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A solvothermal method combining a calcination process was conducted to synthesize Fe 3 O 4 @NiO core–shell hierarchical nanostructures. First, Fe 3 O 4 microspheres were synthesized through a solvothermal method by using ethylene glycol as solvent. Second, Fe 3 O 4 @Ni(OH) 2 core–shell hierarchical nanostructures were prepared through an in situ growing procedure. Third, Fe 3 O 4 @NiO core–shell hierarchical nanostructures were obtained from the Fe 3 O 4 @Ni(OH) 2 precursors by a simple calcination procedure. The results showed that the Fe 3 O 4 core was about 250 nm in diameter and the NiO shell was around 30 nm in thickness. The Fe 3 O 4 @NiO core–shell nanostructures were used as a magnetically separable adsorbent for the removal of Congo red (CR) dye from aueous solution, which exhibited a high adsorption capacity of ~128.9 mg g −1 . Moreover, the Fe 3 O 4 @NiO core–shell nanostructures displayed a superior catalytic property for the epoxidation of styrene with an extremely high selectivity (100%), conversion (99%) and yield (99%). Such Fe 3 O 4 @NiO catalyst could be conveniently recycled from the reaction system by using a magnet and without any noticeable catalytic deactivation even after five cycles. The results indicate that the as-prepared core–shell materials can be used as a recyclable catalyst for the epoxidation of styrene. [ABSTRACT FROM AUTHOR]