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Calcium molybdate (CaMoO4) is of significant interest due to its unique properties and numerous industrial applications, such as catalysis, electrochemistry, and optoelectronics. In this study, we developed an economical and environmentally friendly method to synthesize calcium molybdate from Moroccan phosphogypsum (PG) industrial waste and sodium molybdate, all at room temperature. Comprehensive analysis through X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman vibrational spectroscopy, and scanning electron microscopy (SEM) revealed the high purity of the synthesized calcium molybdate, with particle sizes of only 12 nm. Additionally, optical characteristics were studied using ultraviolet-visible spectroscopy (UV-vis), which showed an optical band gap of Egap = 3.96 eV for CaMoO4. These results confirm the successful synthesis of calcium molybdate nanoparticles from Moroccan phosphogypsum, demonstrating an effective pathway to valorize this industrial waste into a valuable material. This approach contributes to environmental sustainability by reducing dependence on rare chemicals while offering innovative solutions for the industry’s sustainable development.