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Chlorophenols (CPs) are a kind of important organic chemical intermediates, which are produced in various industrial processes. Currently, electrochemical method is the most effective treatment for the degradation of chlorophenols (CPs) in wastewater. In this study, a three-dimensional electrode electrochemical reactor, constructed using the Sn/Sb-Mn-GAC (granular activated carbon) particle electrodes, was used to treat the wastewater containing 4-chlorophenol. On the basis of single factor experiments, the process conditions of the designed three-dimensional electrochemical reactor were optimized using the response surface methodology. The experimental results showed that the three-dimensional electrochemical reactor could effectively reduce 4-chlorophenol by 96.13% at the optimum Na2SO4 concentration of 2 g·L−1, electrode plate distance of 2 cm, current intensity of 2 A, and particle electrode dosage of 14 g. The experimental observations were in reasonable agreement with the modeled values, thus verifying the design of the proposed reactor.