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A three-dimensional electrochemical reactor with Ti/SnO₂–Sb/β-PbO₂ anode and granular activated carbon (3DER-GAC) particle electrodes were used for degradation of 2,4-dichlorophenol (2,4-DCP). Process modeling and optimization were performed using an orthogonal central composite design (OCCD) and genetic algorithm (GA), respectively. Ti/SnO₂–Sb/β-PbO₂ anode was prepared by electrochemical deposition method and then its properties were studied by FESEM, EDX, XRD, Linear sweep voltammetry and accelerated lifetime test techniques. The results showed that lead oxide was precipitated as highly compact pyramidal clusters in the form of β-PbO₂ on the electrode surface. In addition, the prepared anode had high stability (170 h) and oxygen evolution potential (2.32 V). A robust quadratic model (p-value < 0.0001 and R² > 0.99) was developed to predict the 2,4-DCP removal efficiency in the …