The contamination of wastewater by azo dyes indicates serious environmental risks. Currently, industries worldwide use approximately 700,000 tons of these dyes annually, making their removal a significant challenge. In photocatalysis research, a prominent area of dedication to the advancement of visible light photocatalysis aims to achieve superior performance in overall activity. In this study, we fabricated ZnCdS nanoparticles (NPs) via a simple co-precipitation strategy, and sulphur (S)-defect-rich ZnCdS NPs (D-ZnCdS) were created through the ball milling method. These S-defect nanoparticle (NPs) catalysts were utilized for rhodamine B (RhB) dye photocatalytic degradation experiment. (XRD) X-ray diffractometer, X-ray photoelectron spectroscopy (XPS), surface-enhanced Raman spectroscopy, and photoluminescence (PL) spectroscopy characterization studies explained the induced S-defect rich in D-ZnCdS NPs. Further, the morphological, band gap determination, and photogenerated charge carrier recombination efficiency were studied using different analytical and spectroscopic characterization techniques. The Brunauer-emmett-teller (BET) results indicate the increased surface area of D-ZnCdS NPs thereby providing more active sites. The photocatalytic degrading efficiency of D-ZnCdS over RhB explains the complete degradation of pollutants within 260 min. This enhancement in the catalytic process is attributed to the increased absorption of photon energy from the visible light and large defect-rich active sites. Further, the involvement of hydroxyl (*OH) and superoxide radicals (O2*-) in the degradation of RhB along with the presence of sulphur defects, significantly improves the charge transfer in ZnCdS NPs. The involvement of certain factors like pH, ions, NCs catalyst and different RhB concentrations on RhB degradation was investigated. Additionally, D-ZnCdS NPs showed stable degrading capability even after six consecutive cycles of catalytic RhB degradation. The by products formed during the RhB photodegradation experiment were identified using Gas chromatography-mass spectrometer (GC-MS) analysis, and toxicity in fish, daphnia, and algae was examined using the Ecological structure-activity relationships (ECOSAR) program. From the above findings, the current research work provides a new strategy for utilizing defect-engineered D-ZnCdS NPs as a promising catalyst for various environmental remediation applications and paves a ways for manufacturing innovation.