This work designed and synthesized three complexes by the hydrothermal synthetic method, They are [Zn (nic)2(H2O)2]n (1), [Ni2(nic)4 (μ2-H2O)]n (2), [Co2(nic)4 (μ2-H2O)]n (3), respectively. The complexes were characterized by elemental analysis, infrared spectrum, ultraviolet spectrum, thermogravimetric analysis and X-ray powder diffraction etc. The crystal structures of complexes 1–3 were measured by X-ray single crystal diffraction. Complex 1 formed a 3D supramolecular structure through hydrogen bonds, and complexes 2–3 formed 3D network structures with coordination bonds. The adsorption properties of complexes 1–3 on the coomass bright blue G250 (CBB) were tested, meanwhile, whose adsorption kinetics were also studied.