This work focues on the development of a heterostructure composed by two semiconductors, capable to decrease the electron/hole recombination rate through a robust charge separation, and at the same time, this nanohybrid is sensitive to visible light spectrum. The charge separation is achieved by the injection of free electrons within the conduction band (BC) of TiO2 in anatase form, which come from the highest-occupied-molecular-orbital (HOMO) of acetylacetone (Acac), linked to the anatase nanoparticles, followed by the injection into unoccupied Fe3+ d-orbital within band-gap energy of the ferrititanate nanosheets. Additionally, the absorption of visible light could be assured by ferrititanate nanosheets, considering the interaction of the energy levels of Fe3+ with visible light and the valence and conduction bands, as well as, the formation of the charge transfer complex (CTC), between the anatase nanoparticles and Acac. The mesoporous nanohybrids (called also as heterostructures) were produced by different routes of junction of two components: i) ferrititanate nanosheets, which were synthesized from ilmenite mineral sands, and then they were exfoliated into single layers and ii) TiO2 nanoparticles, modified with Acac, which formed the CTC. The characterization techniques, such as N2 adsorption-desorption, photoluminescence emission spectroscopy (PL) and diffuse reflectance spectroscopy (DRS), and so on, confirmed the formation of the mesoporous heterostructures sensitive to visible light and with a robust mechanism of charge separation. The photodegradation of NO pollutant gas within the visible light spectrum through several mesoporous nanohybrids (photocatalysts) demonstrated being well succeeded, exhibiting an efficiency more than seven times higher than the activity benchmark TiO2 (Degussa P-25) photocatalyst.