A new technique of flyash utilization was presented and high-purity silica was prepared by alkali leaching. The flyash was added into sodium hydroxide solution, and then the suspension was heated to 115 °C for 30 min. After filtrated, the filtrate was collected and carbon dioxide was imported into the solution. Finally, the silica would precipitate from the solution. The silica was characterized by scanning electron microscopy, X-ray diffraction and X-ray fluorescence spectrometer. The high-purity silica prepared from flyash was qualified for the rubber reinforcing agent used in shoemaking.