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The reaction behaviors of A12O3 and SiO2 from high alumina coal fly ash during various alkali hydrothermal conditions were studied in this work.The X-ray diffraction (XRD), X-Ray fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR), and Scanning electron microscopy (SEM) analyses were used to measure the changes in crystal structure and morphology of the coal fly ash, the obtained solid samples after hydrothermal treatment, and the dissolved amount of Si4+ and A13+ in alkali solution.