Composite zeolite sorbents based on analcime with inclusions of hydrated zirconium dioxide (ZrO2-analcime) have been obtained by hydrothermal treatment of coal fly ash cenospheres with a high glass phase content in the presence of a zirconium compound and an alkaline activating agent at 150 °C and different stirring modes of the reaction mixture. The synthesis products were characterized by XRD, SEM-EDS, STA and low-temperature nitrogen adsorption; their sorption properties with respect to Cs+ and Sr2+ were studied in the pH range of 2–10. It was found that the ZrO2-analcime compositions surpass unmodified analcime by 2–5 times in terms of sorption of Cs+ and Sr2+ and by two orders of magnitude in terms of the distribution coefficient value (KD ~106 ml/g). The process of high-temperature solid-phase transformation of Cs+/Sr2+-exchanged forms of the compositions was studied, which simulates the process of conversion of water-soluble forms of Cs‑137 and Sr‑90 radionuclides into a mineral-like form. It was shown that at 1000 °C the ZrO2-analcime compositions with sorbed Cs+ and Sr2+ undergo the phase transformation resulting in polyphase systems of similar composition based on nepheline, tetragonal ZrO2, and glass phase