In this paper, a facile one-pot bottom-up approach for the preparation of graphene and Ni/graphene nanostructures at normal pressure and low temperature (150 ℃) has been developed. The graphene and Ni/graphene nanostructures were prepared by reducing hexachloro-benzene (C6Cl6 Þ with potassium in n-tetradecane (C14H30) solution without the presence of a catalyst. Meanwhile, the effect of Ni content on the specific surface area (SSA) of the final products was investigated. The testing results display that the as-prepared samples have large SSA and high C/O ratio, implying that the designed synthesis method is simple and efficient. To evaluate the adsorption performances of the samples, we select organic dye rhodamine B (RhB) as the model organic contaminant in aqueous solutions. The experimental results show that the samples possess high adsorption capacity (qmax = 943.4mg g -1), ultrafast adsorption rate (> 99%, 2 min), high adsorption efficiency ( ≥ 99.8%) and good chemical stability in a wide pH range (2–11), high salt tolerance (> 80 mg mL -1), and good reusability (> 99.5%, 9 cycles) for dye RhB from water. In particular, the samples exhibit a good property for the treatment of the raw industrial wastewater (RIW).