Rapid activation of sodium persulfate (SPS) for the degradation of C.I. Reactive Red 218 (RR218) was achieved using Ti3C2 MXene reduction of trace Fe3+. The degradation rate of RR218 reached 97.7% using a mixture containing 3 g L−1 of SPS, 3.35 mg L−1 of Fe3+ and 60 mg L−1 of MXene stirred at 25 °C for 30 min. The intense reduction of Ti3C2 MXene triggers the Fe3+/Fe2+ cycle thereby accelerating the activation of SPS. When reactive dyes were degraded by Fe3+/SPS/MXene process, ·OH played a major role. The dye degradation capacity of the Fe3+/SPS/MXene process decreased after 5 cycles of recycling. In addition, the wastewater treated under these conditions resulted in high dyeing efficiencies in reuse experiments. This study not only improves the understanding of the catalytic reaction of MXene but also provides a wastewater treatment and reuse process with low metal consumption and high efficiency.