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A new theoretical and practical framework has been developed through operando study of the zeolite catalytic cracking of low‐density polyethylene (as a model reaction) under reaction conditions. Results show that microporous ZSM‐5 gives rise to less cracking products. Hierarchical ZSM‐5 zeolites are more active cracking catalysts, rendering more C2‐C5 hydrocarbons, with a delayed deactivation due to the secondary porosity. This tool in combination with thermogravimetric analysis provides complementary and valuable information for the study, and design of advanced catalysts.

The strength of the acidic sites rules the catalytic cracking: reduced acidic strength is not compensated by an increased accessibility of the acidic sites.

Comparative studies over micro-/mesoporous Cu-containing zeolites ZSM-5 prepared by top-down treatment involving NaOH, TPAOH or mixture of NaOH/TPAOH (tetrapropylammonium hydroxide) were conducted. The results of the catalytic data revealed the highest activity of the Cu-ZSM-5 catalyst both in the absence and presence of water vapor. The physico-chemical characterization (diffuse reflectance UV-Vis (DR UV-Vis), Fourier transform infrared (FT-IR) spectroscopy, electron paramagnetic resonance (EPR) spectroscopy, temperature-programmed desorption of NOx (TPD-NOx), and microkinetic modeling) results indicated that the microporous structure of ZSM-5 effectively stabilized isolated Cu ion monomers. Besides the attempts targeted to the modification of the textural properties of the parent ZSM-5, in the next approach, we studied the effect of the co-presence of sodium and copper cations in the microporous H-ZSM-5. The presence of co-cation promoted the evolution of [Cu–O–Cu]2+ dimers that bind NOx strongly with the desorption energy barrier of least 80 kJ mol−1. Water presence in the gas phase significantly decreases the rate of ammonia oxidation, while the reaction rates and activation energies of NH3-SCR remain unaffected.