A novel Ni9S8/C electrocatalyst for methanol oxidation reaction (MOR) is synthesized by a simple, cost-effective and one-pot strategy. The electrocatalyst Ni9S8 composed of micro and nanoparticles encapsulated inside carbon layers serves as carbon-supporter and fast ion and electron mobilization through the Ni9S8/C support materials. The sizes of Ni9S8/C nanoparticles range from 2.4 to 7.99 nm, reveals large surface area availability with plenty of active sites for electro-oxidation of methanol. The oxidation performance of electrocatalyst is determined in different solution of methanol and alcohol at various scan rates. At a scan rate of 50 mV s−1, the Ni9S8/C catalyst delivers total 52 mA cm−2 current density for 1.75 V potential (vs RHE) for 1 M KOH and 0.5 M methanol. The electrocatalyst shows low Rct circle and linear chronoamperometric graph for 5000 s, which demonstrate the outstanding stability of the electrocatalyst for methanol electro-oxidation reaction.