<p>Corncob, an agricultural based lignocellulosic biomass (LCB) feedstock is wasted during the collection of corn grains in agro-industries, despite containing 15–20% of lignin, a potential renewable source of chemical and fuels. The isolation of lignin from the LCB in high purity and less condensed form is a major challenge. This study focuses on the optimization of the organosolv process (OS) for lignin isolation from corncob using THF-H<sub>2</sub>O solvent mixture. The design of experiment (DoE) based machine learning driven regression model was employed by considering reaction time, temperature, THF: H<sub>2</sub>O ratio, solid: liquid ratio as degrees of freedom. A combination of Central Composite Design (CCD) and SOBOL sampling ensured uniform coverage of the experimental space. Ridge regression modeling was used to identify optimal conditions for maximum lignin yield. The optimized lignin isolation conditions (reaction time: 95&#xa0;min, temperature: 230&#xa0;°C, THF: H<sub>2</sub>O: 4:1, solid: liquid: 0.0801:1) yielded 47.4% lignin with 81.3% purity. Analysis of variance (ANOVA) was conducted to study the impact of the interaction of process parameters on lignin yield based on the p-value. The isolated lignin was characterized by elemental analysis (CHNSO), powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), <sup>1</sup>H and <sup>13</sup>C nuclear magnetic resonance spectroscopy (NMR), and thermogravimetric analysis (TGA) methods. The characterization results confirmed that the OS lignin is amorphous in nature, thermally stable and contains aromatic, aliphatic, C-C moieties, and β-O-4&#xa0;linkages including other linkages similar to kraft lignin. Comparison of characterization results with kraft lignin (KL) ensures the efficacy of the OS extraction method for isolation of the high-quality lignin from corncob.</p> Graphical Abstract <p></p>

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Optimization of organosolv process for isolation of lignin from corncob in THF-H2O solvent mixture

  • Sakshi Manekar,
  • Rashi Verma,
  • Kolli Harsha Vardhan,
  • Kishalay Mitra,
  • Debaprasad Shee

摘要

Corncob, an agricultural based lignocellulosic biomass (LCB) feedstock is wasted during the collection of corn grains in agro-industries, despite containing 15–20% of lignin, a potential renewable source of chemical and fuels. The isolation of lignin from the LCB in high purity and less condensed form is a major challenge. This study focuses on the optimization of the organosolv process (OS) for lignin isolation from corncob using THF-H2O solvent mixture. The design of experiment (DoE) based machine learning driven regression model was employed by considering reaction time, temperature, THF: H2O ratio, solid: liquid ratio as degrees of freedom. A combination of Central Composite Design (CCD) and SOBOL sampling ensured uniform coverage of the experimental space. Ridge regression modeling was used to identify optimal conditions for maximum lignin yield. The optimized lignin isolation conditions (reaction time: 95 min, temperature: 230 °C, THF: H2O: 4:1, solid: liquid: 0.0801:1) yielded 47.4% lignin with 81.3% purity. Analysis of variance (ANOVA) was conducted to study the impact of the interaction of process parameters on lignin yield based on the p-value. The isolated lignin was characterized by elemental analysis (CHNSO), powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), 1H and 13C nuclear magnetic resonance spectroscopy (NMR), and thermogravimetric analysis (TGA) methods. The characterization results confirmed that the OS lignin is amorphous in nature, thermally stable and contains aromatic, aliphatic, C-C moieties, and β-O-4 linkages including other linkages similar to kraft lignin. Comparison of characterization results with kraft lignin (KL) ensures the efficacy of the OS extraction method for isolation of the high-quality lignin from corncob.

Graphical Abstract