In the present work, a novel triptycene-based imine-linked covalent organic polymer (TP-COP) was designed and synthesized via room-temperature, solvent-free mechanochemical grinding. The as-synthesized TP-COP material was fully characterized by Fourier transform infrared spectroscopy, solid-state NMR, field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), Brunauer−Emmett−Teller method, thermogravimetric analysis, diffuse reflectance spectroscopy (DRS), and electron paramagnetic resonance (EPR). The HRTEM image of TP-COP clearly indicates the presence of graphene-like layered morphology (exfoliated layers). The DRS study reveals that TP-COP exhibited a low optical band gap value of 2.49 eV, implying its semiconducting nature. Further, the EPR study confirmed the semiconducting behavior of TP-COP through the generation of free radicals. These findings suggest that TP-COP could be used as an efficient photocatayst for the degradation of organic dye (RhB) under solar irradiation. Moreover, TP-COP showed excellent reusability in degrading dye (RhB) without obvious performance decay.

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