Developing adsorbent materials based on biomass that can be easily recycled and reused to remove water pollutants has received widespread attention. A novel method for the preparation of calcium alginate/poly (vinyl alcohol)/boric acid (as-synthesized Ca-APB) aerogel fibers for highly efficient adsorption of methylene blue by directed freezing wet-spinning was presented in this paper. The Ca-APB-0.5 aerogel fibers exhibited a hierarchical structure consisting of a honeycomb micron pore structure with mesopores walls, with a maximum adsorption capacity of 508.99 mg/g in 5 h at 293 K. Meanwhile, the experimental data for Ca-APB-0.5 aerogel fibers showed the best fit to the Freundlich model and pseudo-second-order model. Moreover, the adsorption capacity was investigated for three consecutive cycles, with 469.37, 457.19, and 439.77 mg/g in the first, second, and third cycles, respectively. This paper proves that the hierarchical structure of alginate-based aerogel fiber is an effective dye adsorption material with high efficiency, reusability, and eco-friendliness.
