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The removing of fluoride from water is highly desired from the viewpoint of environmental protection and sustainable development due to the adverse impacts on human and ecosystem. In this study, the hierarchical porous layered double hydroxide (LDH)/biomass carbon fiber (BCF) has been successfully fabricated by the combined sol-gel, carbonization and hydrothermal processes using sustainable bamboo fibers as raw material based on the assembly the LDH nanosheets on BCF surfaces. Structural characterization indicates that the LDH nanosheets were attached to the BCF surface via in situ crystal growth. N 2 sorption measurements show that the LDH/BCF has relatively uniform accessible mesochannel size of 3.56 nm, and the surface area is as high as 39.89 m 2 /g. The resulting LDH/BCF exhibit a noticeable enhanced adsorption capacity for fluoride removal compared to that of Al 2 O 3 /BCF, accompanied by 15.21 mg/g of the adsorption capacity. The presence of the high negative charge anions had negligible influence on fluoride adsorption. Importantly, recovery adsorption capacity for fluoride was obtained for LDH/BCF for 5 consecutive cycles without a significant decrease in its adsorption properties. Therefore, the current research can offer a green approach to fabricate LDH/BCF with hierarchical structures for efficient removing fluoride from water, and the fabricated LDH/BCF will be an excellent candidate for pollution control based on the synergistic effects of BCF and LDH, high adsorption properties with good reusability. which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.

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