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The rapid development of the resin industry has led to a large amount of high-concentration resin production wastewater, which has created serious water pollution problems while limiting the development of related enterprises. In this study, a combined pretreatment hydrolysis acidification/two-stage anaerobic oxic (AO) process for high-concentration resin production wastewater was constructed, and the effect of operation time on the treatment efficiency of the hydrolysis acidification and the two-stage AO unit was investigated using chemical oxygen demand (COD), total nitrogen (TN), and NH₃-H (ammonia nitrogen) as indicators. The effect of operation time on the treatment efficiency of the hydrolysis acidification and the two-stage AO unit was investigated. Results showed that the pretreatment of “alkaline digestion + ozone oxidation” could effectively remove volatile phenols and phenolic organic pollutants from the wastewater. The average removal rates of COD, TN, and NH₃-H (ammonia nitrogen) of resin production were 91.96%, 85.35%, and 85.67%, respectively. The average concentrations of final biochemical effluent were 404.7, 21.4, and 11.4 mg/L, respectively.