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A novel phosphorus‐doped graphitic carbon nitride nanosheets (PS‐CN) photocatalyst was prepared by thermal polycondensation and thermal stripping method, and its physicochemical properties were characterized. The results show that PS‐CN formed a thin sheet and multi‐cavity structure by thermal delamination that could enhance the surface area, light reception, and adsorption capacity. The prepared PS‐CN activated sodium percarbonate system (PS‐CN/SPC) was developed for the degradation of dyeing wastewater with methylene blue (MB) as the target pollutant and the degradation mechanism was analyzed. At room temperature (20 °C), the degradation rate of MB in PS‐CN/SPC system within 10 min (88.13 %) was three times that of pure g‐C3N4. In addition, the MB was completely degraded under visible light within 60 min. Moreover, PS‐CN exhibited excellent reusability that the degradation rates of MB have remained above 96 % in five consecutive cycles. The free radical quenching experiments showed that hole (h+), hydroxyl radical (•OH) and superoxide radical (•O2−) all participated in MB degradation, and •OH was the main active species. The PS‐CN/SPC system would provide a high‐value solution for the treatment of dye wastewater due to the low cost of raw materials, superior photocatalytic activity, simple synthesis method, and reusability of the catalyst. [ABSTRACT FROM AUTHOR]