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In this work, a hematite/porous graphite carbon-nitride (α-Fe₂O₃/g-C₃N₄) catalyst was synthesized through the doping of hematite loaded onto porous graphite carbon-nitride using a heat treatment process. Then, the ability of catalyst was evaluated to degrade diazinon (DZN) for the first time, mainly via the sonophotocatalytic process. Among the samples, the greatest DZN degradation was observed in the sonophotocatalytic system, which separated 100% of DZN from the aqueous solution after 50 min, while the removal percentages for the sonocatalytic, photocatalytic, and adsorption systems were 72.9, 89.1, and 58.1%, respectively. The results of scavengers showed that both sulfate and hydroxyl radicals (^•OH) participated in removing DZN, although positive holes and negative ^•OH played a major role. Moreover, the removal efficiencies of the target pollutant using the sonophotocatalytic process were higher than those using the photocatalytic, sonocatalytic, and adsorption processes. The reaction profile followed pseudo-first-order kinetics, and the reaction rate coefficient for the sonophotocatalytic system was 2.2 times higher than that of the photocatalytic system and 2.64 times higher than that of the sonocatalytic system. The energy consumption of the sonophotocatalytic system after 60 min was 11.6 kWh/m³, while it was 31.1 kWh/m³ for the photocatalytic system. A DZN removal percentage of 100% was obtained after 50 min under the following conditions: UV intensity of 36 watts, ultrasound frequency of 36 kHz, DZN concentration of 50 mg/L at pH 5, and α-Fe₂O₃/g-C₃N₄ dosage of 0.4 g/L. The catalyst reusability was examined with only a 9.9% reduction in efficiency after eight consecutive cycles. The chemical oxygen demand (COD) and total organic compound (TOC) removal percentages were 95.6% and 88.6%, respectively, and the five-day biochemical oxygen demand (BOD₅)/COD ratio was 0.16 at the beginning of the degradation process and 0.69 at the end of the process. In addition, toxicological experiments showed that degradation of DZN by the sonophotocatalytic process exhibited low toxicity. All results confirmed that the sonophotocatalytic process using α-Fe₂O₃/g-C₃N₄ was a highly efficient process for DZN pollutant removal from liquid wastes.