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This study reported a novel technique for spray coating zinc oxide (ZnO) on one side of fiberglass (FG) substrate and chitosan (CS) on the opposite side, resulting in the production of ZnO/FG/CS composite. This strategy alters the morphology of the pure FG, creating smooth and rough surfaces on the CS and ZnO sides, respectively. ZnO/FG/CS demonstrated remarkable photoremoval activity in a combined solution of methylene blue-methyl orange and real wastewater with the addition of hydrogen peroxide and facilitated moderate reusability over five cycles. This strategy revealed an insight for developing an integrated adsorption and photocatalytic process with high-performance capabilities.