Combining photocatalytic technology with the Fenton system may help overcome these technologies’ limitations. Photo-Fenton catalysis is economical and eco-friendly. The Fe based heterogeneous photo-Fenton process appears to be a promising wastewater treatment technology. Herein, an Fe based metal–organic framework (MIL-101 (Fe)) was produced via hydrothermal processing. Subsequently, Bi2S3 was loaded onto the surface of MIL-101 (Fe) to form a composite catalyst. A type-II heterojunction was established between MIL-101 (Fe) and Bi2S3. The 10 % Bi2S3-loaded MIL-101 (Fe) (MBS-10) was effective in the photocatalytic degradation of tetracycline, particularly after H2O2 addition. This outcome was due to the enhanced generation of radical species through the photo-Fenton process. The MBS-10 photocatalyst promoted Fe (II)/Fe (III) cycling in the presence of H2O2 and under visible light irradiation. MBS-10 also showed a higher kinetic rate constant during the photocatalytic reaction compared to MIL-101 (Fe) and Bi2S3, suggesting enhanced activity through greater electron-hole separation. Furthermore, MBS-10 proved to be stable and reusable photocatalyst after four testing cycles. The charge-transfer mechanism was elucidated through radical scavenging experiments which demonstrated that superoxide and hydroxyl radicals are the major charge carriers. Therefore, the Bi2S3-MIL-101 (Fe) composite exhibits great potential for degrading tetracycline antibiotics.