Eucalyptus globulus wood was subjected to autohydrolysis pretreatment at different severity factors. The pretreated materials were enzymatically saccharified at a substrate load of 10% (w/v) using a cellulase enzyme complex. Around 82-95% of original glucans were retained in the pretreated material, and the enzymatic hydrolysis yields ranged from 58% to 90%. The chemical and structural changes in the pretreated materials were investigated by microscopic (SEM, LSCM) and spectroscopic (2D-HSQC NMR and FT-IR) techniques. 2D-NMR results showed a reduction in the amounts of β-O-4 aryl-ether linkages and suggested the presence of newly condensed structures of lignin in the biomass pretreated at the more severe conditions. Furthermore, the microscopic analysis showed that lignin migrates out of the cell wall and re-deposits in certain regions of the fibers at the more severe conditions to form droplet-like structures and expose the cellulose surface. These changes improved the glucose yield up to 69%, on dry wood basis.

This work aimed to evaluate the effect of the precipitation of CaCO3 via subsequential in-situ mineral formation based on a solution-exchange process of two solution-exchange cycles via impregnation with CaCl2 in ethanol and NaHCO3 in water. The effects were investigated in terms of the structure of the wood and the thermal, physical, mechanical, and decay resistance properties of nine species commonly used in commercial reforestation in Costa Rica. The thermogravimetric analysis results showed that the woods with the highest formation of CaCO3 showed a more pronounced signal at 200 °C in relation to untreated/wood; therefore, they were more thermostable. The fire-retardancy test showed that flame time in CaCO3/wood composites was longer than for untreated/wood in half of the species tested, presenting a positive effect of mineralization. Wood density, decay resistance, modulus of rupture (MOR), modulus of elasticity (MOE) in flexion, and MOR in compression were slightly affected by mineralization. Water absorption increased, but it had no negative effect on the dimensional stability. In general, mineralization can be a chemical treatment to increase the dimensional stability and fire resistance of hardwood species without modifying the wood’s physical and mechanical properties.

Eucalyptus globulus wood chips were subjected to autohydrolysis pretreatment at 175ºC at three different residence times. Part of the recovered solids were submitted to alkaline extraction with NaOH solution to remove leachable lignin. The chemical composition of the fibrous material was analyzed by HPLC, Py-GCMS and 2D-NMR HSQC, while morphological changes were evaluated by SEM and LSCM. The pretreated materials were hydrolyzed with cellulases at a substrate loading of 10% (w/v) for up to 72 h. Glucose yields (based on dry wood) obtained in the enzymatic hydrolysis ranged between 38% and 65%, depending on reaction time in the autohydrolysis pretreatment. After the alkaline extraction, no significant change was observed in the yields in the enzymatic hydrolysis at 72 h, but at the lower severities, the initial rates of saccharification increased. The main effect of the hydrothermal pretreatment was removal of hemicelluloses, resulting in enriched cellulose pulps. SEM and LSCM images of the hydrothermal pretreated samples showed a disruption of the fiber surface, mainly in those samples obtained at the higher severity. Py-GC/MS and HSQC analysis showed that no major changes in the lignin structure occurred in the samples obtained by autohydrolysis and further alkaline extraction. By autohydrolysis at the higher severity (So=4.02), the lateral chains in lignin were cleaved and the formation of lignin droplets was observed. Hemicelluloses removal and lignin redeposition as droplets in certain regions of the fiber surface was associated with the higher accessibility of cellulose and the yield increase of the enzymatic hydrolysis.

Acetylation of softwoods has been largely investigated to increase the dimensional stability and biological resistance of wood. However, the knowledge of this technology has not been applied to tropical hardwood species up to date. The objective of this work was to study the effect of acetylation on nine tropical hardwood species, from forest plantations in Costa Rica, by applying acetic anhydride in three different treatment times (1 h, 2.5 h, 4 h), as well as to evaluate this by Fourier-Transform Infrared Spectroscopy (FTIR). Results showed that weight percentage gain (WPG) of wood varied from 2.2 to 16.8%, with Vochysia ferruginea species showing the highest WPG, and Gmelina arborea and Tectona grandis species exhibiting the lowest WPGs. Tropical woods such as Enterolobium cyclocarpum, Hieronyma alchorneoides and Samanea saman exhibited statistical differences among treatment times, whereas the rest of the species studied showed no significant differences. In general, the most effective acetylation time was 2.5 h for all the species. The ratio of intensity (RI) from the FTIR spectra was greater at the 1732 cm −1 , 1372 cm −1 and 1228 cm −1 peaks for all tropical species, associated with lignin. A good correlation between the RI of those peaks and WPG was found; the same was also found between all RIs and each other. Meanwhile, RI associated to the hemicelluloses and lignin (1592 cm −1 and 1034 cm −1 peaks, respectively) showed no correlation with WPG, nor between each other or with the other RIs. Furthermore, it was suggested that RI at 1732 cm −1 (associated to acetyl groups C=O) can be considered as a reliable indicator of the degree of acetylation for tropical hardwood species. Finally, it was observed that tropical hardwoods having more suitable anatomical features, like larger vessel diameter, higher ray width and frequency, and lesser deposits such as gums and tyloses in the vessels, resulted in significantly higher WPGs.