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Metal-organic frameworks (MOFs) are a class of nanoporous materials. The development of efficient and environmentally friendly methods for activating MOFs is of great significance for its industrial application. In this work, nanoscale magnetic core-shell Cu-BTC@Fe 3 O 4 was prepared through a secondary growth strategy. The effects of different activation solvents (dichloromethane and ethanol, respectively) and temperatures on the surface area, pore structures and the adsorption of xylene isomers on Cu-BTC@Fe 3 O 4 were investigated. Ethanol as an activation solvent could more easily displace the precursors remaining in the channels of Cu-BTC@Fe 3 O 4 than dichloromethane, while the temperature change has no significant influence on the pore structure. The adsorption separation of xylene isomers on Cu-BTC@Fe 3 O 4 composite materials was studied using the batch vapor-phase adsorption, and liquid-phase breakthrough experiments. The activated Cu-BTC@Fe 3 O 4 (CH 2 Cl 2 -200 ​°C ​− ​C 2 H 5 OH) material has the highest adsorption capacity of 210.26 ​mg ​g−1 for p -xylene (p X). Cu-BTC@Fe 3 O 4 (C 2 H 5 OH) and Cu-BTC@Fe 3 O 4 materials have excellent adsorption capacity for m -xylene (m X), with the values of 200.19 ​mg ​g−1 and 219.63 ​mg ​g−1, respectively, which is about 4 times higher than that of Cu-BTC@Fe 3 O 4 (CH 2 Cl 2). The adsorption capacity sequence of xylene on Cu-BTC@Fe 3 O 4 (C 2 H 5 OH) and Cu-BTC@Fe 3 O 4 materials is m -xylene (m X) ​> ​ p -xylene (p X) ​> ​ o -xylene (o X), and that of other materials is p X ​> ​ m X ​> ​ o X. Nanoscale magnetic core-shell Cu-BTC@Fe 3 O 4 was prepared through a secondary growth strategy towards the adsorption separation of xylene isomers. [Display omitted] • Nanoscale magnetic core-shell Cu-BTC@Fe 3 O 4 was prepared through a secondary growth strategy. • The effects of different activation solvents and temperatures on the xylene isomers adsorption of Cu-BTC@Fe 3 O 4 were studied. • Using ethanol as an activation solvent could more easily displace the precursors remaining in the channels of Cu-BTC@Fe 3 O 4. [ABSTRACT FROM AUTHOR]