The use of acid mud produced during the aluminum extraction of kaolinite to synthesize mobil composition of matter no. 41 (MCM‐41) type material is proposed in this work. The acid mud was placed in contact with NaOH at 550°C to release the silicon and aluminum, then the fused material obtained was mixed with cetyltrimethylammonium bromide (CTAB) followed by a hydrothermal treatment considering a factorial design 2k with four experimental factors (CTAB dose, synthesis time, temperature, and solid/liquid ratio). The formation of MCM‐41 was evaluated via X‐ray diffraction (XRD) and scanning electron microscopy coupled with electrons dispersive spectroscopy (SEM‐EDS) analysis complemented with surface area analysis from which a maximum value of 550 m2/g was obtained for the best material. XRD results showed the typical pattern of MCM‐41 measured at low angle, furthermore, the characteristic type IV isotherm of adsorption–desorption was observed in certain materials. The elemental analysis showed the presence of iron and titanium oxide, which could be of great interest for the use of the material as a photocatalyst. Preliminary tests, using the MCM‐41 samples synthesized and methyl orange revealed a moderate photocatalytic activity of the material as compared to a commercial product (P25); opening up opportunities for the further development of such materials as potential and cost‐effective photocatalysts for pollutants degradation in wastewater. © 2018 American Institute of Chemical Engineers Environ Prog, 38:e13069, 2019