Navegando por Assunto "13C Multiple Cross-Polarization solid-state"

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    Synthesis and application of sugarcane bagasse cellulose mixed esters. Part I : removal of Co2+ and Ni2+ from single spiked aqueous solutions in batch mode using sugarcane bagasse cellulose succinate phthalate.
    (2019) Carvalho, Megg Madonyk Cota Elias; Ferreira, Gabriel Max Dias; Almeida, Francine Tatiane Rezende de; Rosa, Nathália Cristina Martins; Silva, Isabela Almeida; Filgueiras, Jefferson Gonçalves; Azevedo, Eduardo Ribeiro de; Silva, Luis Henrique Mendes da; Melo, Tânia Márcia Sacramento; Gil, Laurent Frédéric; Gurgel, Leandro Vinícius Alves
    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 (χSA) on the responses weight gain (wg), number of carboxylic acid groups (nT,COOH), and adsorption capacity (q) of Co2+ and Ni2+ were evaluated by a 23 experimental design. The chemical structure of the material was elucidated by Fourier transform infrared, 13C Multiple Cross-Polarization solid-state NMR spectroscopy and 1H NMR relaxometry. The best SBSPh synthesis condition (100 °C, 11 h, χSA of 0.2) yielded a wg of 59.1%, nT,COOH of 3.41 mmol g−1, and values of qCo2+ and qNi2+ 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 °C) estimated by this model were 0.62 and 0.53 mmol g−1 for Co2+ and Ni2+, respectively. The ΔadsH° 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 22 experimental design, which showed that SBSPh adsorbent can be recovered and reused without significant loss of adsorption capacity.