVI-activated PS process. SMZ transformation was improved by increasing the PS concentration and temperature. Natural water …