Thermogravimetry analysis was used to study the thermal decomposition of Ti-MCM-41 to determine the best calcination conditions. Ti-MCM-41 molecular sieve was synthesized using a hydrothermal route in which Ti ions were incorporated into the pore channels of MCM-41 starting from a hydrogel method according to the following molar composition: 1.00 CTMABr:4.00 SiO 2 :X TiO 2 :1.00 Na 2 O:200.00 H 2 O. Physicochemical properties of samples were investigated using XRD, FTIR, and N 2 adsorptiondesorption to confirm the incorporation of TiO 2 nanoparticles inside of MCM-41 mesoporous without destroying its structure. The high temperatures facilitate the rapid removal of the surfactant; however, it caused destruction of the MCM-41 structure by breaking the bonds of the silica tetrahedral structure. The procedures to obtain the apparent activation energies of CTMABr decomposition were based on the kinetic model proposed by Flynn-Wall using thermal analysis of data performed with heating rates 5, 10, and 20 °C min -1 .