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The present article reports a facile approach to fabrication of mesoporous octahedron-shaped tricobalt tetroxide nanoparticles (Co 3 O 4 NPs) with a very narrow size distribution for eco-friendly remediation of toxic dyes. Co 3 O 4 NPs were fabricated by a sol−gel process using cobalt chloride hexahydrate (CoCl 2 • 6H 2 O) and monosodium succinate (C 4 H 5 O 4 Na) as a chelating/ structure-directing agent and sodium dodecyl sulfate as a surfactant. Moreover, the phase structure, elemental composition, and thermal and morphological facets of Co 3 O 4 NPs were investigated using XRD, FT-IR, EDS, Raman, XPS, TGA, SEM, and TEM techniques. The face-centered cubic spinel crystalline structure of the Co 3 O 4 NPs was confirmed by XRD and SEM, and TEM analysis revealed their octahedron morphology with a smooth surface. Moreover, the narrow pore size distribution and the mesoporous nature of the Co 3 O 4 NPs were confirmed by Brunauer−Emmett−Teller measurements. The photocatalytic activity of Co 3 O 4 NPs for degradation of methyl red (MR), Eriochrome Black-T (EBT), bromophenol blue (BPB), and malachite green (MG) was examined under visible light irradiation, and the kinetics of the dye degradation was pseudo-zero-order with the rate constant in the order of MR > EBT > MG > BPB. Furthermore, the mechanism of photo-disintegration mechanism of the dye was examined by a scavenging test using liquid chromatography−mass chromatography, and its excellent photodegradation activities were attributed to the photogenerated holes (h + ), superoxide (O 2 − ) anions, and hydroxyl ( • OH) radicals. Finally, the synergistic effect of the nano-interconnected channels with octahedron geometry, mesoporous nature, and charge transfer properties along with photogenerated charge separations leads to an enhanced Co 3 O 4 photocatalytic activity.

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