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In this work, a C@Ni hierarchical structure was carefully designed by entangling carbon microspheres with curving nickel nanosheets. The presence of copious mesopores between adjoining nanosheets and microspheres greatly enhanced the specific surface area from 314.7 m2 g−1 for pristine carbon spheres to 448.7 m2 g−1 for this well‐designed C@Ni architecture. This salient structural feature enabled it as an ideal magnetic adsorbent for CrVI removal in wastewater. The high CrVI adsorption capacity of ca. 550 mg g−1 at 298 K, remarkable adsorption rate of 3.38 mg g‐1 min‐1 and excellent regeneration efficiencies above 90% were highly desirable for its widespread potential applications in water treatment.