Traditional planar PbO anodes have been used extensively for the electrocatalytic degradation process. However, by using porous PbO anodes that have a three-dimensional architecture, the efficiency of the process can be significantly upgraded. In the current study, carbon felt (CF) with a highly porous structure and a conventional planar graphite sheet (G) were used as electrode substrate for PbO anodes. Both CF/β-PbO and G/β-PbO anodes were prepared by the anodic deposition method. The main properties of the electrodes were characterized by XRD, EDX-mapping, FESEM, and BET-BJH techniques. The electrocatalytic degradation of diuron using three-dimensional porous CF/β-PbO anode was modeled and optimized by a rotatable central composite design. After optimizing the process, the ability of porous CF/β-PbO and planar G/β-PbO anodes to degrade and mineralize diuron was compared. The electrocatalytic degradation of the diuron was well described by a quadratic model (R > 0.99). Under optimal conditions, the kinetics of diuron removal using CF/β-PbO anode was 3 times faster than the G/β-PbO anode. The energy consumed for the complete mineralization of diuron using CF/β-PbO anode was 2077 kWh kg TOC. However, the G/β-PbO anode removed only 65% of the TOC by consuming 54% more energy. The CF/β-PbO had more stability (115 vs. 91 h), larger surface area (1.6287 vs. 0.8565 m g), and higher oxygen evolution potential (1.89 vs. 1.84 V) compared to the G/β-PbO. In the proposed pathways for diuron degradation, the aromatic ring and groups of carbonyl, dimethyl urea, and amide were the main targets for HO radical attacks.

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