| Summary: | Fenton reaction is a powerful technology for pollutants’ removal from water. However, the cost of H<sub>2</sub>O<sub>2</sub> becomes one of the major stumbling blocks in its application. H<sub>2</sub>O<sub>2</sub> has a relatively high price and is easily decomposed during transportation and use; therefore, in situ synthesis of H<sub>2</sub>O<sub>2</sub> could improve economic benefits effectively. In this study, a Fe/Ni/Pd ternary metal-doped graphitic carbon nitride (FeNi-Pd@CN) is prepared, and in situ H<sub>2</sub>O<sub>2</sub> generation using formic acid as hydrogen sources for organics removal was proved. The catalyst is advantageous, as H<sub>2</sub>O<sub>2</sub> could accumulate to 1.69 mmol/L in 150 min when pumping air rather than oxygen gases in other studies. Furthermore, 92.0% of Acid Red 73 (200 mg/L) and 93.2% of tetracycline hydrochloride (10 mg/L) could be removed in 150 min without any pH adjustment. Characterization results show that the catalyst has good stability in metal leaching and reuse tests. It is proved that •OH and •O<sub>2</sub><sup>−</sup> are the main reactive oxygen species, and a synergistic effect between Fe and Ni exists that enhances ROS generation for organics degradation. This work offers a promising method to remove refectory organic contaminants from industrial wastewater.
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