The aim of the current study is to obtain the thermal behavior and kinetic analyses of the removal of surfactant from MCM-41 synthesized from tailings slurry at different heating rates. X-ray diffraction and thermogravimetric analyses were carried out to determine the characterization of the synthesized samples. Kissinger-Akahira-Sunose and Friedman isoconversional kinetic methods were applied for the purpose of determining the kinetic analysis parameters of the decomposition of surfactant from the mesoporous molecular sieves MCM-41 under non-isothermal conditions. For the comparison of these results, MCM-41 was synthesized from a pure silica source. The thermal behaviors of MCM-41 synthesized from tailings slurry do not differ from samples synthesized from pure silica during the decomposition reactions. The kinetic analysis' results indicate that the decomposition reactions of the synthesized MCM-41 samples had complex reaction mechanisms.