Sugarcane bagasse cellulose mixed ester succinate phthalate (SBSPh) was synthesized by a novel one-pot reaction method. The effects of temperature, time and mole fraction of succinic anhydride (chi(SA)) on the responses weight gain (wg), number of carboxylic acid groups (n(T,COOH)), and adsorption capacity (q) of Co2+ and Ni2+ were evaluated by a 2(3) experimental design. The chemical structure of the material was elucidated by Fourier transform infrared, C-13 Multiple Cross-Polarization solid-state NMR spectroscopy and H-1 NMR relaxometry. The best SBSPh synthesis condition (100 degrees C, 11 h, chi(SA) of 0.2) yielded a wg of 59.1%, n(T,COOH) of 3.41 mmol g(-1), and values of q(co)(2+) and q(Ni)(2+) of 0.348 and 0.346 mmol g(-1), respectively. The Sips model fitted better the equilibrium data, and the maximum adsorption capacities (pH 5.75 and 25 degrees C) estimated by this model were 0.62 and 0.53 mmol g(-1) for Co2+ and Ni2+, respectively. The Delta H-adS degrees values estimated by isothermal titration calorimetry were 8.43 and 7.79 kJ mol(-1) for Co2+ and Ni2+, respectively. Desorption and re adsorption efficiencies were evaluated by a 2(2) experimental design, which showed that SBSPh adsorbent can be recovered and reused without significant loss of adsorption capacity. (C) 2018 Elsevier Inc. All rights reserved.