Navegando por Assunto "13C multiple cross-polarization solid-state"

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    Synthesis and application of sugarcane bagasse cellulose mixed esters. Part II : removal of Co2+ and Ni2+ from single spiked aqueous solutions in batch and continuous mode.
    (2019) Almeida, Francine Tatiane Rezende de; Carvalho, Megg Madonyk Cota Elias; Xavier, Amália Luísa Pedrosa; Ferreira, Gabriel Max Dias; Silva, Isabela Almeida; Filgueiras, Jefferson Gonçalves; Azevedo, Eduardo Ribeiro de; Silva, Luís Henrique Mendes da; Gil, Laurent Frédéric; Gurgel, Leandro Vinícius Alves
    Sugarcane bagasse cellulose succinate trimellitate (SBST) was prepared by a one-pot synthesis method. The synthesis of this novel mixed ester was investigated by a 23-factorial design. The parameters investigated were time, temperature, and succinic anhydride mole fraction (χSA). The responses evaluated were the adsorption capacity (qCo2+ and qNi2+), weight gain (wg), and number of carboxylic acid groups (nT,COOH). 13C Multiple Cross-Polarization solid-state NMR spectroscopy, 1H NMR relaxometry, and Fourier-transform infrared spectroscopy were used to elucidate the SBST structure. The best SBST reaction conditions were 100 °C, 660 min, and χSA of 0.2, which yielded SBST with a wg of 57.1%, nT,COOH of 4.48 mmol g−1, and qCo2+ and qNi2+ of 0.900 and 0.963 mmol g−1, respectively. The maximum adsorption capacities (Qmax) (pH 5.75, 25 °C) estimated by the Redlich-Peterson model for Co2+ and Ni2+ were 1.16 and 1.29 mmol g−1. The ΔadsH° values for Co2+ and Ni2+ adsorption obtained by isothermal titration calorimetry were 8.03 and 6.94 kJ mol−1. Regeneration and reuse of SBST were investigated and the best conditions applied for fixed-bed column adsorption in five consecutive cycles. SBST was fully desorbed and Qmax values for Co2+ (0.95 mmol g−1) and Ni2+ (1.02 mmol g−1) were estimated using the Bohart-Adams model.