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Author: search.filters.author.Peralta, MicaelaSubject: search.filters.subject.Hydroxymethylation

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    Mechanistic insight into hydroxy‑methylation of hardwood kraft lignin
    (2024-09-24) Peralta, Micaela; Pajer, Nicolò; Crestini, Claudia; Nicolau, Verónica V.
    In view of developing upcycling strategies for hardwood Kraft lignin, hydroxymethylation of Eucalyptus Kraft lignin under alkaline conditions (pH 9 and 11) at different temperatures (50 °C and 70 °C) was studied in the present effort with the double objective of optimizing the reaction conditions and understanding the functionalization mechanism of C5 in either terminal or internal guaiacyl units during hydroxy-methylation. Formaldehyde consumption was estimated via titration of the oximated free formaldehyde; the hydroxy-methylation degree under the reaction was estimated by calculating the ratio in Condensed hydroxyl/Guaiacyl (Condensed OH/G-OH) via a new difference UV-spectroscopy. The reliability of the difference UV-method results for the analyses of the hydroxy-methylated lignins was statistically analysed and compared with that of vacuum-dried and sonicated samples. Hydroxy-methylated samples were then fully characterised by NMR (31P and HSQC) and GPC. The reaction temperature of 50 °C, pH 11, and period time of one hour resulted as the optimal conditions for the hydroxy-methylation, preventing the side-reactions leading to the formation of dimethylene-glycol addition products.The 31P and 1H–13C HSQC NMR revealed the absence of undesirable formaldehyde Cannizzaro by-products and the lack of hydroxymethyl groups in the aliphatic side chain under the studied conditions. GPC analyses, comparing two methodologies, revealed increases in molar mass of the hydroxy-methylated samples upon the formaldehyde addition. The selective hydroxy-methylation at the C5 guaiacyl site demonstrates that Eucalyptus Kraft lignin is as a promising candidate for resolproduction
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    Lignin-phenol-formaldehyde resol for high pressure decorative laminates evaluation of lignin levels on final properties
    (2023-06) Peralta, Micaela; Nicolau, Verónica V.
    High pressure decorative laminates (HPDL) are composite materials made of core layers of Kraft papers impregnated with a resol type phenol-formaldehyde resin (PF) and a surface décor paper saturated with melamine-formaldehyde resin (MF). The set of saturated papers is cured by compression moulding at high pressure and high temperature. In the aim of replacing non-renewable petroleum-based phenol (P), among biomass components, lignin (L) seems to be an attractive substitute owing to its structural similarity to PF resins. In this sense, hardwood Eucalyptus spp species are the main source of Kraft L in South America. However, the poor solubility and reactivity limit its exploitation in resol resins making necessary a previous chemical modification such as hydroxymethylation in alkaline conditions [1]. Free F increased with L levels in resols being less than 2% for P replacements up to 60 wt%. The resistance to immersion in boiling water test exhibited higher increase in weight and thickness with higher L levels. Delamination and blister defects were observed for HPDLs with 70 and 80 wt% P replacement. Weight increments for HPDL with 0% and 60% P substitution were 5.66 (±0.37)% and 7.60 (±0.56)% meanwhile thickness increments were 8.97 (±1.60)% and 10.22 (±0.45)%, respectively. Gaining on weight and thickness comply the Australian/New Zealand Standard AS/NZS 2924.1:1998 specifications, thus demonstrating hardwood L as a high potential substitute for P in HPDLs manufacturing.
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    Determinación de grupos hidroxilo fenólicos reactivos en lignina Kraft de madera dura por titulación acuosa potenciométrica
    (AJEA- Actas de Jornadas y Eventos Académicos de UTN, 2023-12) Peralta, Micaela; Dobler, Santiago; Lesta, Mateo Ariel; Nicolau, Verónica V.
    Las ligninas Kraft son polímeros naturales polifenólicos de estructura compleja cuya baja reactividad puede sortearse mediante la activación por hidroximetilación con incorporación de grupos hidroximetilo reactivos necesarios en la fabricación de poliuretanos y adhesivos fenólicos. El trabajo experimental consistió en la optimización de una técnica potenciométrica para la determinación de grupos hidroxilo fenólicos y su monitoreo durante la funcionalización de una lignina de madera dura por hidroximetilación a temperaturas de 50 y 70 °C y pH 9 y 11. La optimización de la técnica potenciométrica permitió una reducción del 38 % en el tiempo de pretratamiento total de la muestra. La lignina hidroximetilada a pH 11 y 70 °C exhibió la mayor conversión (31 %) de grupos hidroxilo fenólicos.