Silver Nanoparticle‐Loaded Conjugated Microporous Polymers: A Highly Efficient Photocatalyst for Methylene Blue Degradation

Photocatalytic degradation offers a promising solution for dye wastewater treatment using solar energy, addressing regeneration and secondary pollution issues, and mitigating regeneration and secondary pollution concerns associated with conventional methods. However, polymer‐based photocatalysts encounter several challenges, including complex synthesis routes, limited photocatalytic efficiency, and prolonged reaction durations. Herein, we synthesized four functionalized conjugated microporous polymers (CMPs) containing naphthyl, anthryl, phenyl, and n‐propyl groups via Sonogashira–Hagihara coupling, and developed a silver nanoparticle‐decorated conjugated microporous polymers composite that achieved near‐complete (99.99%) degradation of methylene blue within 20 min under visible light, retaining 99.87% efficiency after five cycles. Mechanistic studies revealed the generation of reactive oxygen species (hydroxyl radical (·OH) and superoxide anion (·O 2 − )) responsible for efficient dye mineralization to degradation products, including CO 2 and H 2 O. This work provides a new strategy for designing high‐performance photocatalytic composites for wastewater treatment.