The water produced by alkaline–surfactant–polymer (ASP) flooding is difficult to treat due to the presence of residual chemicals. Therefore, research and development of efficient and low-cost methods for the treatment of ASP flooding produced water is necessary. Chemical destabilization is the most common and effective way to treat the produced water. This paper describes an optimization method for demulsification and flocculation. Some demulsifiers and flocculants commonly used in oilfields were screened, compounded, and optimized. Since the effect of treatment using only demulsifier or flocculant to treat the produced water is often not enough to meet the reinjection standard, an orthogonal experiment was carried out to study the demulsification–flocculation method to treat produced water. Five main influencing factors of the oil concentration were investigated. Based on the results of the range analysis and the relationship between the five factors and oil concentration, the order of significant factors was found to be demulsifier dosage > flocculant dosage > settling time > stirring time > stirring intensity, and the optimal demulsification–flocculation treatment conditions were successfully optimized.