Synthesis and characterization of methylcellulose produced from bacterial cellulose under heterogeneous condition
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In this work, methylcellulose (MC) was produced from bacterial cellulose (BC), using dimethyl sulfate in a 3 h (MC3h) or 5 h (MC5h) reaction under heterogeneous conditions, with reagent substitution at each hour. MC3h showed a degree of substitution (DS) of 2.26 ± 0.13 and MC5h showed a DS of 2.33 ± 0.05. The two samples were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), differential thermal analysis (DTA), thermal gravimetric analysis (TGA), <sup>13</sup>C nuclear magnetic ressonance (NMR) and <sup>1</sup>H NMR techniques. The FTIR spectra of the BC and MC samples present significant differences in the regions from 3750 to 2750 cm<sup>-1</sup> and from 1500 to 750 cm<sup>-1</sup>, which evidence the methylation of the samples. Solid state NMR spectroscopy of the MC samples was used to identify the <sup>13</sup>C NMR signals of substitution at sites C-2, C-3 or C-6 in the glucopyranose units. The modification of bacterial cellulose produced a material with a high DS, determined by three different techniques (chemically and using the liquid <sup>1</sup>H and solid <sup>13</sup>C NMR spectra). These samples also demonstrate high crystallinity and thermal stability. With the MC samples synthesized in this work, transparent and resistant films were prepared and also a highly porous sponge like material.