Pyrite (FeS2) exhibits considerable promise as a photocatalyst owing to its favorable electronic and optical characteristics. In this study, the synthesis of pyrite was achieved through a hydrothermal method using ferrous sulfate heptahydrate (FeSO₄·7H₂O) and sodium thiosulfate pentahydrate (Na₂S₂O₃·5H₂O) as precursors with various ratios. Moreover, the effects of surfactants, polyethylene glycol (PEG), cetyltrimethylammonium bromide (CTAB), and added contents on the structural, morphological, and photocatalytic properties of pyrite were investigated. The properties of the synthesized materials were studied using XRD, SEM, and BET. The high specific surface area pyrite (35.69 m2/g) was successfully synthesized. The synthesis of pyrite with CTAB had a significantly higher specific surface area than pyrite without surfactant and with PEG. In addition, the content of surfactant plays an important role in the surface area value of synthesized pyrite. Photodegradation of Rhodamine B (RhB) experiments demonstrated that pyrite with CTAB exhibited superior performance, achieving up to 94.39% under visible light irradiation. The findings of this investigation suggest that pyrite synthesized in the presence of surfactants can prepare a high surface area and performance photocatalysts for wastewater treatment.