Wastewater treatment for the removal of heavy metals can reduce environmental contamination, enable safer industrial activities, and enhance sustainable practices. Efficient materials processing oriented to low temperature operating conditions; thus, the development and modeling of carbon nanotube/SDS-alumina nanocomposite-based adsorbents (CNT/ SDS-alumina) for efficient wastewater treatment are investigated in this work. The optimization of a low temperature-based process is targeted in this work to achieve a cost-effective method for fabrication of CNT/SDSalumina nanocomposites. The fabrication process involves the investigation of various heating conditions in an oven and autoclave with successful optimization for the formation of porous CNT/SDS-alumina nanocomposite-based adsorbents. The fabricated materials were characterized by TEM, SEM, XRD, FTIR, and surface area analysis. The results indicate that the heating condition is the factor controlling the formation of the porous structure of the CNT/SDS-alumina nanocomposite, which affects the wastewater treatment application. The surface area was higher (49.26−51.02 cm 2 /g) for CNT/SDS-alumina nanocomposite-based adsorbents prepared under autoclave heating conditions. The best adsorption capacity values obtained using the CNT/SDS-alumina nanocomposite prepared under autoclave conditions were 463 mg/g for arsenic ions and 418 mg/g for mercury ions, revealing the high efficiency of the prepared materials for the adsorption of pollutants. The adsorption process for the removal of arsenic and mercury is reported to follow the second-order kinetic model. The adsorption data for the CNT/SDS-alumina nanocomposite-based adsorbents prepared under autoclave heating conditions are well fitted with the Langmuir isotherm, suggesting a monolayer adsorption mechanism. Additionally, the prepared CNT/SDS-alumina nanocomposite-based adsorbents are recommended for potential applications involving the adsorption of various heavy metals for real wastewater treatment situations.