Mesostructured pillared zeolite materials in the form of lamellar phases with a crystal structure of mordenite (MOR) and ZSM-5 (MFI) were grown using CTAB as an agent that creates mesopores, in a one-pot synthesis; then into the CTAB layers separating the 2D zeolite plates were introduced by diffusion the TEOS molecules which were further hydrolyzed, and finally the material was annealed to remove the organic phase, leaving the 2D zeolite plates separated by pillars of silicon dioxide. To monitor the successive structural changes and the state of the atoms of the zeolite framework and organic compounds at all the steps of the synthesis of pillared MOR and MFI zeolites, the nuclear magnetic resonance method (NMR) with magic angle spinning (MAS) was applied. The ²⁷Al and ²⁹Si MAS NMR spectra confirm the regularity of the zeolite frameworks of the as synthetized materials. Analysis of the ¹H and ¹³C MAS NMR spectra and an experiment with variable contact time evidence a strong interaction between the charged “heads” –[N(CH₃)₃]⁺ of CTAB and the zeolite framework at the place of [AlO₄]⁻ location. According to ²⁷Al and ²⁹Si MAS NMR the evacuation of organic cations leads to a partial but not critical collapse of the local zeolite structure.

A chabazite-type zeolite was prepared by the hydrothermal method. Before ion exchange, the chabazite was activated with ammonium chloride (NH₄Cl). The ion exchange process was carried out at a controlled temperature and constant stirring to obtain ion-exchanged chabazites of Ti⁴⁺ chabazite (TiCHA), Zn²⁺ chabazite (ZnCHA), Cu²⁺ chabazite (CuCHA), Ag⁺ chabazite (AgCHA) and Au³⁺ chabazite (AuCHA). Modified chabazite samples were characterized by X-ray diffraction (XRD), scanning electron microscope equipped with energy-dispersive spectroscopy (SEM-EDS), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), N₂ adsorption methods and UV–visible diffuse reflectance spectroscopy (DRS). XRD results revealed that the chabazite structure did not undergo any modification during the exchange treatments. The photocatalytic activity of chabazite samples was evaluated by the degradation of methylene blue (MB) in the presence of H₂O₂ under ultraviolet (UV) light illumination. The photodegradation results showed a higher degradation efficiency of modified chabazites, compared to the synthesized chabazite. CuCHA showed an efficiency of 98.92% in MB degradation, with a constant of k = 0.0266 min⁻¹ following a first-order kinetic mechanism. Then, it was demonstrated that the modified chabazites could be used for the photodegradation of dyes.