The discharge of congo red dye into water sources by factories has been associated with a range of health concerns, such as cancer, redness, skin irritation, and allergic reactions. As a result, this research focused on the cost-effective and straightforward production of MgAl₂O₄ nanoparticles by using the Pechini sol-gel process. Subsequently, these nanoparticles were employed for the successful photocatalytic decomposition of congo red dye. Moreover, extensive characterization of the fabricated MgAl₂O₄ nanoparticles was conducted through diverse methodologies, which included Fourier-transform infrared spectroscopy, ultraviolet-visible spectrophotometry, high-resolution transmission electron microscopy (HR-TEM), field-emission scanning electron microscopy (FE-SEM), and powder X-ray diffraction (XRD). Furthermore, the XRD analysis disclosed that the average crystal size of the produced MgAl₂O₄ nanoparticles is 10.36 nm, and their optical energy gap was determined to be 3.71 eV. The FE-SEM examination unveiled a combination of spherical and disorganized structures with a 0.14 μm average grain size. HR-TEM analysis, in turn, revealed that the fabricated MgAl₂O₄ nanoparticles were composed of minuscule spherical particles with an average diameter of 8.75 nm. The maximum degradation of 50 mL of congo red dye at a concentration of 25 mg/L reached 99.27% within 80 min at a pH of 3. Additionally, the findings confirmed the consistent decomposition activity toward congo red dye even after four cycles, thereby validating the effectiveness and reusability of the MgAl₂O₄ nanoparticles that were developed in this study.