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Although widely used in the textile industry, methyl orange is considered one of the most toxic dyes, which have negative impacts on the aquatic environment and needs to be removed from water bodies. Hence, the present paper reports the synthesis of new floating photo-Fenton catalysts based on the immobilization of Fe2O3 nanoparticles on the surface of Luffa sponges for the oxalate-induced-degradation of methyl orange. The floating catalytic sponges were prepared through a simple precipitation method followed by a reflux heating process and then characterized by field emission scanning electron microscopy, X-ray diffraction, atomic absorption spectrometry, and nitrogen adsorption-desorption experiments. According to the experimental results, methyl orange was effectively degraded over our floating catalytic sponges under light illumination at near neutral pH. The catalytic activity was also found to be enhanced with the increase in crystallinity of Fe2O3 nanoparticles, which can be achieved by the reflux heating. Besides, owing to the floating feature, these sponges are easily separated from the solution, thereby not forming a secondary source of pollution for water