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The sustainable synthesis of metal oxide materials provides an ecofriendly and more exciting approach in the domain of a clean environment. Besides, plant extracts to synthesize nanoparticles have been considered one of the more superior ecofriendly methods. This paper describes the biosynthetic preparation route of three different sizes of tetragonal structure SnO 2 nanoparticles (SNPs) from the agro-waste cotton boll peel aqueous extract at 200, 500, and 800 °C for 3 h and represents a low-cost and alternative preparation method. The samples were characterized by X-ray diffraction, Fourier transform infrared spectrophotometry, ultraviolet–visible absorption spectroscopy, high-resolution transmission electron microscopy (HR-TEM), and energy-dispersive X-ray spectroscopy. Surface area and porosity size distribution were identified by nitrogen adsorption–desorption isotherms and Brunauer–Emmett–Teller analysis. The photocatalytic properties of the SNP samples were studied against methylene blue (MB) and methyl orange (MO), and the degradation was evaluated with three different size nanomaterials of 3.97, 8.48, and 13.43 nm. Photocatalytic activities were carried out under a multilamp (125 W Hg lamps) photoreactor. The smallest size sample exhibited the highest MB degradation efficiency within 30 min than the most significant size sample, which lasted 80 min. Similarly, in the case of MO, the smallest sample showed a more superior degradation efficiency with a shorter period (40 min) than the large-size samples (100 min). Therefore, our studies suggested that the developed SNP nanomaterials could be potential, promising photocatalysts against the degradation of industrial effluents.

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