Pelargonic acid vanillylamide (PAVA), a capsaicin-type dacryagogue agent utilized for counter-terrorism and riot control, possesses a low stimulus threshold. This characteristic can lead to environmental contamination following its application and may easily result in secondary stimulation to personnel. Cobalt-doped Ti3C2-MXene nanosheets (Co3O4/Ti3C2@C) were synthesized for the purpose of activating peracetic acid (PAA) and degrading PAVA. A carbon layer was coated on the surface of Ti3C2-MXene nanosheets to address the challenge of poor oxygen resistance in MXenes, thus preventing a significant decline in surface reactivity. The BET surface area of Co3O4/Ti3C2@C was expanded to 149.6 m2/g, significantly exceeding that of Ti3C2 (13.0 m2/g) and Co3O4 (56.4 m2/g). With 0.5 mg/mL of Co3O4/Ti3C2@C and 0.35 mM of PAA, 100 mg/L of PAVA was completely degraded within 60 min. The augmented BET surface area and the presence of more active sites confer remarkable PAA activation and catalytic degradation properties toward PAVA. Parameters such as initial pH, PAVA concentration, catalyst dosage, and PAA concentration on PAVA degradation were systematically assessed. Furthermore, the reusability and stability of the nanocomposite were substantiated through recycling tests. Radical quenching experiments and electron paramagnetic resonance analysis demonstrated the acetylperoxy radical (CH3CO3) as the primary species responsible for PAVA degradation. This research serves as an illustration of the utilization of MXene and transition metal activated PAA in wastewater treatment.