Industrialization in the current times has become extremely rapid. Some of these industries are responsible for discharging dye-containing wastewater into natural water bodies and hence causing environmental deterioration. The purpose of this research is to investigate an inexpensive and easy-to-set-up photodegradation process for the mineralization of methylene blue (MB) dye. The optimum conditions required for maximum degradation of the dye were explored by varying different experimental parameters such as the initial concentration of Fe(III) and dye, pH of the reaction mixture, nature of light sources, and intensity of ultraviolet (UV) light. Approximately 97% photodegradation of methylene blue was recorded at pH 2.30 for the optimum concentration of MB of 3.00 × 10−5 M and Fe(III) aqueous solution of 8.00 × 10−4 M when irradiated under UV light of intensity 3.31 × 10−9 Ein cm−3 s−1. Under sunlight, with similar experimental conditions, 73% degradation of the dye was achieved. This is an environment-friendly, efficient, and low-cost degradation process of methylene blue.