A novel heterogeneous catalyst, designated mgal-c-ni(ii)l, was prepared by the immobilization of ni(ii) schiff base complex, derived from the condensation of 1,2-diaminopropane with 2,5-dihydroxybenzaldehyde, in the reconstituted oxide mgal-c. The behavior of the composite catalyst was tested in the electrooxidation reaction of methanol. The Electrochemical process was followed by cyclic voltammetry experiments in a 1 M KOH solution. The physicochemical characterization revealed the formation of Ni(II) Schiff base complex and their immobilization on the LDH interlayer.Structural-textural properties were explored and the possible complex insertion setting,as well as the formed interaction in the LDH interlamellar space were also investigated by density functional theory (DFT) based simulations. The MgAl-C-Ni(II)L catalyst has been combined with graphite powder to form a modified electrode for further improvement of the electrocatalytic performance. Significant enhancements in peak currents (Ipa) with increasing methanol concentration were observed in the electrochemical process. The modified electrode exhibited high electrocatalytic oxidation activity and stability in an alkaline medium. It induced electrocatalytic oxidation peaks at low potentials with higher current densities. A systematic study was carried out to investigate the effect of parameters such as scanning rate and methanol concentration on the electrooxidation reaction. The results obtained highlight the promising potential of MgAl-C-Ni(II)L composite as an efficient and potentially suitable catalyst for recent advanced electrochemical applications.