As a metal-free photocatalyst, graphitic carbon nitride (g-C 3 N 4 ) has been widely used in organic pollutant degradation. However, its photocatalytic efficiency is restricted by its low absorbance of visible light and rapid electron-hole recombination rate. To enhance the catalytic activity in pollutant degradation, a hybrid photo-Fenton catalyst was prepared by coupling FeS 2 with g-C 3 N 4 via a simple hydrothermal method. Consequently, a huge enhancement in degradation efficiency was observed as the model molecule (RhB) can be completely degraded in 60 min in the presence of 5 mM H 2 O 2 under visible light irradiation. Furthermore, the catalyst shows a high stability and degradation efficiency even after 5 consecutive runs. The mechanism investigations reveal: (1) the heterostructure between FeS 2 and g-C 3 N 4 can shorten the band gap and accelerate the separation and transportation of photoexcited charge carriers; (2) the formation of the heterostructure can not only boosts Fe 2+ catalyzed ·OH production via H 2 O 2 , but also increases the formation of ·O 2 − from O 2 ; (3) the generated ·OH and ·O 2 − as well as the photoinduced holes have all contributed to the improvement of degradation efficiency. Thus present work provides a promising way of building a highly efficient photo-Fenton catalyst that is applicable in purification of wastewater. • Novel FeS 2 @g-C 3 N 4 photo-Fenton catalyst with heterojunction was fabricated. • The FeS 2 @g-C 3 N 4 exhibited high efficiency for pollutant degradation. • 50 mg/L of RhB could be completely degraded within 60 min visible irradiation. • The FeS 2 @g-C 3 N 4 showed the excellent stability and reusability. • The reasonable mechanism for RhB degradation was proposed.