Propyl-sulfonic (PS) acid-functionalized nanoparticles were synthesized, characterized and evaluated as catalysts for pretreatment of corn stover. Silica coated nanoparticles were functionalized with 0.5% mercaptopropyltrimethoxysilane (MPTMS) at neutral pH in a mixture of water and ethanol. Sulfur contents of the acid functionalized nanoparticles, measured in a CHNS analyzer, varied from 6%-10%, and the acid load ranged from 0.040 to 0.066 mmol H + /g. A Box-Behnken design was employed to calculate the minimum number experiments required to obtain an estimate of the surface response for temperature, catalyst load, and %S content of the catalyst. Pretreatment of corn stover was carried out at three temperature levels 160, 180, and 200˚C for 1 h. Three levels of catalyst load were used 0.1, 0.2, and 0.3 g of catalyst per gram of biomass. Hydro-thermolysis controls were carried at each temperature level. The catalyst load did not have an effect on the glucose yield at 160˚C, and the average glucose yield obtained at this temperature was 59.0%. The glucose yield was linearly correlated to the catalyst load during pretreatment at 180˚C, and a maximum glucose yield of 90% was reached when using 0.2 g of PS nanoparticles that had a total sulfur content of 6.1%. Complete hydrolysis of glucose was reached at 200˚C but the average xylose yield was 4.6%, and about 20.2% of the combined glucose and xylose were lost as hydroxymethylfurfural and furfural. Results showed that acid-functionalized nanoparticles can be potential catalysts for the pretreatment of biomass for its later conversion to ethanol.