Abstract: Zeolite phase adsorbents were prepared by roasting activation hydrothermal two-step method with illite as raw materials and calcium carbonate and calcium sulfate as activators, and their adsorption properties for heavy metal ion Cr³⁺ were studied. The optimum conditions for the preparation of zeolite phase adsorption materials were determined as follows: the mass ratio of sodium silicate to sodium metaaluminate was 2∶1, the solid-liquid ratio was 1∶10, and the hydrothermal temperature was 150 ℃. The adsorption performance of zeolite phase adsorbent for Cr³⁺ was also studied, the initial pH value of the solution was 6.5, the initial concentration of the solution was 20 µg/mL, and the addition amount of adsorbent was 0.03 g, the adsorption rate of zeolite adsorbent for Cr³⁺ was 90.52%. The kinetic of zeolite adsorption materials for Cr³⁺ meets the quasi second-order kinetics, the adsorption process shows that it is Freundlich isothermal adsorption model, which is mainly multi-layer chemical adsorption.