The aim of this study was to prepare biocarbons by biomass activation with carbon(IV) oxide. Fennel and caraway fruits were used as the precursors of bioadsorbents. The impact of the precursor type and temperature of activation on the physicochemical properties of the obtained biocarbons and their interaction with methyl red sodium salt upon adsorption process have been checked. The obtained bioadsorbents were characterized by determination of-low temperature nitrogen adsorption/desorption, elemental analysis, ash content, Boehm titration, and pH of water extracts. The biocarbons have surface area varying from 233–371 m2/g and basic in nature with acidic/basic oxygen-containing functional groups (3.23–5.08 mmol/g). The adsorption capacity varied from 63 to 141 mg/g. The influence of different parameters, such as the effectiveness of methyl red sodium salt adsorption, was evaluated. The adsorption kinetics was well fitted using a pseudo-second-order model. The Freundlich model best represented the equilibrium data. The amount of adsorbed dye was also found to increase with the increasing temperature of the process.