The environmentally benign, harmless to human, and economically effective process to produce high-purity amorphous SiO2 materials from rice husks has been established by using a carboxylic acid leaching, not the conventional strong acids. TG-DTA measurement and GCMS analysis indicated that the leaching was effective for the hydrolysis of celluloses and hemicelluloses contained in rice husks at 473–873 K, which produced the same results in using the conventional sulfuric acid. In particular, the formation of furfurals and levoglucosans occurred via the hydrolysis at 473 K and 673 K, respectively, when using rice husks leached by citric acid solutions. The metallic impurities could be also removed from the husks via a chelate reaction between carboxyl groups (–COOH) and the metal elements. Concerning the burning conditions of rice husks after the acid leaching, it was necessary to supply a suitable amount of air to completely combust organics; for example, it required air supplement of 50 mL/min or more. High-purity amorphous silica materials with 99 wt% or more were prepared from rice husks by applying the citric acid leaching treatment and burning process at 1073 K in air.