In this study, a new multi-walled carbon nanotube(MWCNT) based hybrid material was obtained and used as adsorbent for the removal of Cu(II) and Co(II) from aqueous solutions. In the synthesis, firstly, the surface of MWCNT was modified via Hummer method to give oxidized MWCNT-O. In the following step, the oxidized MWCNT was treated with 3-aminopropyl triethoxysilane (APTES) to give a silanized form of MWCNT having free amine end groups. Finally, the silanized MWCNT was reacted with 3, 5-dichlorosalicylaldehyde to give the hybrid material. The new hybrid material was characterized by analytical and spectroscopic methods (FT-IR, UV-Vis., TGA, Raman Spectra, SEM, TEM, EDX and XRD studies). The hybrid material was used as adsorbent for the removal of Cu(II) and Co(II) ions from aqueous solutions. The effects of adsorption parameters such as pH, contact time, temperature, and initial concentrations on adsorption behaviors were investigated.