In situ infrared spectroscopy was used to systematically study the electro-oxidation reaction information of p-toluenesulfonic acid (p-TSA) on the titanium-based lead dioxide (Ti/PbO2) electrode. The results of cyclic voltammentry curve indicated that Ti/PbO2 electrode exhibited a high electrochemical activity for the oxidation of p-TSA, and the direct oxidation potential ranged from 0.55-0.9 V. When the voltage was less than 1000 mV (vs. SCE), the multi-step potential FTIRS (MSFTIRS) and time-resolved FTIRS (TRFTIRS) analysis showed that the p-TSA was in the process of breaking of sulfonic acid group and methyl group oxidation of side-chain of benzene ring. When the voltage was higher than 1000 mV (vs. SCE), the aromatic ring of p-TSA was degradated. Meanwhile, the compounds of acid, alcohol and ketone were generated. The results of the reaction kinetics study showed that the apparent rate constant K of p-TSA electrooxidation has a linear relationship with the current density j, the removal of chemical oxygen demand (COD) increased with the increase of specific charge, and the average current efficiency showed a downward trend. © 2021, Editorial Board of CIESC Journal. All right reserved.