In order to effectively alleviate the environmental pressure, in this paper, FeTi/C nanomaterials were prepared by microwave-catalysed

pyrolysis of PVC pretreated with dechlorination using homemade FeTiOx catalysts and applied in the field of phenol degradation. The dechlorinated pre-treated PVC contains only 0.41 wt% chlorine. Pre-treated PVC was mixed with FeTiOx catalyst and placed in 800 W microwave field for pyrolysis, and it was found that the FeTiOx catalyst containing low-valent iron oxide after hydrogen reduction promoted the microwave pyrolysis process more easily than the FeTiOx catalyst containing only high-valent iron oxide, which could increase the mixture from room temperature to 700 °C in a very short period of time. As the reduction temperature of the FeTiOx catalyst increased from 450 °C to 900 °C, its particle size gradually increased and the microwave absorption heating rate accelerated synchronously; meanwhile, the titanium dioxide (TiO₂) phase was gradually formed in the system, the microscopic morphology of the pyrolytic carbon was consequently transformed from highly graphitized carbon nanotubes to low-graphitized onion-like carbon and carbon flakes, and the carbon yield decreased from 36.5 wt% to 26 wt%. The obtained FeTi/C nanomaterials efficiently degraded phenol in the water with high degradation rates of 93.08%-96.42% in 60 min, indicating that the synthesised FeTi/C nanomaterials have potential applications in organic wastewater.