The invention relates to a novel process for preparing xylitol, which belongs to the technical field of functional sugar alcohol production. Pre-treatment, hydrolysis, neutralization, decoloring, ion exchange, evaporation and concentration and chromatography are carried out to corncob or bagasse and other agricultural waste which contains hemicellulose, high-content xylose solution is collected and distillated, and then continuously hydrogenated, so that the xylose solution is converted into xylitol solution, and finally a xylitol crystal is obtained through refining, concentration, crystallization, centrifugation and drying; the process comprises: corncob-> pre-treatment->hydrolysis->neutralization and decoloring->ion exchange->evaporation and concentration->chromatography->high-content xylose solution collection and distillation-> hydrogenatio->refining->concentration->crystallization->centrifugation->drying->finished crystal xylitol product obtaining. The novel process for preparing xylitol saves a xylose crystallization procedure and a conversion process xylose crystal into sugar, shortens a production procedure, adopts a chromatography technology to improve the content of thexylose solution, facilitates the obtaining of high-content xylitol solution after hydrogenation can prepare the high-grade xylitol product, adopts a continuous hydrogenation process, improves the hydrogenation efficiency, reduces the labor intensity of a worker, and saves the production cost.