Pre-processing provides an effective way for fly ash's high value-added utilization. However, the shortcomings of pre-processing methods such as grinding and flotation are apparent with many disadvantages that make it more challenging to use efficiently. Microwave heating helps the SiO₂-Al₂O₃ bond break, not only can make the structural change of the material can also promote the chemical reaction process. In the article, XRD, SEM, FT-IR, ammonia nitrogen adsorption, and other methods were used to analyze the changes in the properties of fly ash before and after microwave pre-treatment, the change in adsorption performance of fly ash before and after microwave treatment was analyzed. The study found that under microwave conditions of 600 W and 15 min, the adsorption rate of ammonia nitrogen by fly ash reached a maximum of 29.67%. The intensity of mullite and amorphous diffraction peaks decreased after 20 min at 600 W. The Si-O-(Si, Al) and Si-O-(Si) bonds showed significant changes at 15 min and 20 min under 600 W conditions. Based on the results, the microwave conditions were selected at 600 W for different periods, and semi-quantitative analysis was carried out by XRD-Rietveld, infrared peak fitting, and nuclear magnetic resonance. The XRD-Rietveld analysis showed that the amorphous phase content reached 46.18% at 15 min. In the infrared peak fitting, the fitting area at 1300-900 cm^-1 and 600-400 cm^-1 peaks at 56.92% at 25 min and 17.5% at 15 min, respectively. The silicon-oxygen network's degree of connection and polymerization was reduced after 15 min of microwave treatment for the nuclear magnetic resonance analysis. By combining specific surface area measurements, it was discovered that the maximum specific surface area attained a value of 3.122 m²/g at 15 min.