In this study, we report the fabrication of hollow reduced graphene oxide microspheres with well-distributed Fe2O3 nanoparticles (Fe-rGOS) via a spray-drying methodology. L-Ascorbic acid was-employed to reduce graphite oxide (GO) and improve velocity of electrons transfer. Because of L-ascorbic acid and the spray-drying procedure, the in situ Fe2O3 nanoparticles with a mean size of 5-10 nm were uniformly deposited on rGO support and the rGO migrated to the surface of the drop to form microspheres. The well dispersed nanoparticles not only generated more active sites-and interface contact which was beneficial to enhance the stability of catalysts but also acted as pillars between the rGO layers to achieve mesoporous structure. The formed mesoporous frameworks enhanced mass transfer to a large extent and led to the much better catalytic efficiency. Therefore, the prepared Fe-rGOS exhibited a remarkable photocatalytic activity in a wide pH range and superior recyclability with low leaching of iron ions.