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@Fe3O4 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@Fe3O4 were investigated. Ethanol as an activation solvent could more easily displace the precursors remaining in the channels of Cu-BTC@Fe3O4 than dichloromethane, while the temperature change has no significant influence on the pore structure. The adsorption separation of xylene isomers on Cu-BTC@Fe3O4 composite materials was studied using the batch vapor-phase adsorption, and liquid-phase breakthrough experiments. The activated Cu-BTC@Fe3O4 (CH2Cl2-200 °C − C2H5OH) material has the highest adsorption capacity of 210.26 mg g−1 for p-xylene (pX). Cu-BTC@Fe3O4 (C2H5OH) and Cu-BTC@Fe3O4 materials have excellent adsorption capacity for m-xylene (mX), 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@Fe3O4 (CH2Cl2). The adsorption capacity sequence of xylene on Cu-BTC@Fe3O4 (C2H5OH) and Cu-BTC@Fe3O4 materials is m-xylene (mX) > p-xylene (pX) > o-xylene (oX), and that of other materials is pX > mX > oX.
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