In this work, Fe3O4/FeS2/g-C3N4 nanocomposites were developed for catalytic hydrogen generation from sodium borohydride. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and environmental scanning electron microscopy (ESEM) were used to analyze these nanocomposites. The XRD diffraction peaks of Fe3O4 and FeS2 cubic phase showed an average crystal size of calculation of 15 and 20 nm. ESEM micrographs showed a 2D broken up sheet structure having more edge sites. The BET surface areas for S@g-C3N4, 1.0, 2.0, and 3.0 wt% Fe3O4/FeS2 were 40, 109, 137 and 162 m2/g, respectively. Even though Fe3O4/FeS2 were incorporated into the nanosheet, the pore size was increased from 2.0 to 2.15 nm. S@g-C3N4 has an average band gap of 2.60 eV that decreased to 2.30, 2.21 and 2.18 eV at 1.0, 2.0 and 3.0 wt% of FeS2. In addition, Fe3O4/FeS2/g-C3N4 nanosheets showed an emission band at 460 nm. Moreover, the intensity of this band decreased as the content of Fe3O4/FeS2 reached 3.0 wt%. The rate of hydrogen production is accelerated as the percentage of Fe3O4/FeS2 increased from 1.0 to 3.0 wt%. The sample 3.0 wt% Fe3O4/FeS2 showed the best rate of hydrogen production (8480 mL/g·min).