The emergence of 2D materials has significantly expanded the wide range of nanomaterials with diverse applications. Notably, their high conductivity, catalytic efficiency, and hydrophobicity have fueled heightened research interests for water treatment applications. This research aimed to investigate the synthesis and characterization of MXene and reduced graphene oxide (rGO) nanocomposites with silver nanoparticles (Ag) for enhanced catalytic activity in the decomposition of Direct Blue-24 dye. In this study, we employed well-established methods, previously documented in the literature, to prepare two distinct nanocomposites. Novel nanocomposites, namely reduced graphene oxide–silver nanoparticles (rGO–Ag) and MXene–silver nanoparticles (MXene–Ag), were synthesized using the hydrothermal and direct reduction method with an ammoniacal solution (aqueous solution). Comprehensive characterization using advanced tools revealed that the introduced Ag particles integrated seamlessly onto the parent nanofilms of the Carbon derivatives, forming a secondary phase with enhanced catalytic functionality. These nanocomposites demonstrated significant improvements in the catalytic decomposition reactions in simulated wastewater. Verification involved the reduction reaction of Direct Blue-24 dye at known nanocomposite concentrations. The results indicated that MXene–Ag exhibited a superior catalytic activity of 98% in 10 min compared to the rGO–Ag nanocomposite films, which achieved 96% in 35 min. The results indicated that MXene–Ag nanocomposites exhibited a 20–25% increase in catalytic efficiency compared to the rGO–Ag nanocomposites. The outcomes of this research hold promise for practical applications in textile wastewater management and various industrial sectors dealing with mutagenic and carcinogenic chemicals containing azo and/or phthalocyanine products.
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