Hyper cross linkage phosphothiol polymer (HCPTP) is a new adsorbent that offers an excellent synergistic effect for the adsorption of Zirconium ions. FT-IR, 1HNMR, 13C, and 31P NMR, FTIR, SEM, GC-Mass, and BET were used to characterize the modified new chitosan adsorbent. The Freundlich isotherm model accurately represents the adsorption effect with a maximum adsorption capacity of 307 mg/g. It was noted that the up-taking process of Zirconium ions corresponded more closely to the pseudo-second order kinetic. The thermodynamic tools ΔS, ΔH and ΔG were also evaluated indicating spontaneous endothermic adsorption process with a randomness increasing. The prepared new adsorbent is successfully used to adsorption of Zirconium ions from the actual leach liquor of Egyptian Rosetta zircon sample.