We demonstrate, for the first time, the chemical/electrochemical synthesis of uniformly dispersed nickel hydroxide nanoparticles (Ni(OH) 2 -NPs) embedded in an adsorbed lignosulfonate layer (LS) deposited on a glassy carbon (GC) electrode. This approach is based on the oxidative deposition of Ni(II) lignosulfonates (Ni-LS) followed by Ni(OH) 2 -NP precipitation in alkaline electrolyte. The morphology of this composite was investigated by scanning electron microscopy (SEM). The SEM results show that the NPs have a nano-globular structure in the range ca. 50–200nm. The composite displays reversible electrochemical transition due to a Ni(II)/Ni(III) redox couple and electrocatalytic activity leading to the oxidation of methanol in alkaline solution. The electrochemical properties of the resulting material deposited as a redox film were investigated by cyclic voltammetry and chronoamperometry techniques. Using Laviron's theory, the electron-transfer rate constant and the transfer coefficient were determined to be k s =4.1 s −1 and α=0.42 respectively for a modifier film (Γ Ni =2.5×10 −9 molcm −2 ) in 0.1M sodium hydroxide electrolyte. Chronoamperometric studies were used to determine the catalytic rate constant for the catalytic reaction of the tested modifier with methanol (k ch =1.0×10 4 cm 3 mol −1 s −1 ). The dependence of the methanol oxidation current on alcohol concentration is discussed. The modified electrode for methanol oxidation offers simple preparation, good stability and reproducibility.