Abstract Lignocellulosic biomass is considered a sustainable source for the production of biofuels and platform molecules such as furfural (FAL). In this study, a series of solids with different acidity were tested for the production of FAL from xylose and corn residues. Functionalized Cloisite Na + (CLOI-SO 3 H) and Preyssler heteropolyacid (HPA-Preyssler) showed the best catalytic performance in the production of FAL form xylose. Under optimal reaction conditions, the HPA-Preyssler catalyst achieved a maximum yield of 75% in just 15 min and maintained its activity for 5 consecutive reaction cycles, while the CLOI-SO 3 H catalyst obtained a 97% yield in 15 min, but its activity decreased considerably during reuse. Using techniques such as FTIR, SEM, EDS, and TGA, the possible causes of the decrease in the activity of the catalysts were established. The cellulose, hemicellulose, and lignin contents of different corn residues were determined to determine the most appropriate for the production of FAL. Using the HPA-Preyssler, the temperature and amount of catalyst selected for the dehydration of xylose to FAL, the appropriate time, amount of substrate, and type of solvent were established to obtain FAL directly from yellow corn stalks, reaching a maximum yield of 14% concerning hemicellulose content in 3 h at 180 °C in DMSO without performing any pretreatment to the corn residues, and the catalyst was recovered for subsequent reactions. Therefore, using the HPA-Preyssler catalyst is a new alternative for efficiently converting xylose or residual lignocellulosic biomass into FAL.