▎ 摘　　要

Graphene oxide/nanodiamond (GO/ND) microspheres were synthesized via coupling electrostatic self-assembly and capillary force in the presence of aniline for Pb(II) removal. The results indicate the presence of ND particles prevents from the restacking of GO nanosheets. Aniline with both benzene ring and amino group plays the synergistic effects on forming GO/15 %ND microspheres by pi-pi interactions and acid-base reaction etc. The formed microsphere with the fixed ratio of GO/ND as 85/15 (named as GO/15 %ND) has the unique hollow structure and abundant oxygen functional groups. The minimum size of GO/15 %ND microsphere is about 600 mu m by tailoring the rotational speed and the ratio of GO/aniline. The isotherm and kinetics data indicate that the Pb(II) ion adsorption processes are well described by the Langmuir and pseudo-second-order kinetics mode. The maximum Pb(II) adsorption capacity of GO/15 %ND microsphere is 303.03 mg g(-1) with the merits of high adsorption capacity, easy separation and facile recovery.