Fly ash is a kind of industrial solid waste, which mainly comes from thermal power plants using coal as power fuel. The lack of effective disposal and utilization of fly ash has led to its not only destroying and polluting the ecological environment but also seriously endangering human health. In addition, the treatment of ammonia nitrogen wastewater is an important issue in environmental pollution control, so the study of efficient and low-cost separation materials has become a challenging topic. This study utilises the hydrothermal method to convert fly ash into fly ash-based zeolite, which is capable of treating ammonia nitrogen wastewater. The successful synthesis of Zeolite X, zeolite A and zeolite A-X are confirmed through various characterisation techniques, including XRD, TG-DSC, TEM, BET, and FT-IR. Simultaneously, the synthesized zeolite is tested for its capacity to adsorb and regenerate ammonia nitrogen wastewater. The pure zeolite with the largest adsorption capacity, simpler preparation process, good stability, and high regeneration capacity is selected.