The invention provides a preparation method of a nickel-cobalt layered bimetallic hydroxide/graphene electrocatalyst, which belongs to the technical field of electrocatalysts. The method disclosed bythe invention comprises the following steps: graphene and cobalt nitrate are uniformly dispersed in a methanol solvent by ultrasonic waves, so that an ultrasonic solution is obtained; the ultrasonic solution is added into a methanol solution of dimethylimidazole, is uniformly mixed and then is enabled to stand, and centrifuging, washing and drying are then carried out, so that a ZIF-67/graphene composite material is obtained; the ZIF-67/graphene composite material and nickel salt are mixed and dissolved in a solvent, refluxing is carried out for reaction, centrifugal separation is then carriedout, obtained precipitate is washed with absolute ethyl alcohol, and drying is carried out to obtain a NiCo LDH/G composite material with a nanoscale morphology. The method disclosed by the inventionovercomes the defects of high requirement on equipment, need for high temperature and high pressure and need for an expensive surfactant existing in conventional synthesis methods, and compared withthe prior art, the preparation method has the advantages of simple process, low cost, easy reaction process control and the like, and is suitable for industrial mass production.