In this study, Aloe Vera leaves wastes-based sulfuric acid modified activated carbon (AV-SAC) was applied for the sorption of aniline as a health-toxic substance and methyl orange (MO) as a anionic dye from aqueous phase. The batch sorption system was used to assess the effect of different parameters including contact time, pH, adsorbent dosage, and adsorbate contents on the adsorption. The equilibrium was obtained at contact time of 60 min for both the adsorbates. The pH of 3 had a significant influence on the uptake capacities of aniline and MO from aqueous media. Fitting the experimental data to different kinetics and isotherms models indicated that the experimental data were well fitted by the pseudo-second-order kinetic and Freundlich isotherm models, respectively. The maximum monolayer adsorption capacities were acquired 185.18 and 196.07 mg/g for aniline and MO, respectively. Due to its low-cost and high uptake capacity, AV-SAC can be considered as one of the effective sorbents for wastewater treatment contains of aniline and MO.