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Water polluted by organic dyes is normally present in industrial production, which seriously threatens environmental safety. Research on dye adsorption has recently been related to nanomaterials due to their large specific surface area. However, there are still some problems associated with their preparation, application, and recovery. In this study, we developed the one‐step synthesis of lignocellulosic‐Fe(OH)3 hybrid fibers by in situ growth of Fe(OH)3 nanoparticles on lignocellulosic, which could be used as effective adsorbents for dye removal. The formed Fe(OH)3 nanoparticles were dispersed homogeneously on the surface of lignocellulosic. The as‐prepared hybrid fibers featured a large absorption capacity for methylene blue, up to 150.9 mg/g. In a fixed‐bed column separation process, dye pollutants were successfully removed from the water even at a high speed of 5.0 mL/min, with the separation efficiency higher than 99.99%. Remarkably, 1.0 g of lignocellulosic‐Fe(OH)3 was capable of separating over 1200 mL of dye solution continuously and thoroughly. Notably, the underlying adsorption mechanism analyses suggested that multi‐interactions of hydrogen bonds, π–π interactions, and coordinate bonds contribute to the adsorption ability of lignocellulosic‐Fe(OH)3. [ABSTRACT FROM AUTHOR]