In the present work, the preparation of activated carbon pellets from cigarette butts by thermal treatment was evaluated. The morphological, textural, topological, and surface chemical properties were studied by SEM-EDX, N2 adsorption, Raman, and FTIR spectroscopy. For adsorption assays, activated carbon was tested for the adsorption of phenol as a model molecule at different solution pH, temperature, and type of water. In addition, leaching tests before and after carbonization were conducted to evaluate the lixiviation of ions present in the solid. The results revealed a microporous material, composed of cylindrical fibers (thickness of 13 µm) with a microporous area of 713 m2 /g and narrow and uniform slit-shaped pores (0.4–0.8 nm). The surface chemistry analysis evidenced the presence of oxygenated groups (carboxylic, esters, and phenolics). Activated carbon leaching tests indicated that the concentrations of the leached ions did not exceed the maximum permissible limit for drinking water. Phenol adsorption revealed an exothermic process with a maximum adsorption capacity of 272 mg/g at 10◦ C. Finally, it was confirmed that phenol diffusion was drastically affected by hindered phenomena due to the similarity in the molecular size of phenol and the average size of micropores, and as a result an effective diffusion coefficient between 6.10 × 10−0 and 5.50 × 10−12 cm2 /s and a maximum tortuosity value of 3.3 were obtained.