Abstract: A series of new composites have been synthesized—TiO2 nanoparticles introduced in the interlayer space of layered mordenite. The effect of the hydrolysis medium of titanium tetraethoxide (water or a mixture of water with ethanol) and hydrolysis time (from 6 to 24 h) on the properties and texture of the composite was studied. Treatment in ethanol leads to partially preserved ordered layered structure of 2D mordenite, presumably due to the slowdown of the hydrolysis of titanium tetraethoxide; this, in turn, provides higher mesoporosity after calcination, created by anatase nanoparticles of ~4 nm in the interlayer space. Immobilization of TiO2 on the zeolite surface is indicated by the formation of Si–O–Ti bonds. © Pleiades Publishing, Ltd. 2024. ISSN 0036-0244, Russian Journal of Physical Chemistry A, 2024, Vol. 98, No. 10, pp. 2298–2301. Pleiades Publishing, Ltd., 2024.