The release of azo dye contaminants from textile industries into the environment is an issue of major concern. Nanoscale zerovalent iron (nZVI) has been extensively studied in the degradation of azo dye pollutants such as methyl orange (MO). In this study, iron was coupled with copper and silver to make trimetallic Fe/Cu/Ag nanoparticles, in order to enhance the degradation of MO and increase reactivity of the catalyst by delaying the rate of oxidation of iron. The synthesis of the trimetallic nanoparticles (Fe/Cu/Ag) was carried out using the sodium borohydride reduction method. The characterization of the particles was performed using XRD, XPS, EDX, and TEM. The analyses confirmed the successful synthesis of the nanoparticles; the TEM images also showed the desired structures and geometry of the nanoscale zerovalent iron particles. The assessment of the nanoparticles in the degradation of methyl orange showed a notable degradation within few minutes into the reaction. The effect of parameters such as nanoparticle dosage, initial MO concentration, and the solution pH on the degradation of MO using the nanoparticles was investigated. Methyl orange degradation efficiency reached 100% within 1 min into the reaction at a low pH, with lower initial MO concentration and higher nanoparticle dosage. The degradation rate of MO using the nanoparticles followed pseudo first-order kinetics and was greatly influenced by the studied parameters. Additionally, LC-MS technique confirmed the degradation of MO within 1 min and that the degradation occurs through the splitting of the azo bond. The Fe/Cu/Ag trimetallic nanoparticles have proven to be an appropriate and efficient alternative for the treatment of dye wastewater.