Ethanol production from renewable sources, such as lignocellulosic materials, is already underway in several countries. The interest in the technology stems from concerns about global warming and the environmental impacts of solid waste disposal. Moreover, the conversion of agro-industrial wastes into ethanol is a value-adding strategy. This study aimed to evaluate the physicochemical characteristics of three lignocellulosic materials— rice straw bran, sugarcane bagasse, and corn peel bran—and determine, on the basis of these analyses, their suitability as feedstocks for second-generation ethanol production. Physicochemical characterization included the determination of particle size, moisture, ash, total solids, water activity, crude fat, protein, total extractives, soluble and insoluble lignin, holocellulose, cellulose, hemicellulose, and total carbohydrates. Rice straw bran is composed of 38.33% cellulose and 19.73% hemicellulose, sugarcane bagasse is composed of 27.09% cellulose and 5.61% hemicellulose, and corn peel bran is composed of 55.75% cellulose and 12.93% hemicellulose. The characterization showed the high concentration of cellulose in the residue of the corn peel bran. The results indicate that the three biomasses are suitable raw materials for biofuel production.