A novel nickel recovery method was designed using tetraoxalyl ethylenediamine melamine chelate resin grafted-carbon fibers (MFT/CFs) from the spent electroless nickel plating baths. The process involved inoculation of tetraoxalyl ethylenediamine melamine chelate resin at CFs, the adsorption and eletrodeposition of Ni2+ at MFT/CFs. Ethylenediamine was covalently modified at CFs by constant potential, tetraoxaryl ethylenediamine was grafted at the CFs by amidation reaction, then melamine, formaldehyde and tetraoxalyl ethylenediamine could be polymerized at the CFs. The MFT/CFs showed an excellent uptake effect for Ni2+ with a pseudo-second order model. The interaction mechanism between Ni2+ and active sites has been interpreted as chelation. Nano-nickel coated-MFT/CFs materials could be obtained by electrodeposition (Ni/MFT/CFs). The present materials were carefully examined by fourier transform infrared spectroscopy, field emission scanning electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy and electrochemistry techniques. The characterization results suggested the formation of Ni/MFT/CFs with a good electrocatalysis for ethanol oxidation. (C) 2012 Elsevier B.V. All rights reserved.