| Summary: | Biogenic synthesis of nanoparticles using plant extract is a promising trend in research to reduce chemical consumption and avoid wastewater treatment complications. In this work, the zero-valent Fe/Fe<sub>3</sub>O<sub>4</sub> nanoparticles (Fe<sup>0</sup>/Fe<sub>3</sub>O<sub>4</sub> NPs) were synthesized using <i>Caralluma acutangula</i> (CA) plant, widespread in the Jazan region in Saudi Arabia. The synthesis process involves hydrothermal treatment of plant extract and iron (III) mixture at 80 °C to facilitate the reduction reaction of iron (III) cations. The Fe<sup>0</sup>/Fe<sub>3</sub>O<sub>4</sub> NPs were characterized by XRD, FTIR, SEM, EDX, TEM, XPS, TGA, UV, and S<sub>BET</sub>. The obtained data support the formation of Fe<sup>0</sup>/Fe<sub>3</sub>O<sub>4</sub> NPs crystal structure with an average particle size of 9.6 nm and surface area of 89 m<sup>2</sup>.g<sup>−1</sup>. The biosynthesized Fe<sup>0</sup>/Fe<sub>3</sub>O<sub>4</sub> NPs were then applied for the photodegradation of Methylene blue (MB) dye as one of the most common organic dyes in wastewater due to several industrial human activities. Different parameters for MB degradation were performed, such as kinetics and thermodynamics studies. The data obtained reflect the nonspontaneous endothermic process with 87.8 KJ. mol<sup>−1</sup> activation energy (<i>E<sub>a</sub></i>).
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