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The hydrolysis of rice straw into xylose and glucose in dilute sulfuric acid aqueous solution was studied with a two-step process in batch autoclave reactor. The results showed that compared with the traditional one-step acid hydrolysis, both xylose and glucose could be produced in high yields from rice straw by using the two-step acid hydrolysis process. The effects of reaction temperature, reaction time, the amount of rice straw and acid concentration on the hydrolysis of rice straw were systematically studied, and showed that except initial rice straw loading amount, the other parameters had remarkable influence on the products distribution and yields. In the first-step of the hydrolysis process, a high xylose yield of 162.6 g·kg-1 was obtained at 140℃ after 120 min reaction time. When the solid residues from the first step were subjected to a second-step hydrolysis, a glucose yield as high as 216.5 g·kg-1 could be achieved at 180℃ after 120 min. This work provides a promising strategy for the efficient and value-added utilization of agricultural wastes such as rice straw. [ABSTRACT FROM AUTHOR]