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Shi, Shuai, et al. Industrial Crops and Products 214 (2024): 118524.
Tetramethylammonium hydroxide (TMAH) demonstrates exceptional efficiency as an alkaline extraction solvent for isolating hemicellulosic polysaccharides from lignocellulosic biomass. In this study, 20% aqueous TMAH was employed to extract arabinoxylan from reed straw (AXRS), enabling complete dissolution of the polysaccharide fraction under mild conditions. Reed straw powder was treated with TMAH at 50 °C for 4 hours, followed by neutralization, ethanol precipitation, and purification to yield AXRS with high recovery.
Compositional analysis revealed that TMAH-extracted AXRS consisted primarily of D-xylose and L-arabinose, displaying a relatively low molecular weight of 104 kDa as determined by HPLC and GPC. FT-IR, NMR, and XRD confirmed that the structural features of AXRS closely resemble arabinoxylans isolated from other biomass sources, demonstrating that the TMAH extraction process maintains the polysaccharide's native chemical architecture. Thermal analysis indicated water loss below 240 °C and major decomposition between 240 °C and 350 °C.
Rheological studies further highlighted the unique behavior of AXRS in 20% TMAH solution: complete dissolution occurred at low concentrations, while aggregation emerged beyond a critical concentration of ~0.062 g mL⁻¹, accompanied by significant increases in storage modulus.
Collectively, this work underscores tetramethylammonium hydroxide as a powerful solvent for the extraction, solubilization, and structural investigation of hemicellulosic polymers, offering a robust approach for biomass valorization and polysaccharide research.
Tian, Rui, et al. International Journal of Biological Macromolecules 254 (2024): 127499.
Tetramethylammonium hydroxide (TMAH) has emerged as a highly promising solvent for the selective fractionation of hemicelluloses from lignocellulosic biomass, providing an efficient pathway for biomass valorization. In this study, TMAH solutions of varying concentrations were used to pretreat poplar thermomechanical pulp (PTMP), enabling high-yield extraction of hemicellulosic fractions while preserving cellulose integrity.
Pretreatment with 25 wt% TMAH afforded the highest hemicellulose yield of 65.0%, accompanied by an impressive cellulose retention rate of 93.3%. Notably, delignification remained moderate (33.9%), highlighting the high selectivity of TMAH toward hemicellulose removal. The resulting hemicellulose fractions exhibited high molecular weights (109,800-118,500 g/mol), low Klason lignin content (3.2-5.9%), and a dominant 4-O-methylglucurono-β-D-xylan structure. Compared with conventional H₂SO₄ and NaOH methods, the TMAH-based process generated hemicelluloses of higher purity, greater structural completeness, and superior molecular integrity.
Importantly, TMAH pretreatment preserved the crystalline structure of cellulose, enabling a substantial improvement in enzymatic hydrolysis performance. The maximum glucose yield reached 57.5%, representing a 3.3-fold enhancement over untreated PTMP. Additionally, TMAH retained its fractionation efficiency after multiple recycling cycles, underscoring its potential for sustainable biorefinery operations.
This case study demonstrates tetramethylammonium hydroxide as an efficient and recyclable solvent for selective hemicellulose fractionation, offering significant advantages for poplar-based bioprocessing and lignocellulosic biomass conversion.
Tian, Rui, et al. Bioresource Technology 369 (2023): 128490.
This case study highlights the application of tetramethylammonium hydroxide (TMAH) as a highly effective solvent system for the selective fractionation of hemicelluloses from lignocellulosic biomass. Traditional alkaline solvents such as NaOH often lead to partial structural degradation, limiting the quality and molecular integrity of isolated hemicelluloses. In contrast, TMAH demonstrates superior solvating capability, enabling high-yield, room-temperature extraction while preserving polymeric structure.
Using poplar holocellulose as the model substrate, TMAH solutions (5-25 wt%) dissolved approximately 90% of hemicelluloses within 1 hour, delivering a hemicellulose yield of up to 81.9%, markedly higher and structurally more intact than those obtained via NaOH. Structural analyses confirmed that TMAH-extracted hemicelluloses exhibited higher purity and fewer degradation signatures, underscoring its mild yet efficient extraction mechanism.
Importantly, TMAH treatment maintained the integrity of the cellulose-rich residue. The cellulose retention rate reached 90.2%, and its crystallinity remained essentially unchanged, demonstrating that TMAH selectively targets hemicellulosic domains without compromising the cellulose framework. Additionally, the solvent was fully recoverable, enhancing the process sustainability and reducing operational cost.
Overall, TMAH provides a refined, energy-saving, and recyclable approach for the fractionation of hemicelluloses and purification of cellulose. This work positions tetramethylammonium hydroxide as a valuable reagent for biomass valorization, biorefinery development, and high-value polysaccharide production.
