Magnetic Fe 3 O 4 particles were synthesized by solvo-thermal method, and then hydrolysis method was used to encapsulate a compact layer of SiO 2 on the surface of Fe 3 O 4 particles. Finally, the magnetic MOF5@SiO 2 @Fe 3 O 4 catalysts were prepared by in situ coating different contents of MOF-5 on the surface of SiO 2 @Fe 3 O 4 particles. The as-synthesized samples were characterized by TEM, SEM, XRD, FT-IR, N 2 adsorption/desorption, VSM and NH 3 -TPD. The catalytic activities of the magnetic MOF-5@SiO 2 @Fe 3 O 4 catalysts for the FriedelCrafts alkylation of toluene with benzyl chloride were evaluated. The results showed that magnetic MOF5@SiO 2 @Fe 3 O 4 catalysts exhibited superparamagnetic property, and could be separated by a magnet from the liquid reaction system. The conversion of toluene was increased gradually with the increase of catalyst contents and reaction temperature, respectively. 97 % conversion of toluene has been achieved by using 26.8 %MOF-5@SiO 2 @Fe 3 O 4 catalyst at 120°C for 6 h. Furthermore, electron-donating group, such as -OCH 3 , and -CH 3 , exhibited positive effect on the alkylation reaction. Besides, the catalyst could be easily separated from the reaction mixture after the reaction and reused for five times without significant decrease in activity.