Search Results (28)

The global demand for sustainable energy has accelerated the development of biofuels, aiming to reduce fossil fuel reliance and environmental impact. Second-generation ethanol (2G), produced from lignocellulosic biomass such as sugarcane bagasse and straw, is a promising alternative aligned with the circular economy. Its production relies on pretreatments to improve the enzymatic access to polysaccharides. Among the available methods, the organosolv (O) and hydrothermal (H) pretreatments are effective in separating the biomass into cellulose-rich pulps and hemicellulosic liquors. In this study, these pretreatments were applied to sugarcane bagasse (SCB) and straw (SS), aiming to obtain hemicellulosic fractions for bioconversion. The characterization of pretreated biomasses showed increased cellulose content, indicating successful delignification. After the lignin precipitation, the hemicellulosic liquors were submitted to enzymatic hydrolysis, with increases in the total reducing sugar (TRS) concentrations, from 11.144 to 13.440 g·L⁻¹ (SBO), 16.507 to 22.492 g·L⁻¹ (SBH), 8.560 to 9.478 g·L⁻¹ (SSO), and 14.164 to 22.830 g·L⁻¹ (SSH), with highlights for the hydrothermal pretreated hydrolysates in the improvement of sugar release. HPLC confirmed these gains, notably in the xylose content. The results indicated the potential of hemicellulosic liquors for the fermentation of pentoses, supporting integrated bioethanol production. This approach promotes the efficient use of agro-residues and strengthens the role of biofuels in low-carbon and sustainable energy systems. Full article

Developing efficient, clean, and sustainable lignocellulose pretreatment technologies is essential for second-generation biofuel production. In this study, we attempted to use downstream-separated binary acetone-water, n-butanol-water, and ethanol-water solutions as the initial liquor for upstream organosolv pulping, in order to achieve the efficient and economic closed-circuit clean fractionation of the lignocelluloses for biological acetone–butanol–ethanol (ABE) production. Parameters, including concentration and temperature of the organosolv pulping, were optimized systematically. Results indicated that the 50 wt% ethanol and 30 wt% acetone aqueous solutions and pulping at 200 °C for 1 h exhibited better corn stover fractionation performances with higher fermentable sugar production. The total monosaccharide recovery (including glucose and xylose) was 50.92% and 50.89%, respectively, in subsequent enzymatic saccharification. While pulping corn stover using n-butanol solution as initial liquor showed higher delignification 86.16% (50 wt% of n-butanol and 200 °C for 1 h), the hydrolysate obtained by the organosolv pulps always exhibited good fermentability. A maximized 15.0 g/L of ABE with 0.36 g/g of yield was obtained in Ethanol-200 °C-50% group, corresponding to 112 g of ABE production from 1 kg of raw corn stover. As expected, the lignin specimens fractionated by closed-circuit organosolv pulping exhibited narrow molecule weight distribution, high purity, and high preservation of active groups, which supports further valorization. This novel strategy tightly bridges the upstream and downstream processes of second-generation ABE production, providing a new route for ‘energy-matter intensive’ and environmentally friendly lignocelluloses biorefineries. Full article

A comprehensive techno-economic assessment was undertaken to determine the viability of bioethanol production from sugarcane bagasse in Thailand through organosolv fractionation, incorporating three distinct catalytic systems: sulfuric acid, formic acid, and sodium methoxide. Rigorous process simulations were executed using Aspen Plus, facilitating the derivation of detailed mass and energy balances, which served as the foundational input for downstream cost modeling. Economic performance metrics, including the total annualized cost and minimum ethanol selling price, were systematically quantified for each scenario. Among the evaluated configurations, the formic acid-catalyzed organosolv system exhibited superior techno-economic attributes, achieving the lowest unit production costs of 1.14 USD/L for ethanol and 1.84 USD/kg for lignin, corresponding to an estimated ethanol selling price of approximately 1.14 USD/L. This favorable outcome was attained with only moderate capital intensity, indicating a well-balanced trade-off between operational efficiency and investment burden. Conversely, the sodium methoxide-based process configuration imposed the highest economic burden, with a TAC of 15.27 million USD/year, culminating in a markedly elevated MESP of 5.49 USD/kg (approximately 4.33 USD/L). The sulfuric acid-driven system demonstrated effective delignification performance. Sensitivity analysis revealed that reagent procurement costs exert the greatest impact on TAC variation, highlighting chemical expenditure as the key economic driver. These findings emphasize the critical role of solvent choice, catalytic performance, and process integration in improving the cost-efficiency of lignocellulosic ethanol production. Among the examined options, the formic acid-based organosolv process stands out as the most economically viable for large-scale implementation within Thailand’s bioeconomy. Full article

Research studies for cellulose recovery from lignocellulosic materials are essential in order to propose sustainable alternatives to harness residual biomasses, solving problems caused by their abundance and inadequate use. In this study, olive-tree pruning biomass has been subjected to different pretreatments with different organosolvents (acetone, ethanol, and $\gamma$-valerolactone) with microwave radiation assistance. The effect of operating parameters has been studied, considering specific ranges of variables values according to each experimental design but, in any case, located in the ranges of 33–67% (chemical compound concentration), 130–170 °C (temperature), 5–30 min (reaction time), and 1/20–1/5 (solid/liquid ratio, s/L). Based on the R² and R²_adj values (mostly above 0.97), the experimental data were adequately adjusted to four selected response variables: post-solids cellulose and lignin content apart from removal percentages of both structural components. The optimization process resulted in post-treatment solids with meaningful cellulose yields (higher than 84.7%) and reduced lignin content (lower than 4.2%). The best results were obtained using 66.5% acetone (155 °C, 8.4 min and s/L = 1/19), involving greater material deconstruction, a high percentage of delignification (96.7%), not very significant cellulose loss (29.4%), and a post-treatment solid consisting almost exclusively of cellulose (≈99%). Full article

This study determined the optimal production of furfural (FuR) from liquid hydrolysate xylan liquor obtained through a two-stage pretreatment process using NaOH for de-ashing and EtOH for the delignification of raw rice husk (RH). The de-ashing pretreatment was conducted at 150 °C, with 6.0% (w/v) NaOH and a reaction time of 40 min. The optimal conditions for delignification pretreatment, performed using an organosolv fractionation method with EtOH, were a reaction temperature of 150 °C, 60% (v/v) EtOH, 0.25% (w/v) H₂SO₄, and a reaction time of 90 min. Through a two-stage pretreatment process, a liquid hydrolysate in the form of xylan liquor was obtained, which was subjected to an acid catalytic conversion process to produce FuR. The process conditions were varied, with reaction temperatures of 130–170 °C, H₂SO₄ catalyst concentrations of 1.0–3.0 wt.%, and reaction times of 0–90 min. The Response Surface Methodology tool was used to identify the optimal FuR yield from xylan liquor. Ultimately, the optimal process conditions for the acid catalytic conversion were found to be a substrate-to-catalyst ratio of 2:8, a reaction temperature of 168.9 °C, a catalyst concentration of 1.9 wt.%, and a reaction time of 41.24 min, achieving an FuR yield of 67.31%. Full article

This research explores the potential of agricultural waste, specifically flax straw, as a sustainable raw material for eco-friendly packaging materials. This study investigates a three-stage delignification process involving nitric acid, alkaline treatment, and organosolvent solutions. This method effectively removes lignin from the straw, resulting in high-quality technical pulp with 67.7% α-cellulose and a significantly reduced ash content (8.5%). X-ray diffraction (XRD) and thermogravimetric analysis (TGA) were employed to characterize the treated flax straw. XRD analysis revealed changes in the cellulose structure, while TGA indicated enhanced thermal stability compared to untreated straw. Microscopic analysis of the pulp fibers shows a parallel and aligned arrangement, suggesting a high fiber content and a strong paper lattice. The particle size distribution of the ground pulp, influenced by fiber size, has implications for the packing density and mechanical properties of the final product. This study demonstrates the potential of agricultural waste as a sustainable source for packaging materials, contributing to the circular economy and waste reduction. Full article

Lignocellulosic biomass represents an excellent alternative to fossil fuels in terms of both energy production and raw material usage for a plethora of daily-use products. Organosolv pretreatment is a fractionation technique able to separate lignocellulosic biomass into individual streams of cellulose, hemicellulose, and lignin under controlled conditions. Sawdust, the by-product of sawmill processing of Picea abies wood, was the subject of our investigation in this work. The aim was to evaluate the effects of different parameters of the organosolv process of spruce sawdust on the yield of components and how this affects the enzymatic saccharification of cellulose. Sixteen distinct pretreatments were performed with ethanol concentrations of 50 and 60% v/v at 180 and 200 °C for 15 and 30 min. Half of the pretreatments contained 1% sulfuric acid as a catalyst, while the other half were acid-free. Thereafter, the effects of different variables on the yield of products were assessed and compared to determine the ideal pretreatment condition. The results showed that cellulose-rich pulps, with cellulose content as high as 55% were generated from an initial mass of 37.7% spruce sawdust with the reactor operating at 180 °C for 30 min using 60% ethanol and 1% sulfuric acid. With the pretreatments performed with the catalyst at 200 °C, hemicellulose was almost entirely removed from the pulps obtained. The recovered hemicellulose fraction was composed mainly of monomers achieving up to 10 g/100 g of biomass. Delignification values of up to 65.7% were achieved with this pretreatment technique. Fractionated lignin presented low levels of sugar and ashes contamination, with values as low as 1.29% w/w. Enzymatic saccharification of the pretreated pulps yielded 78% cellulose hydrolysis, with glucose release higher than 0.54 g/g of biomass, indicating the potential of the pulps to be applied in a fermentation process. Full article

Pretreatment is an essential step for breaking the recalcitrant structure of lignocellulosic biomass and allowing conversion to high-value-added chemicals. In this study, coconut fiber was subjected to three pretreatment methods to compare their impacts on the biomass’s structural characteristics and their efficiency in fractionating the biomass. This comparative approach was conducted to identify mild biomass pretreatment conditions that efficiently extract lignin and recover cellulose-rich pulp for the production of bioproducts. To this end, autohydrolysis, alkaline, and organosolv pretreatments were performed under different experimental conditions, and the physicochemical properties of the samples were evaluated using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), and chemical characterization of the cellulose, hemicellulose, and lignin fractions. Therefore, efficient experimental conditions were identified to pretreat coconut fibers with an extended understanding of the methods to process lignocellulose. Great delignification efficiency and pulp yield were obtained with organosolv > alkaline extraction > autohydrolysis under the selected conditions of 2 h at 185 °C in the presence of a catalyst, namely, 0.5 M NaOH, for 2 h at 55 °C and 20 min at 195 °C, respectively. FT-IR revealed a predominance of hydroxyl groups in fibers obtained from alkaline and organosolv pretreatment, showing higher lignin degradation and cellulose concentration in these samples. TGA revealed mass loss curves with similar behaviors but different patterns and intensities, and MVE analysis showed differences on the surfaces of each sample. The comparison of experimental parameters allowed the identification of suitable conditions for each extraction method, and structural analyses identified the specific characteristics of the fibers that could be obtained according to the method used. Therefore, the results are of great importance for developing sustainable and effective industrial processes. Full article

Lignocellulosic biomass (LCB), such as the oil palm empty fruit bunches (OPEFB), has emerged as one of the sustainable alternative renewable bioresources in retrieving valuable bioproducts, such as lignin, cellulose, and hemicellulose. The natural recalcitrance of LCB by the disarray of lignin is overcome through the combinative application of organosolv pre-treatment followed by microwave irradiation, which helps to break down LCB into its respective components. This physicochemical treatment process was conducted to evaluate the effect of ethanol solvent, microwave power, and microwave duration against delignification and the total sugar yield. The highest delignification rate was achieved, and the optimum level of total sugars was obtained, with the smallest amount of lignin left in the OPEFB sample at 0.57% and total sugars at 87.8 mg/L, respectively. This was observed for the OPEFB samples pre-treated with 55 vol% of ethanol subjected to a reaction time of 90 min and a microwave power of 520 W. Microwave irradiation functions were used to increase the temperature of the ethanol organic solvent, which in turn helped to break the protective lignin layer of OPEFB. On the other hand, the surface morphology supported this finding, where OPEFB samples pre-treated with 55 vol% of solvent subjected to similar microwave duration and power were observed to have higher opened and deepened surface structures. Consequently, higher thermal degradation can lead to more lignin being removed in order to expose and extract the total sugars. Therefore, it can be concluded that organosolv pre-treatment in combination with microwave irradiation can serve as a novel integrated method to optimize the total sugar yield synthesized from OPEFB. Full article

Corn cob is an abundant agricultural residue worldwide, with high potential and interesting composition, and its valorization still needs to be studied. Selectively fractionating its structural components (hemicellulose, cellulose, and lignin), value-added products can be produced, eliminating waste. In this work, integrated fractionation approaches were developed and evaluated. First, an organosolv process was optimized (ethanol:water, 50:50, w/w). Then, as a comparative method, alkaline delignification (using NaOH, 1–2%) was also studied. The organosolv process allowed a significant delignification of the material (79% delignification yield) and, at the same time, a liquid phase containing a relevant concentration (14.6 g/L) of xylooligosaccharides (XOS). The resulting solid fraction, rich in cellulose, showed an enzymatic digestibility of 90%. The alkaline process increased the delignification yield to 94%, producing a solid fraction with a cellulose enzymatic digestibility of 83%. The two later techniques were also used in a combined strategy of hydrothermal processing (autohydrolysis) followed by delignification. The first allowed the selective hydrolysis of hemicellulose to produce XOS-rich hydrolysates (26.8 g/L, 67.3 g/100 g initial xylan). The further delignification processes, alkaline or organosolv, led to global delignification yields of 76% and 93%, respectively. The solid residue, enriched in glucan (above 75% for both combined processes), also presented high enzymatic saccharification yields, 89% and 90%, respectively. The fractionation strategies proposed, and the results obtained are very promising, enabling the integrated upgrading of this material into a biorefinery framework. Full article

European aspen (Populus tremula (L.) (Salicaceae)) bark is a promising raw material in multi-step biorefinery schemes due to its wide availability and higher content of secondary metabolites in comparison to stem wood biomass. The main objective of this study was to investigate the major cell wall component-enriched fractions that were obtained from aspen bark residue after extractives isolation, primarily focusing on integration of separated lignin fractions and cellulose-enriched bark residue into complex valorization pathways. The “lignin first” biorefinery approach was applied using mild organosolv delignification. The varying solvent systems and process conditions for optimal delignification of residual aspen bark biomass were studied using a response surface methodology approach. The conditions for maximum process desirability at which the highest amount of lignin-enriched fraction was separated were as follows: 20-h treatment time at 117 °C, butanol/water 4:1 (v/v) solvent system with solid to liquid ratio of 1 to 10. At optimal separation conditions, lignin-enriched fraction exhibited a higher content of β–O–4 linkages vs. C–C linkages content in its structure as well as a high amount of hydroxyl groups, being attractive for its further valorization. At the same time, the content of glucose in products of cellulose-enriched residue hydrolysis was 52.1%, increased from 10.3% in untreated aspen bark. This indicates that this fraction is a promising raw material for obtaining cellulose and fermentable glucose. These results show that mild organosolv delignification of extracted tree bark can be proposed as a novel biorefinery approach for isolation of renewable value-added products with various application potentials. Full article

Bromelia hemisphaerica Lam., a wild plant native to Mexico, has medicinal attributes and is mainly used for its hemisphericin content in foods. However, the residues of its leaves and fruits are underutilized, representing an area of opportunity for foods or materials. Lignocellulosic material from leaves and fruit bagasse was isolated using an organosolv treatment to separate their components (cellulose, hemicellulose and lignin) and to determine the influence after processing on the physicochemical, thermal and microstructural characteristics. The extracted fiber presented a cellulose content of 44% in the leaf and 33.5% in the fruit. The release of lignin after the organosolv process represented a greater amount of amorphous material in the leaf than in the fruit. By FTIR and X-ray diffraction (DRx), the change in the crystallinity of the cellulose was determined (from 18% higher in the leaf than the fruit before to 14% higher in the fruit after the organosolv process), with values similar to type I cellulose. The thermal properties showed a high order in the structure of the cellulose. Microscopy and digital analysis techniques showed the microstructural changes and the effectiveness of delignification during the process. It is concluded that the leaf fiber of B. hemisphaerica presents characteristics that make it useful as a potential ingredient for food product development and other uses. Full article

Olive stones (OS) are a by-product generated in the olive oil production process. This residue is obtained in industries after the oil extraction process, and it is recognized as an interesting feedstock for the production of bioenergy and value-added products. Nevertheless, currently, it is only used as a low-cost solid biofuel for combustion. An alternative valorization approach has been developed based on an acid-catalyzed process for the solubilization of hemicelluloses [¹] and the production of furfural [²]. This process yields a solid cellulose and lignin-rich material, which can be further upgraded. In this work, an organosolv process for the delignification of the material and improvement of the enzymatic digestibility was applied and optimized. The organosolv stage was carried out with an ethanol:water ratio (50:50, w/w) in a Parr reactor, varying the temperature (140–190 °C) and the addition of the catalyst (0–100 mM H₂SO₄). The liquid fraction obtained was analyzed to evaluate the presence of value-added products, such as phenolic compounds with antioxidant activity. The total phenolic content was determined by the Folin–Ciocalteu method, obtaining a phenol concentration between 5 and 13 g GAE/L, corresponding to a phenol yield of 8 g GAE/100 g of processed material, which ranks in the range of those obtained from other plant sources, in other olive by-products such as exhausted olive pomace, up to 9 g GAE/100 g of extract have been reported [³]. The phenolic profile was obtained by capillary electrophoresis analysis, allowing the identification, among others, of vanillin and syringaldehyde as naturally occurring flavor components exhibiting antioxidant and antimicrobial properties. Therefore, with the present study, we were able to determine that the liquor obtained after the organosolv pretreatment of olive stones can also be valued as a bio-source of non-synthetic preservatives and additives for the food industry. Full article

One of the primary targets for the new lignocellulosic feedstock-based biorefinery is the simultaneous valorization of holocellulose and lignin. Acidified organosolv treatment is among the most promising strategy for recovering technical lignin, water-soluble hemicellulose, and cellulose pulp with increased accessibility to hydrolytic enzymes. In this work, a design-of-experiment (DoE) approach was used to increase the cellulose recovery, digestibility, and the delignification of Cynara cardunculus L. feedstock. In the first treatment, the milled biomass was subjected to microwave-assisted extraction using an acidified GVL/water mixture to separate lignin and hemicellulose from cellulose. In the second treatment, the cellulose pulp was hydrolyzed by cellulolytic enzymes to demonstrate the enhanced digestibility. At the optimal condition (154 °C, 2.24% H₂SO₄, and 0.62 GVL/water ratio), the cellulose pulp showed a cellulose content of 87.59%, while the lignin content was lower than 8%. The cellulose recovery and digestibility were equal to 79.46% and 86.94%, respectively. About 40% of the initial hemicellulose was recovered as monosaccharides. This study demonstrated the effectiveness of the two-step organosolv treatment for biomass fractionation; however, as suggested by DoE analysis, a confirmative study at a low temperature (<154 °C) should be performed to further increase the cellulose recovery. Full article

Empty fruit bunch (EFB), which is one of the primary agricultural wastes generated from the palm oil plantation, is generally discharged into the open environment or ends up in landfills. The utilization of this EFB waste for other value-added applications such as activated carbon and biofuels remain low, despite extensive research efforts. One of the reasons is that the EFB is highly vulnerable to microbial and fungi degradation under natural environment owning to its inherent characteristic of high organic matter and moisture content. This can rapidly deteriorate its quality and results in poor performance when processed into other products. However, the lignocellulosic components in degraded EFB (DEFB) still largely remain intact. Consequently, it could become a promising feedstock for production of bio-products after suitable pretreatment with organic solvents. In this study, DEFB was subjected to five different types of organic solvents for the pretreatment, including ethanol, ethylene glycol, 2-propanol, acetic acid and acetone. The effects of temperature and residence time were also investigated during the pretreatment. Organosolv pretreatment in ethylene glycol (50 v/v%) with the addition of NaOH (3 v/v%) as an alkaline catalyst successfully detached 81.5 wt.% hemicellulose and 75.1 wt.% lignin. As high as 90.4 wt.% cellulose was also successfully retrieved at mild temperature (80 °C) and short duration (45 min), while the purity of cellulose in treated DEFB was recorded at 84.3%. High-purity lignin was successfully recovered from the pretreatment liquor by using sulfuric acid for precipitation. The amount of recovered lignin from alkaline ethylene glycol liquor was 74.6% at pH 2.0. The high recovery of cellulose and lignin in DEFB by using organosolv pretreatment rendered it as one of the suitable feedstocks to be applied in downstream biorefinery processes. This can be further investigated in more detailed studies in the future. Full article