This study aimed to evaluate the yield and efficiency of lignin extraction from Eucalyptus grandis × Eucalyptus urophylla wood chips from treatments with sodium xylenesulphonate (SXS), and to determine their optimum conditions. First the wood’s physical, chemical, and morphological properties were characterized. Then, the wood chips underwent treatments from a combination of the following factors: time, SXS concentration, and temperature. For each treatment the yield and lignin content remaining in wood chips was determined, from which optimum points were obtained for maximum yield and lignin extraction. The physical, chemical, and morphological characterization showed that the concerned wood showed values in line with those cited in previous literature. Treatments with SXS were efficient in lignin extraction. The treatment that provided the highest calculated yield of wood was 1 h, 0%, 117.5 ºC; and the greatest lignin extraction was with 12 h, 30%, 130 ºC, removing 39.6% of lignin from wood chips. In general, the treatment of E. grandis × E. urophylla wood chips with SXS was effective in extracting lignin. However, the calculated yield and lignin extraction showed antagonistic behaviors; therefore, in light of the objectives, a careful assessment is required when using this treatment on an industrial scale to seek a balance point between the two parameters.