The preparation of xylo-oligosaccharides(XOSs)through hydrolysis of hemicelluloses was studied.The hemicelluloses were isolated from the press lye discharged in the production of viscose,which contained about 30%xylan.Then,a factorial experimental design was applied to compare the influences of several factors including the concentrations of sulphuric acid and hemicelluloses,the duration and temperature of the hydrolysis,on the conversion of xylan,and the selectivity for the product–XOSs.The results showed that the hydrolysis duration affects the yield of XOSs to the greatest extent.It is difficult to obtain a high yield of XOSs with sulphuric acid as the hydrolysis catalyst.