Unique Fe 3 S 4 /Cu 2 O composites were constructed with high Fentonlike photocatalytic activity through the impregnation coprecipitation method. The structure, morphology, optical, magnetic, and photocatalytic properties of the asprepared composites were explored in detail. The findings suggest that small Cu 2 O particles were grown on the surface of Fe 3 S 4 . The removal efficiency of TCH by Fe 3 S 4 /Cu 2 O was 65.7, 4.75, and 3.67 times higher than that of pure Fe 3 S 4 , Cu 2 O, and the Fe 3 S 4 + Cu 2 O mixture, respectively, when the mass ratio of Fe 3 S 4 and Cu 2 O was 1:1 at pH 7.2. The synergistic effect between Cu 2 O and Fe 3 S 4 was the main factor for TCH degradation. The Cu + species from Cu 2 O increased the Fe 3+ /Fe 2+ cycle during the Fenton reaction. • O 2 − and h + were the main active radicals; however, • OH and e − played the second role in the photocatalytic degradation reaction. Moreover, the Fe 3 S 4 /Cu 2 O composite retained good recyclability and versatility, and could be conveniently separated by a magnet.