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The weaker van der Waals force between layers inhibits the interlayer electron migration, which greatly limiting the enhancement of the photocatalytic activity over graphitic carbon nitride (g-C 3 N 4). Herein, the metal-free sulfur-doped 2D/3D van der Waals (vdW) homojunction (2D/3D CNSCN) that containing 2D sulfur-doped g-C 3 N 4 nanosheets (CNS) and 3D g-C 3 N 4 flower-like hierarchical structure (CN) was fabricated. Thanks to the cooperative effect of 2D-3D structural and good compatibility between CNS and CN, an in situ formed 2D/3D vdW homojunction served as the driving force for promoting charge carrier separation and transfer. The optimal photocatalytic H 2 evolution of 2D/3D CNSCN reached up to 2196 μmol h−1g−1, which was 4.1 and 3.2 times higher than that of CN and CNS, respectively. 10 mg of the 2D/3D CNSCN photocatalyst was able to totally remove of rhodamine B (RhB) solution in less than 80 min under the visible light. This study provides new opportunities to construct novel 2D/3D mixed-dimensional vdW homojunction, and broad interest in vdW homojunction research for the applications in energy conversion and environmental protection field. [Display omitted] • 2D/3D mixed-dimensional vdW homojunction of CN is prepared for the first time. • CNSCN has high activity and stability in photocatalytic H 2 evolution and removing RhB. • The optimal photocatalytic H 2 evolution of 2D/3D CNSCN reaches up to 2196 μmol h−1g−1. • CNSCN exhibits ultrahigh charge-carrier separation and transfer efficiency. • A possible photocatalytic mechanism is proposed. [ABSTRACT FROM AUTHOR]