Fe-doped NaBiO nanoscaled compounds were prepared by hydrothermal method and evaluated as a highly efficient photo-Fenton-like catalyst under visible light irradiation. The Fe-doped NaBiO compound had a specific surface area of 41.42 m g, which is considerably larger than that of NaBiO nanoparticles (28.81 m g). The compound exhibited an excellent visible light-Fenton-like catalysis activity, which is influenced by the iron content of the compound and the pH value of the solution. Under the optimal conditions, the Fe-doped NaBiO compound led to fast degradation of Nonylphenol with an apparent rate constant of 5.71 × 10 min, which was 8.23-fold of that achieved by using NaBiO. The significantly enhanced visible light-Fenton-like catalytic property of the Fe-doped NaBiO was attributed to the large surface area and the high adsorption capacity of the compound, and the Fenton catalytic ability of iron in the compound.