The invention relates to a method for preparing a bimetallic arene adsorbent. Sodium silicate, inorganic acid, deionized water and metal salt are adopted as raw materials, and the method comprises the following steps that 1, sodium silicate and inorganic acid serve as raw materials to synthesize silicon dioxide sol; 2, silicon dioxide sol is washed, first metal modifying soaking is carried out through an alkaline-earth metal saline solution, and filtering is carried out to obtain a filter cake; 3, the filter cake is pulped with deionized water; 4, a spray drying device is used for carrying out drying molding on slurry, and a silicon dioxide spherical carrier is prepared; 5, a transition metal saline solution is adopted for carrying out equivalent-volume impregnation on the spherical carrier, the grain size ranges from 0.5 mm to 1.0 mm, the average pore size ranges from 2 nm to 15 nm, the specific surface area ranges from 300 m<2>/g to 600 m<2>/g, the pore volume ranges from 0.4 ml/g to 1.5 ml/g, and the total metal content ranges from 0.2 wt% to 5 wt%; arene in megilp can be effectively adsorbed, the arene removal rate is 95% or above, and the method is suitable for adsorbing and separating high boiling point solvent megilp arene.