A preparation method of a novel sulfhydrylization graphene oxide and iron and manganese oxide composite material is simple and convenient. The method comprises the steps that a ferrous sulfate solution and a potassium permanganate solution are added into a graphene oxide suspension in sequence, mixing is conducted to be uniform, the pH is adjusted to be 7.5, stirring and standing are conducted, water washing is conducted till the mixture is neutral, and after freeze drying is conducted, graphene oxide and iron and manganese oxide composite material powder is obtained; the powder is cleaned with ethyl alcohol, ultrasonic dispersion is conducted for 1 h in methylbenzene, after cleaning is conducted with ethyl alcohol, the treated powder is dispersed in a 2% 3-mercaptopropyltrimethoxysilane (95% ethyl alcohol) solution, stirring is conducted for 6 h, the pH is adjusted to be 9.5 with ammonia water, stirring is conducted for 24 h, water washing and freeze drying are conducted, and sulfhydrylization graphene oxide and iron and manganese oxide composite material powder is obtained. Graphene oxide is combined with iron and manganese oxides, agglomeration of the iron and manganese oxides is blocked, and the removal effect of methylmercury in water is significantly improved by means of introduction of a sulfhydryl group. The preparation method of the novel sulfhydrylization graphene oxide and iron and manganese oxide composite material has the advantages of being simple in process, stable in effect, wide in application range, environmentally friendly, high in selectivity and the like.