| Summary: | Covalent organic frameworks (COFs) have been widely used in photocatalytic hydrogen peroxide (H<sub>2</sub>O<sub>2</sub>) production due to their favorable band structure and excellent light absorption. Due to the rapid recombination rate of charge carriers, however, their applications are mainly restricted. This study presents the design and development of two highly conjugated triazine-based COFs (TBP-COF and TTP-COF) and evaluates their photocatalytic H<sub>2</sub>O<sub>2</sub> production performance. The nitrogen-rich structures and high degrees of conjugation of TBP-COF and TTP-COF facilitate improved light absorption, promote O<sub>2</sub> adsorption, enhance their redox power, and enable the efficient separation and transfer of photogenerated charge carriers. There is thus an increase in the photocatalytic activity for the production of H<sub>2</sub>O<sub>2</sub>. When exposed to 10 W LED visible light irradiation at a wavelength of 420 nm, the pyridine-based TTP-COF produced 4244 μmol h<sup>−1</sup> g<sup>−1</sup> of H<sub>2</sub>O<sub>2</sub> from pure water in the absence of a sacrificial agent. Compared to TBP-COF (1882 μmol h<sup>−1</sup> g<sup>−1</sup>), which has a similar structure but lacks pyridine sites, TTP-COF demonstrated nearly 2.5 times greater efficiency. Furthermore, it exhibited superior performance compared to most previously published nonmetal COF-based photocatalysts.
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