Corncob is an abundant agricultural residue containing high content of hemicellulose. In this paper, the hemicellulosic hydrolysate was prepared from the hydrolysis of corncob using the solid acid sulfated zirconia as a catalyst. According to response surface analysis experiments, the optimum conditions for preparing hemicellulosic hydrolysate catalyzed by sulfated zirconia were determined as follows: solid (sulfated zirconia)-solid (corncob) ratio was 0.33, solid (corncob)-liquid (water) ratio was 0.09, temperature was 153 degrees C, and time was 5.3 h. Under the optimized conditions, the soluble sugar concentration was 30.12 g/L with a yield of 033 g/g corncob. Subsequently, xylitol production from the resulting hemicellulosic hydrolysate was demonstrated byCandida tropicalis, and results showed that the yield of xylitol from the hemicellulosic hydrolysate could be significantly improved on a basis of decolorization and detoxification before fermentation. The maximum yield of xylitol from the hemicellulosic hydrolysate fermented byC. tropicaliswas 0.76 g/g. This study provides a new attempt for xylitol production from the hemicellulosic hydrolysate.