Organic Sodium Salt‐Assisted Synthesis of Multi‐Defective Highly Dense Structural Carbon Nitride for Efficient Photocatalytic H2O2 Production

Abstract The construction of multi‐defective highly dense structural CN with a large surface area has shown great promise in photosynthesis of H 2 O 2, whereas there remains a great challenge. In the present work, a novel and facile approach is proposed to prepare porous carbon nitride (CN) enriched with cyano groups, nitrogen vacancies, sodium doping, and oxygen‐containing functional groups by pre‐constructing sodium‐containing supramolecular precursors under the assistance of sodium dichloroisocyanurate (DCCNa) with subsequent pyrolysis, which integrates the merits of alkali‐metals‐assisted pyrolysis and supramolecular structures. Such multi‐defective features not only improve the visible light absorption capacity and oxygen reduction ability but also facilitate efficient separation and transfer of photo‐generated electrons and holes, which is beneficial to enhance its photocatalytic performance for H 2 O 2 production. The optimal CN‐DCCNa 0.5 exhibits a high H 2 O 2 yield of 1032.8 µ m within 4 h, which is 8.32 times higher than pristine CN (123.2 µ m ). This study provides new insights into optimizing CN‐based photocatalysts for efficient and green photocatalytic H 2 O 2 synthesis.