Sonochemical Synthesis of Benzodifuran‐Based Conjugated Polymers for Efficient Photocatalytic H 2 O 2 Production

Photocatalytic O 2 reduction to H 2 O 2 offers a sustainable route for green H 2 O 2 production. However, the rapid and scalable preparation of efficient organic polymer photocatalysts remains challenging. Herein, we report a sonochemical strategy for the gram‐scale synthesis of two novel benzodifuran‐based conjugated polymers, BDF‐CP1 and BDF‐CP2, in aqueous solution without the use of any additional organic solvent. This methodology allows rapid assembly of conjugated architectures within drastically curtailed reaction periods, whose optical absorption profiles and morphological characteristics are comparable to those derived from conventional solvothermal protocols. More importantly, benefiting from its donor–acceptor skeleton, triazine‐linked BDF‐CP1 displays efficient charge transfer, reduced exciton binding energy, and enhanced proton conductivity. Consequently, it delivers an exceptional photocatalytic H 2 O 2 evolution rate of 10984 µmol h − 1 g − 1 in the presence of benzyl alcohol. Experimental and theoretical investigations demonstrate that incorporated triazine moieties as electron acceptors to tailor the electronic configuration of BDF‐CP1, thereby facilitating the formation and stabilization of the vital * OOH intermediate. This work presents a scalable synthetic strategy for constructing conjugated polymer‐based semiconductors and offers new insights into the rational design of high‐performance photocatalysts toward practical solar‐driven H 2 O 2 production.