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Constructing heterostructured photocatalysts and depositing an appropriate co‐catalyst to facilitate charge separation are crucial steps to improve photocatalytic H2 evolution from water splitting. Herein, we reported the synthesis of C‐doped ZrO2/g‐C3N4/Ni2P (C‐ZrO2/g‐C3N4/Ni2P) composite based on the UiO‐66‐NH2 material for photocatalytic H2 production under visible‐light irradiation. The optimal H2 evolution rate over C‐ZrO2/g‐C3N4/20 %Ni2P was 10.04 mmol g−1 h−1, which was more than 10 times higher than that of C‐ZrO2/20 %Ni2P (0.90 mmol g−1 h−1). The apparent quantum yield of C‐ZrO2/g‐C3N4/20 %Ni2P at 420 nm reached 35.5 %. A detailed analysis of the action mechanism revealed that the improved photocatalytic activity could be ascribed to the highly efficient spatial separation of the photoinduced charge carriers between C‐ZrO2 and g‐C3N4, as a result of the tightly bound structure of C‐ZrO2/g‐C3N4/20 %Ni2P and its staggered band energy. The presence of the Ni2P co‐catalyst accelerates the surface reaction as well. This work demonstrates that anchoring appropriate co‐catalysts onto a metal–organic framework (MOF)/g‐C3N4‐derived metal oxide/g‐C3N4 hybrid is an effective way to obtain heterostructured photocatalysts for H2 production.

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