Poly(vinyl alcohol)-sodium alginate-chitosan-activated carbon and FeO hydrogel beads (HPAC/Act. C/FeO) with porous and steady structure were fabricated via hydrogen-bond and electrostatic interactions, and were characterized by FT-IR, BET surface area analyzer, XRD and XRF and effecting tests. The preparation of the HPAC/Act. C/FeO hydrogel bead using chitosan as a precursor, which then cooperated with polyvinyl alcohol (PVA), using trisodium citrate as crosslink agent and stimulating the polymerization reaction to encapsulate the activated carbon. The FeO was added to the mixture to enhance the strength of the chitosan-based hydrogel adsorbent. In addition, the composite material displayed an amorphous carbon structure and possessed a high BET surface area. Furthermore, it demonstrated higher stability in aqueous solutions than the composite hydrogel material without FeO but showed lower swelling in the aqueous solution. In addition, HPAC/Act. C/FeO hydrogel beads demonstrated high adsorption capacity of methylene blue (MB) from water at 95 mg/g, but lower than HPAC/Act. C hydrogel bead (109.78 mg/g). However, the HPAC/Act. C/FeO hydrogel bead had good stability and magnetic separation.