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Radioactive waste management is critical for maintaining the sustainability of nuclear fuel cycles. In this study, we propose a novel bismuth-based reduced graphene oxide (Bi0–rGO) composite for the immobilization of off-gas radioactive iodine. This material synthesized via a solvothermal route exhibited a low surface area (2.96 m2/g) combined with a maximum iodine sorption capacity of 1228 ± 25 mg/g at 200 °C. The iodine sorbent was mixed with Bi2O3 powder and distilled water to fabricate waste matrices, which were cold-sintered at 300 °C under a uniaxial pressure of 500 MPa for 20 min to achieve a relative density of ∼98% and Vickers hardness of 1.3 ± 0.1 GPa. The utilized methodology reduced the iodine leaching rate by approximately 3 orders of magnitude through the formation of a chemically durable iodine-bearing waste form (BiOI). This study demonstrates the high potential of Bi0–rGO as an innovative solution for the immobilization of radioactive waste at relatively low temperatures.