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Magnesium silicate double-walled hollow nanofibers (MSHNFs) with a hierarchical nanostructure have been successfully fabricated by combining the electrospinning technique with a hydrothermal method. The as-prepared MSHNFs are composed of numerous ultrathin nanosheets with a thickness of approximately 10 nm and have a high specific surface area (632.2 m2 g−1) and large pore volume (0.92 cm3 g−1). The MSHNFs exhibit high adsorption capacity and excellent stability in a purification test with organic molecules and a solution of heavy-metal ions. Moreover, the MSHNFs can be easily separated from solution by gravitational sedimentation owing to their unique structure. [ABSTRACT FROM AUTHOR]