In this study, a new method for the controlled preparation of mesoporous Ti/Ce–Mn/meso–SnO2–Sb electrodes was established by introducing a Ce–Mn composite interlayer with Pluronic F127 (EO106PO70EO106) as the pore-forming agent and using a stepwise electrodeposition method. The results of the experiment indicated that the mesoporous electrodes prepared using electrodeposition had a larger specific surface area (68.37 m2 g−1), a high oxygen evolution potential (2.16 V) and good mechanical properties. The degradation extent of phenol increased from 72.34% to 91.83% and the Chemical Oxygen Demand (COD) removal extent increased from 59.31% to 81.25% within 120 min. The service life of the Ti/Ce–Mn/meso–SnO2–Sb electrode was improved nearly 15-fold compared with the conventional Ti/SnO2–Sb electrode produced using the brushing method. The results showed that the stepwise electrodeposition method can refine the coating grains. The introduction of the Ce–Mn intermediate layer increased the bonding between the coating and the Ti substrate. The mesoporous structure provided more in situ catalytic active sites and promoted the generation of •OH and catalytic oxidation of phenol. This method provides technical support and a theoretical basis for achieving controllable preparation and industrial application of high-performance titanium-based tin electrodes.
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