This study presents the preparation and evaluation of a novel adsorbent designed for removing organic solvents from wastewater, focusing on toluene, a common toxic solvent. The adsorbent, a unique blend of silica aerogel, recycled polyethylene terephthalate (rPET) short fibers, FeCl3, and chitosan, was rigorously tested and characterized using a range of methods. The adsorption performance of the adsorbent was tested for various organic solvents, with detailed attention to toluene. The adsorption parameters, including adsorbent dosage, initial toluene concentration (100-1000 ppm), contact time (15-40 minutes), pH (2-10), and temperature (18-40 °C), were investigated using response surface methodology (RSM) based on central composite design (CCD). The maximum toluene removal efficiency was 99.52%, achieved under optimal conditions. The adjusted coefficient of the determination of the model was 0.968, which indicates that the model was entirely appropriate and accurate. Kinetic studies suggested that the adsorption followed pseudo-second-order kinetic, while equilibrium data were well-fitted to Langmuir and Freundlich isotherms. The stability of the adsorbent across four regeneration cycles demonstrates its potential for long-term application in sustainable water treatment. These results, along with the potential for long-term application, suggest that the developed adsorbent is a promising solution for effectively remedying toluene and some organic matters like crude oil-contaminated wastewater, contributing to environmental protection and plastic waste management.