RESUMO
Soybean hulls, a co-product generated in high volumes, were used to obtain pulp and CMC. The pulping process was optimized with the aid of 1%, 2%, and 2.5% NaOH solutions at 90 °C for 2 h. A 22 central composite design was used in order to optimize the bleaching process and the CMC synthesis. Volumes of bleaching solution (VS) of between 55 and 65 mL/g at temperatures between 85 and 95 °C and VS of 70 and 75 mL/g at 95 °C were applied in the pulp bleaching process. The factors considered in the carboxymethylation were the chloroacetic acid mass (1.2-2.1 g/g) and the reaction time (192-228 min), at 63 °C. The soybean hulls contain 40.62% of cellulose and have a low lignin content. The pulping process was optimized when 1% NaOH was used at 90 °C/2 h and bleaching process applying VS = 75 mL at 95 °C/4 h. The pulps showed low lignin content (<6%) and the cellulose had a high degree of crystallinity. The SEM, 1H NMR, XRD, FTIR and TGA/DTG analysis results demonstrated that it is possible to synthesize CMC (DS = 1.45) by acetylating the bleached pulp with 2.1 g of chloroacetic acid for 192 min, at 63 °C.
Assuntos
Carboximetilcelulose Sódica/metabolismo , Glycine max/química , Carboximetilcelulose Sódica/química , Celulose/química , Celulose/metabolismo , Lignina/metabolismo , Microscopia Eletrônica de Varredura , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Difração de Raios XRESUMO
The process employed for the pulping and bleaching of sorghum straw was optimized prior to the synthesis of cellulose acetate. A 22 factorial central composite design was carried out. The variables considered were cooking time (1.5 to 2.5â¯h) and dilute alkali concentration (0.75 to 1.25%) for the pulping and bleaching time (30 to 35â¯min) and bleach volume (20 to 25â¯mL) for the bleaching. The sorghum straw was comprised of 49.43% α-cellulose, 19.18% hemicellulose and 30.42% lignin. The optimum conditions that maximize these processes were 2.5â¯h and 1.25% (dilute alkali concentration) at 90⯰C, and 35â¯min and 25â¯mL (bleach volume) at 80⯰C, respectively, providing pulps with a low Kappa number (<3) and lignin content, and cellulose with a high degree of crystallinity. The 1H NMR, XRD, FTIR spectroscopy, SEM and thermal analysis demonstrated that it is possible to synthetize cellulose acetate (with 2.62 degrees of substitution) by acetylating bleached pulp for 16â¯h at 25⯰C.