In this work, complex of Ni‐modified graphene oxide was prepared and charac- terized using FT‐IR spectroscopy, SEM, XRD, TGA and ICP‐OES techniques. This compound used as an efficient and recoverable catalyst for the C –S cou- pling reaction using sulfur‐transfer reagents (S 8 or thiourea). The catalyst was easily separated using a simple filtration and reusable without significant loss of their catalytic efficiency.