Search Results (20)

Biochar activation is achieved by removing tar formed in the pores during the thermal treatment of biomass, thereby increasing pore volume. This process typically involves entraining tar with steam at elevated temperatures for extended durations. In this study, a reduction in lignin content in grape seeds through partial solubilization, prior to thermal treatment, is proposed. Initially, grape seeds were treated with a basic sodium sulfide solution, followed by conditioning with either phosphoric acid or zinc chloride and then drying and calcination. The synthesized adsorbents were characterized using scanning electron microscopy (SEM), textural analysis, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and evaluation of toluene adsorption capacity. Textural analysis indicated that conditioning with phosphoric acid or zinc chloride increased the specific surface area of biochar by over 20%, with a higher increase observed for phosphoric acid treatment. The toluene adsorption capacity of the adsorbents was assessed in a continuous fixed-bed system. Biochar pretreated with ZnCl₂ exhibited an adsorption capacity of 0.11 cm³ of toluene per gram, while biochar pretreated with phosphoric acid demonstrated a capacity of 0.14 cm³ per gram. These results indicate that preliminary delignification of grape seed biomass maintains its adsorption capacity of toluene at levels comparable to other adsorbents, despite a lower activation temperature. Full article

Sustainable construction requires bio-based insulation materials that achieve low thermal conductivity without compromising mechanical performance. Poplar wood, which is locally abundant in France, serves as an effective carbon sink and represents a promising resource. While recent research has explored bulk wood delignification, the characterization of such modified materials remains insufficient for practical implementation. In this work, we report the development of gradient-delignified poplar wood through partial delignification using alcoholysis and sodium chlorite bleaching. This process produced a hybrid structure with delignified outer layers and a lignified core. Microscopic analyses revealed that lignin removal led to cell wall swelling and the formation of nano-scale pores. Compared to native poplar, the modified material showed lower transverse thermal conductivity (0.057 W·m⁻¹·K⁻¹), higher specific heat capacity (1.4 kJ·K⁻¹·kg⁻¹ at 20 °C), increased hygroscopicity, and reduced longitudinal compressive strength (15.9 MPa). The retention of the lignified core preserved dimensional stability and load-bearing capacity, thereby overcoming the limitations of complete delignification. In contrast to synthetic foams or mineral wools, these findings demonstrate that partial delignification can produce anisotropic wood-based insulation materials that combine thermal efficiency, mechanical stability, and biodegradability. This work highlights the potential of wood modification nanotechnology to reduce the carbon footprint of building materials. Full article

The aim of the study was to perform treatment of juniper wood to obtain wood material with a density and mechanical properties comparable to bone, thus producing a potential material for use in osteosynthesis bone implants. In the first step, partial delignification of wood sample was obtained by Kraft cooking. The second step was extraction with ethanol, ethanol–water mixture, saline, and water to prevent the release of soluble compounds and increase biocompatibility. In the last step, the thermal densification at 100 °C for 24 h was implemented. The results obtained in the dry state are equivalent to the properties of bone. The swelling of chemically pre-treated densified wood was reduced compared to chemically untreated densified wood. Samples showed no cytotoxicity by in vitro cell assays. The results of the study showed that it is possible to obtain noncytotoxic wood samples with mechanical properties equivalent to bones by partial delignification, extraction, and densification. However, further research is needed to ensure the material’s shape stability, water resistance, and reduced swelling. Full article

Plant-based waste biomass with lignocellulose as an important component is produced in large quantities worldwide every year. The components of lignocellulose that typically exhibit high utilization value include cellulose and hemicellulose, as well as pentoses and hexoses derived from their hydrolysis. As a pretreatment for the hydrolysis process, delignification is a pivotal step to enhance cellulose/hemicellulose accessibility and achieve high yields of fermentable sugars. Additionally, deep eutectic solvents (DESs) are the most widely used solvents for delignification during biomass fractionation due to their clean and environmentally friendly attributes. DESs dissolve lignin by inducing a large amount of β-O-4 bond cleavage and partial carbon–carbon bond cleavage, retaining cellulose in the solid residue, while most of the hemicellulose is hydrolyzed in DES pretreatment. This article provides a comprehensive review of the influence of DESs in the lignocellulose separation process. Key factors such as lignin removal rate, sugar conversion rate, and product chemical structure are critically reviewed to assess the feasibility of employing DESs for lignocellulose separation. Full article

This study aimed to analyze the production of poly(3-hydroxybutyrate) (PHB) from lignocellulosic biomass through a series of steps, including microwave irradiation, ammonia delignification, enzymatic hydrolysis, and fermentation, using the Bacillus megaterium ATCC 14581 strain. The lignocellulosic biomass was first pretreated using microwave irradiation at different temperatures (180, 200, and 220 °C) for 10, 20, and 30 min. The optimal pretreatment conditions were determined using the central composite design (CCD) and the response surface methodology (RSM). In the second step, the pretreated biomass was subjected to ammonia delignification, followed by enzymatic hydrolysis. The yield obtained for the pretreated and enzymatically hydrolyzed biomass was lower (70.2%) compared to the pretreated, delignified, and enzymatically hydrolyzed biomass (91.4%). These hydrolysates were used as carbon substrates for the synthesis of PHB using Bacillus megaterium ATCC 14581 in batch cultures. Various analytical methods were employed, namely nuclear magnetic resonance (¹H-NMR and¹³C-NMR), electrospray ionization mass spectrometry (EI-MS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and thermogravimetric analysis (TGA), to identify and characterize the extracted PHB. The XRD analysis confirmed the partially crystalline nature of PHB. Full article

Xylan is a macromolecule of industrial interest that can be solubilized from lignocellulosic materials, such as sugarcane bagasse, which is a renewable source. However, the solubilization methods of xylan need to be better developed for use in industrial applications. The main objective of this study was to evaluate xylan solubilization methods with higher yields and purity by using biomasses/fractions of sugarcane: leaf and stem, internode, node, and external fraction. Two strategies were evaluated by applying diluted sodium chlorite, sodium sulfite, and hydrogen peroxide: a delignification of the biomass before xylan solubilization; and the delignification of the solubilized xylan for residual lignin removal. The delignification of the biomass before the xylan solubilization enabled to identify material and specific conditions for yields higher than 90%. Residual lignin varied from 3.14 to 18.06%, with hydrogen peroxide in alkaline medium partial delignification shown to be effective. The delignification of xylan presented better results using diluted hydrogen peroxide, with a reduction of 58.44% of the initial lignin content. The solubilized xylans were used as a substrate for xylanase activities, resulting in higher activity than commercial xylan. In the delignification of the biomasses, hydrogen peroxide was the reagent with better results concerning the yield, purity, and solubility of the xylan. This reagent (diluted) was also better in the delignification of the solubilized xylan, resulting in lower residual lignin content. The solubility and purity tests (low salt content) indicated that the solubilized xylan presented characteristics that were similar to or even better than commercial xylan. Full article

Arundo donax L samples, before or after aqueous extraction to remove extractives, were subjected to chemical fractionation in H₂SO₄-catalyzed mixtures of 1-butanol and water. The partial miscibility of 1-butanol and water at room temperature allowed the separation of the three major feedstock components in separate streams (lignin, accumulated in the 1-butanol-rich phase; hemicellulose-derived products, accumulated in the aqueous acidic phase; and cellulose, present in the solid phase). The effects of selected variables (temperature, catalyst concentration, reaction time and 1-butanol content of the reaction media) on variables measuring the solid recovery yield and the compositions of phases from fractionation were measured. Using water-extracted A. donax L as a substrate, the best operational conditions enabled 93.2% hemicellulose removal and 85.4% delignification with limited cellulose solubilization (15%). The experimental results provided key information to assess the proposed process in the scope of biorefineries. Full article

Lignocelluloytic enzymes are industrially applied as biocatalysts for the deconstruction of recalcitrant plant biomass. To study their biocatalytic and physiological function, the assessment of their binding behavior and spatial distribution on lignocellulosic material is a crucial prerequisite. In this study, selected hydrolases and oxidoreductases from the white rot fungus Phanerochaete chrysosporium were localized on model substrates as well as poplar wood by confocal laser scanning microscopy. Two different detection approaches were investigated: direct tagging of the enzymes and tagging specific antibodies generated against the enzymes. Site-directed mutagenesis was employed to introduce a single surface-exposed cysteine residue for the maleimide site-specific conjugation. Specific polyclonal antibodies were produced against the enzymes and were labeled using N-hydroxysuccinimide (NHS) ester as a cross-linker. Both methods allowed the visualization of cell wall-bound enzymes but showed slightly different fluorescent yields. Using native poplar thin sections, we identified the innermost secondary cell wall layer as the preferential attack point for cellulose-degrading enzymes. Alkali pretreatment resulted in a partial delignification and promoted substrate accessibility and enzyme binding. The methods presented in this study are suitable for the visualization of enzymes during catalytic biomass degradation and can be further exploited for interaction studies of lignocellulolytic enzymes in biorefineries. Full article

There is increasing interest in furfurylated wood, but the polymerization mechanism between its internal polyfurfuryl alcohol (PFA) and lignin is still uncertain. This paper investigated the distribution of PFA and the feasibility of the polymerization of PFA with lignin in furfurylated balsa wood. The wood first immersed in the furfuryl alcohol (FA) solution followed by in situ polymerization and the distribution of PFA was characterized by Raman, fluorescence microscopy, SEM, and CLSM. Then, the mill wood lignin (MWL) of balsa wood and lignin model molecules were catalytically polymerized with PFA, respectively, studying the mechanism of interaction between PFA and lignin. It was concluded that PFA was mainly deposited in cell corner with high lignin concentration, and additionally partly deposited in wood cell cavity due to high concentration of FA and partial delignification. TGA, FTIR, and NMR analysis showed that the cross-linked network structure generated by the substitution of MWL aromatic ring free position by PFA hydroxymethyl enhanced the thermal stability. New chemical shifts were established between PFA and C₅/C₆ of lignin model A and C₂/C₆ of model B, respectively. The above results illustrated that lignin-CH₂-PFA linkage was created between PFA and lignin in the wood cell wall. Full article

Wood is an attractive and inherently sustainable alternative to many conventional materials. Recent research on improving wood mechanical strength emphasizes wood densification through the partial removal of lignin and hemicelluloses, therefore the chemical and physical properties of delignified and densified wood require further investigation. In this study, poplar wood samples were subjected to alkali and maleic acid hydrotropic delignification with varying degrees of lignin and hemicellulose removal followed by hot pressing, and the microstructure, chemical properties, and dimensional stability of densified wood through delignification were evaluated. The results showed that the complete wood cell collapse was observed near the surface of all the delignified wood blocks, as well as some micro-cracks in the cell walls. The chemical analysis indicated that delignification occurred mainly near the surface of the wood blocks and enhanced hydrogen bonding among the aligned cellulose fibers. For dimensional stability, the set recovery decreased with the increase in alkali dosage, and the considerable fixation of compressive deformation was obtained by a post-densification hydrothermal treatment at 180 °C. These results have demonstrated that the densified wood with delignification can be easily fabricated using the proposed method, and the densified wood exhibited great potential to be used as a sustainable material. Full article

This study aimed to evaluate the effect of ammonium persulfate’s (APS) oxidation time on the characteristics of the cellulose nanocrystals (CNCs) of balsa and kapok fibers after delignification pretreatment with sodium chlorite/acetic acid. This two-step method is important for increasing the zeta potential value and achieving higher thermal stability. The fibers were partially delignified using acidified sodium chlorite for four cycles, followed by APS oxidation at 60 °C for 8, 12, and 16 h. The isolated CNCs with a rod-like structure showed an average diameter in the range of 5.5–12.6 nm and an aspect ratio of 14.7–28.2. Increasing the reaction time resulted in a gradual reduction in the CNC dimensions. The higher surface charge of the balsa and kapok CNCs was observed at a longer oxidation time. The CNCs prepared from kapok had the highest colloid stability after oxidation for 16 h (−62.27 mV). The CNCs with higher crystallinity had longer oxidation times. Thermogravimetric analysis revealed that the CNCs with a higher thermal stability had longer oxidation times. All of the parameters were influenced by the oxidation time. This study indicates that APS oxidation for 8–16 h can produce CNCs from delignified balsa and kapok with satisfactory zeta potential values and thermal stabilities. Full article

Residual biomass from agri-food production chain and forestry are available in huge amounts for further valorisation processes. Delignification is usually the crucial step in the production of biofuels by fermentation as well as in the conversion of cellulose into high added-value compounds. High-intensity ultrasound (US) and hydrodynamic cavitation (HC) have been widely exploited as effective pretreatment techniques for biomass conversion and in particular for cellulose recovery. Due to their peculiar mechanisms, cavitational treatments promote an effective lignocellulosic matrix dismantling with delignification at low temperature (35–50 °C). Cavitation also promotes cellulose decrystallization due to a partial depolymerization. The aim of this review is to highlight recent advances in US and HC-assisted delignification and further cellulose recovery and valorisation. Full article

In this work, sugarcane bagasse fiber, a waste product of agroindustry, was added to mortar mixes at different proportions looking to seal porosities so as to improve the resistance of concrete to carbonation and to improve its mechanical properties. To evaluate the behavior of bagasse fibers in the alkaline media typical of mortars, bagasse fibers were subjected to solutions with alkaline pH values, and their chemical structure and morphological behavior was evaluated using FTIR (Fourier transform infrared spectroscopy) and SEM (Scanning Electron Microscopy). Using mortar cylinders in an accelerated carbonation chamber to obtain results in short lapses, the compressive strength and the carbonation were evaluated. The FTIR analysis results indicate that pH values of 11 and 12 causes a delignification, while at pH 9 and 10, a swelling of the molecule occurs because of the addition of hydroxyl ions, behavior that is confirmed with SEM images. A clear effect of the fiber addition on the performance of concrete was observed as the carbonation front of 35 mm for the sample without fibers was reduced to 2 mm for the sample with 2% fiber addition, resulting in an increase of 5 MPa in compressive strength. These results indicate that in the range of mortar pH, chemical changes occured over the sugarcane surface that could cause the growth of fibers and could partially seal the porosity in the mortars, thus enhancing its performance. Full article

Partial delignification and densification provide a pathway to significant improvement in the mechanical performance of wood. In order to elucidate potential effects of this treatment on the mechanical anisotropy of wood, partially delignified and densified spruce wood veneers were characterized at varying degrees of off-axis alignment. While the tensile strength and the modulus of elasticity (MOE) were clearly improved in parallel to the axis of wood fibers, this improvement quickly leveled off at misalignment angles ≥30°. For transverse tensile strength, the performance of alkaline-treated and densified wood was even inferior to that of untreated wood. Microscopic examination revealed the presence of microscopic cracks in treated wood, which are assumed to be responsible for this observation. It is concluded that impaired transverse tensile properties are a weakness of partially delignified and densified wood and should be considered when a potential usage in load-bearing applications is intended. Full article

Hazelnut shells are an important waste from the hazelnut processing industry that could be valorized in a multi-product biorefinery. Individual or combined pretreatments may be integrated in processes enabling the integral fractionation of biomass. In this study, fractionation methods based on alkaline, alkaline-organosolv, organosolv, or acid-catalyzed organosolv treatments were applied to raw or autohydrolyzed hazelnut shells. A comparative analysis of results confirmed that the highest lignin removal was achieved with the acid-catalyzed organosolv delignification, which also allowed limited cellulose losses. When this treatment was applied to raw hazelnut shells, 65.3% of the lignin was removed, valuable hemicellulose-derived products were obtained, and the cellulose content of the processed solids increased up to 54%. Autohydrolysis of hazelnut shells resulted in the partial solubilization of hemicelluloses (mainly in the form of soluble oligosaccharides). Consecutive stages of autohydrolysis and acid-catalyzed organosolv delignification resulted in 47.9% lignin removal, yielding solids of increased cellulose content (55.4%) and very low content of residual hemicelluloses. The suitability of selected delignified and autohydrolyzed-delignified hazelnut shells as substrates for enzymatic hydrolysis was assessed in additional experiments. The most susceptible substrates (from acid-catalyzed organosolv treatments) reached 74.2% cellulose conversion into glucose, with a concentration of 28.52 g glucose/L. Full article