Abstract: This study was conducted to produce Chitosan/MWNTs/SiO2 (CSMS) nanocomposite powder from aqueous solution through the sol-gel method. The morphology of the CSMS was characterized by Field-Emission Scanning Electron Microscopy (FESEM) X-Ray Diffraction (XRD) Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). The adsorption characteristics were determined by Brunauer-Emmett-Teller (BET) surface area (nitrogen adsorption/desorption isotherms). The results were compared with previously synthesized and characterized Silica Nanoparticles (SiO2 NP). The results showed that CSMS has a 98% adsorption rate which was the largest absorption rate for chitosan by itself. Moreover, the thermal stability of CSMS was demonstrated at temperatures up to 400°C. The pore size of CSMS was determined to be 2.195 nm and the surface area was 478 m2/g. This study’s results indicate that CSMS has novel features that could with stand degradation with efficient adsorption properties.