Acid Pretreatment Research Articles

Yeast based biorefinery for xylitol and ethanol production from sugarcane bagasse

Lignocellulosic biomass is one of the biggest renewable reservoirs for organic carbon that can be exploited as feed for various value-added products like fuel, nutraceuticals enzymes, and proteins. Biofuel is not only valuable but also a top priority target to address the energy crisis. Hence the current work was planned to valorize the cellulose-rich residual biomass (CRB), left after xylitol production for ethanol fermentation by yeast. Xylose-rich hydrolysate was prepared with dilute acid pretreatment (0.1 M H2SO4, 145 ℃, and 90 min) for xylitol production and CRB was further processed for enzymatic hydrolysis (crude cellulase). Acid hydrolysis offered maximum reducing sugars of 0.33±0.01 g⋅g−1biomass comprised of xylose 0.31±0.01 g⋅g−1biomass. Besides sugar, biomass hydrolysis also produced 0.21 ±0.01 g.L−1 furans and 0.34±0.11 g.L−1 acetic acid. Pichia guilliermondii RLV-04 (MH588234.1) have shown 0.90±0.02 gxylitol.g−1xylose conversion of xylose to xylitol. The primary process has left more than 50–55 % biomass that was rich in cellulose. Enzymatic hydrolysis of the CRB using crude cellulase showed maximum glucose recovery of 0.56±0.02 g⋅g−1available cellulose at 15 FPU at 50 ℃, after 12 h. In addition, yeast biomass recovered from xylitol production was hydrolysed and used as a nitrogen source. Under an anaerobic environment, a maximum ethanol yield of 0.36±0.01 g.g−1glucose was achieved with commercial baker’s yeast while the addition of yeast biomass hydrolysate improved the alcohol yield to 0.48±0.02 g.g−1glucose. Reutilization of biocatalysts as nitrogen source not only upgraded fermentation processes but also lowered process waste and improved process economics.

Life cycle analysis of apple pomace biorefining for biofuel and pectin production

This study investigated the environmental impacts associated with converting apple pomace, a globally abundant resource, into biofuels and high-value products using a comparative consequential life cycle assessment. In three developed scenarios, an acid pretreatment method was applied and the pretreated liquid was used for ethanol and pectin production. The pretreated solids were utilized to produce different products: scenario 1 produced biogas, scenario 2 generated butanol, and scenario 3 yielded both biogas and butanol from the solids. The results demonstrated that scenario 1 exhibited the best performance compared to the other two scenarios, imposing the lowest environmental burdens across all damage categories, including human health, ecosystems, and resources. Despite the induced impacts, the benefits of avoided products, i.e., ethanol, natural gas, butanol, acetone, and pectin, compensated for these induced environmental impacts to some extent. The results also revealed that among all products generated through the biorefineries, first-generation ethanol substitution had the most significant positive environmental impacts. Overall, the biorefinery developed in scenario 1 represents the most feasible strategy for a circular bioeconomy. It performs 84.38 % and 72.98 % better than scenarios 2 and 3 in terms of human health, 85.34 % and 74.54 % better in terms of ecosystems, and more than 100 % better in terms of resources. Conversely, scenario 2 resulted in the highest net impacts across all damage categories. Furthermore, in scenario 1, the midpoint results showed 83.10 % and 71.08 % lower impacts on global warming, 85.15 % and 74.17 % lower impacts on terrestrial acidification, and 99.26 % and 98.53 % lower impacts on fossil resource scarcity compared to scenarios 2 and 3, respectively. In conclusion, the first scenario shows promise for the sustainable valorization of apple pomace.

Consolidated bioprocessing of lignocellulosic wastes in Northwest China for D-glucaric acid production by an artificial microbial consortium.

D-glucaric acid is a platform chemical of great importance and the consolidated bioprocessing (CBP) of lignocellulose by the microbial consortium of Trichoderma reesei C10 and Saccharomyces cerevisiae LGA-1C3S2 features prospects in biomanufacturing it. Here we compared some representative lignocelluloses in Northwest China including corn stover, wheat straw and switchgrass, and the leading pretreatments including steam explosion, subcritical water pretreatment, sodium hydroxide pretreatment, aqueous ammonia pretreatment, lime pretreatment, and diluted sulfuric acid pretreatment. It was found that sodium hydroxide pretreated switchgrass (SHPSG) was the best substrate for D-glucaric acid production, resulting in the highest D-glucaric acid titers, 11.69 ± 0.73g/L in shake flask and 15.71 ± 0.80g/L in 10L airlift fermenter, respectively. To the best of our knowledge, this is the highest D-glucaric acid production titer from lignocellulosic biomass. This work offers a paradigm of producing low-cost D-glucaric acid for low-carbon polyethylene 2,5-furandicarboxylate (PEF) and a reference on developing biorefinery in Northwest China.

Current status and future prospects of pretreatment for tobacco stalk lignocellulose.

With the growing demand for sustainable development, tobacco stalks, as a resource-rich and low-cost renewable resource, hold the potential for producing high-value chemicals and materials within a circular economy. Due to the complex and unique structure of tobacco stalk biomass, traditional methods are ineffective in its utilization, making the pretreatment of tobacco stalk lignocellulose a crucial step in obtaining high-value products. This paper reviews recent advancements in various pretreatment technologies for tobacco stalk lignocellulosic biomass, including hydrothermal, steam explosion, acid, alkaline, organic solvent, ionic liquid, and deep eutectic solvent pretreatment. It emphasizes the impact and efficiency of these pretreatment methods on the conversion of tobacco stalk biomass and discusses the advantages and disadvantages of each technique. Finally, the paper forecasts future research directions in the pretreatment of tobacco stalk lignocellulose, providing new insights and methods for enhancing its efficient utilization.

Integrated approach for co-production of bioethanol and light aromatics from lignocellulose through polyethylene glycol-aided acidic glycerol pretreatment

Acid-catalyzed glycerol organosolv (GO) pretreatment is a promising method for lignocellulosic biomass (LCB) fractionation. However, this method often leads to lignin repolymerization, intensifying lignin's inhibitory effects on subsequent enzymatic hydrolysis and limiting the production of highly active lignin, thereby hindering its valorization. This study explored incorporating polyethylene glycol (PEG) into acidic-catalyzed GO to improve bioethanol and bio-oil yields, with a focus on improving the yield of light aromatics, from LCB. Optimized PEG-aided GO pretreatment achieved a significantly higher bioethanol yield (23.7 g/L) compared to GO (17 g/L) and dilute acid (DA: 11.3 g/L) pretreatments. This improvement is attributed to the ability of PEG to mitigate lignin inhibition and modify the physicochemical properties of the pretreated substrate. Furthermore, thermal pyrolysis of PEG-aided GO lignin, obtained after the fermentation process, resulted in a substantially increased bio-oil yield (45.5 %) compared to GO (19 %) and DA (12 %). The enhanced bio-oil yield from PEG-aided GO lignin is ascribed to the promotion of β-O-4 linkages and the formation of β-O-4′ linkages. Characterization of the pyrolysis bio-oil revealed that light aromatic compounds were the dominant fraction, with their relative abundance significantly increasing from DA (5.9 %) to GO (9.7 %) and PEG-aided GO lignin (24.9 %). The PEG-aided GO method achieved an energy output of 8.85 MJ/kg, exceeding that of the GO and DA methods by 31 % and 57 %, respectively. The energy conversion efficiency of the PEG-aided GO method was 70 %, demonstrating a significant improvement compared to GO (57 %) and DA (51 %). This approach promotes the circular economy by upcycling LCB for bioethanol and valuable light aromatic compound production.

Enhancing detoxification of inhibitors in lignocellulosic pretreatment wastewater by bacterial Action: A pathway to improved biomass utilization

The process of preprocessing techniques such as acid and alkali pretreatment in lignocellulosic industry generates substantial solid residues and lignocellulosic pretreatment wastewater (LPW) containing glucose, xylose and toxic byproducts. In this study, furfural and vanillin were selected as model toxic byproducts. Kurthia huakuii as potential strain could tolerate to high concentrations of inhibitors. The results indicated that vanillin exhibited a higher inhibitory effect on K. huakuii (3.95 % inhibition rate at 1 g/L than furfural (0.45 %). However, 0.5 g/L vanillin promoted the bacterial growth (−2.35 % inhibition rate). Interestingly, the combination of furfural and vanillin exhibited antagonistic effects on bacterial growth (Q<0.85). Furfural and vanillin could be bio-transformed into less toxic molecules (furfuryl alcohol, furoic acid, vanillyl alcohol, and vanillic acid) by K. huakuii, and inhibitor degradation rate could be promoted by expression of antioxidant enzymes. This study provides important insights into how bacteria detoxify inhibitors in LPW, potentially enhancing resource utilization.

Effects of Acid Pre-Treatment on Removal of Organic and Inorganic Substances from Black Tilapia Bones and Scales

Fish bones and scales are good sources of gelatin. However, high mineral content in bones and scales often lead to low quality gelatin with high percentage of ash. Therefore, pre-treatment with acid prior to gelatin extraction is necessary. Black tilapia (Oreochromis niloticus) bones and scales were subjected to Hydrochloric (HCl) acid of 0.6 M to 1.4 M for 0 to 32 hr. The suitable pre-treatment conditions were determined using percentage of ash removed and loss of protein from the samples. Results obtained indicate, 99.86 % and 99.84 % of ash can be removed from bones and scales, with 1.4 M HCl (32 hr) and 1.0 M HCl (10 hr), respectively. Further analysis with UV-Vis revealed that, excessive protein breakdown starts to occur at 1.0 M (32 hr) and 0.6 M (12 hr), in bones and scales, respectively. The data suggest using pre-treatment conditions lower than the above to avoid protein loss which may lead to low gelatin yield.

Combined pretreatment of malic acid and kraft pulping for the production of fermentable sugars and highly active lignin

The separation and utilization of cellulose, hemicellulose, and lignin in lignocellulosic biorefineries present significant challenges. This study proposes a pretreatment method for biomass refining by combining acid and kraft pulping. Firstly, the biomass was pretreated by malic acid, resulting in the isolation of xylo-oligosaccharides (XOS) with a yield of 86.26 % with optimized conditions of 180 °C, 1 wt% concentration, 40 min. Secondly, a mixture of 12.98 wt% NaOH and 1.043 wt% Na2S is employed to achieve lignin removal efficiency up to 63.42 %. Physical refinement techniques are then applied to enhance the enzyme digestion efficiency of cellulose, resulting in an increase from 55.03 % to 91.4 % for efficient cellulose conversion. The reacted samples exhibit a lignin composition rich in β-O-4 ether bonds, facilitating their high-value utilization. The results indicated that the combined pretreatment approach demonstrates high efficiency in separating cellulose, hemicellulose, and lignin while obtaining XOS, highly active lignin, and enzyme-digested substrates.

Evaluation of Organic Acids and Ultrasound as Pretreatment in Convective Drying Kinetics and Quality Parameters of Pumpkin.

There is a growing interest in the food industry in new drying technologies that reduce the time required for dehydration, combined with low energy consumption, low environmental impact, and maintenance of the overall quality of the product. This work investigated convective drying of pumpkin with and without ultrasound-organic (citric or acetic) acid pretreatment for different durations (10, 20, and 30 min). Drying was carried out at 60 °C, and the Wang and Singh model had the best fit for the experimental data. Samples pretreated for 30 min had the shortest drying times. Water diffusivities ranged from 6.68 × 10-8 m2/s to 7.31 × 10-8 m2/s, with the pretreated samples presenting the highest values. The dried pumpkin water activity values were below 0.60. Regarding color parameters, there was a slight increase in luminosity, a slight reduction in a*, and a significant increase in b*. Drying resulted in the loss of ascorbic acid and phenolic compounds, but the samples pretreated with citric acid showed better retention. There was also a reduction in the total carotenoid content, but samples pretreated with acetic acid for 10 and 20 min showed the best retention.

Efficient Production of Fermentable Sugars from Common Reed Biomass Through Hydrothermal and Citric Acid Pretreatment Processes

Efficient Production of Fermentable Sugars from Common Reed Biomass Through Hydrothermal and Citric Acid Pretreatment Processes

Physicochemical and functional properties of buffalo (Bubalus bubalis) bone gelatin extracted using acid pre-treatment

This study explored the effects of pre-treatment conditions using hydrochloric acid and citric acid at concentrations of 0.025 M and 0.05 M, on the properties and extractability of gelatin sourced from buffalo bone. The highest yield (6.36 %) and hydroxyproline content (26.98 g/100 g) were obtained from gelatin extracted using 0.025 M HCl pre-treatment (H-1). In comparison, pre-treatment with 0.05 M citric acid (C-2) resulted in the lowest yield (3.79 %) with hydroxyproline content of 12.49 g/100 g. Buffalo bone gelatin had considerably lower moisture content ranging from 7.54 % to 11.92 % than standard bovine gelatin (SBG) (10.91 %) and a pH range of 5.31 to 5.44, indicating it is Type A gelatin. The gelatin that subjected to the pre-treatment by 0.025 M citric acid (C-1) illustrated the highest values for emulsion activity index (EAI), emulsion stability index (ESI), foaming expansion (FE), foaming stability (FS), water holding capacity (WHC), and fat binding capacity (FBC). Fourier Transform Infrared Spectroscopy (FTIR) results indicated a similar secondary structure to SBG explained by the presence of Amide A, B, I, II and III components. Apparent peptides at the α and β regions were observed in the buffalo bone gelatin. Buffalo bone gelatin shows potential as an alternative source of halal gelatin manufacturing.

Comparison of acid and hydrothermal pretreatments of date waste for value creation

The production of date syrup yields a substantial amount of date press cake (DPC), fibrous and moisturising material with great potential for generating value through bioprocessing. However, the recalcitrant structure of DPC affects the yield of products in bioprocesses. To boost the accessibility of the structure as well as increase the soluble fraction of carbohydrates and facilitate further enzymatic hydrolysis, hydrothermal and dilute acid (0.5% (v/v) sulfuric acid) pretreatments as cost-effective and feasible methods were applied on DPC at relatively low temperatures (80, 100, 120 and 140 °C) and reaction times (60 and 90 min). The success in pretreatment was then evaluated by a post-enzymatic treatment using an enzyme cocktail of cellulases and hemicelluloses. Based on total accessible sugar with minimum produced inhibitors, an optimal operating condition was considered acid pretreatment at 120 °C for 90 min with a 55.02% increase in total sugar yield. To explore the potential use of pretreated DPC, an anaerobic digestion was conducted on untreated and acid-pretreated DPC at 120 °C for 90 min. The results showed that pretreatment increased the total bioproduct yield, including hydrogen, ethanol, and volatile fatty acid yields, by 59.75%. This demonstrates the significant impact of pretreatment on product yields in a bioprocess.

High-efficiency conversion of corn bran to ethanol at 150 L scale

Fractionated corn bran was processed to maximize ethanol production from starch, cellulose, and xylan. After various bench-scale experiments, an optimized process with dilute acid pretreatment (1.5 % w/w H2SO4) at 90 °C for 60 min was utilized followed by enzymatic hydrolysis using cellulase and hemicellulase for 48 hr. After simultaneous saccharification (regarding starch) and fermentation at 150 L using an engineered yeast, which consumes both glucose and xylose to make ethanol, the 86 % total sugar conversion yield was achieved, including conversions of 95 % for starch, 77 % for cellulose and 77 % for xylan. Also, an accurate mass balance was formulated for ethanol-producing carbohydrates including starch, cellulose, and xylan from feedstock to final ethanol. A highly efficient process of converting corn fiber to ethanol was successfully scaled up to 150 L.

Supercritical CO2 as effective wheat straw pretreatment for subsequent mild fractionation strategies

The efficient utilization of lignocellulosic biomass in biorefineries is pivotal for the transition to a carbon–neutral society, emphasizing the need for environmentally friendly fractionation techniques. While the extensive use of chemicals in biorefinery operations can yield favorable quantities of specific biomass components, adopting less chemically intense conditions is crucial for holistic methodologies that preserve the inherent potential of all biomass constituents. This study comprehensively investigates the use of supercritical carbon dioxide (sc-CO2) as a green pretreatment to improve subsequent mild fractionation on wheat straw. Sc-CO2 at 300 bars, 100 °C and 70% moisture was found to have minimal impact on the chemical composition and the lignin structure, while there were significant morphological changes as heightened surface area and reduced density. Apart from increasing enzymatic saccharification efficiency, the treatment notably enhanced subsequent mild delignification through alkaline and flow-through organosolv extractions. The combination of the pretreatments enhances the lignin solubilization yields from 49 to 79% for alkaline and 74 to 91% for organosolv extractions, while retaining a high β-O-4 conservation of 49 and 59 linkages per 100 aromatic units, respectively. Additionally, the combined use of sc-CO2 with mild dilute acid pretreatment improved xylose solubilization from 59 to 76 % and enzymatic saccharification from 53 to 90%, albeit with increased lignin condensation. In summary, this study demonstrates the potential of sc-CO2 pretreatment as a versatile tool for biomass valorization within the evolving bioeconomy, by combining enhanced extraction yields with minimal lignin structural impact. Our work thereby highlights the promise of the use of sc-CO2 to contribute to the overall economic potential of improved biorefinery processes.

Porous red mud ceramsite for aquatic phosphorus removal: Application in constructed wetlands

Red mud (RM) and spent oyster mushroom substrate (SOMS), by-products of industrial and agricultural production, can be recycled for polluted freshwater purification, bringing about a win-win situation. In this study, unacidified RM and RM acidified with oxalic acid (O-RM) and hydrochloric acid (H-RM), respectively, were mixed with SOMS to produce a porous ceramsite as a potential constructed wetlands (CWs) substrate. The results showed that the O-RM, H-RM, and RM ceramsites displayed fine compressive strengths of 7.75 ± 1.14, 8.40 ± 1.30, and 8.84 ± 0.69 MPa after calcining at 950 °C for 30 min, respectively. The phosphorus adsorption capacities of H-RM, O-RM, and RM ceramsite at a solid-liquid ratio of 25 g/L were 1.18 mg/g, 0.88 mg/g, and 1.06 mg/g, respectively. Toxicity release experiments showed that the ceramsites did not cause secondary environmental pollution, except for arsenic (ranging from 0.210 to 0.238 mg/L). The H-RM ceramsite was tested in a tidal flow-vertical flow CW (TF-VFCW) with Iris pseudacorus L. and Canna indica L plants. In the TF-VFCW, the average chemical oxygen demand (COD), ammonia nitrogen (NH4+-N), total nitrogen (TN), and total phosphorus (TP) removal rates were 81.01, 90.25, 66.90, and 77.32 %, respectively. Plant growth had less impact on COD and NH4-N removal but had greater limited TN and TP removal. Scanning electron microscopy, Fourier-transform infrared spectroscopy, and X-ray diffraction analysis confirmed that acid pretreatment and the incorporation of SOMS significantly increased the surface and interior porous structures of the ceramsite and enhanced phosphate adsorption by the polyhydroxyl aluminum-iron complex ions. Bacteroides and Campylobacter used the energy produced during polyhydroxyalkanoic acid (PHA) catabolism to absorb phosphorus. Therefore, the synergistic effect of the substrate, plants, and microorganisms achieved the removal of phosphorus from CWs and offered effective and environmentally friendly recycling of RM and SOMS.

Enhanced Cellulose Content in Microwave-Assisted Sulfuric Acid Pretreatment of Java Grass

This study investigated the enhancement of cellulose content in Java grass (Cyperus rotundus) through microwave-assisted sulfuric acid pretreatment. The research involved soaking Java grass in varying concentrations of H2SO4 (1.5%, 3%, and 4.5%) and subjecting it to microwave irradiation at 2450 MHz for different durations (25, 35, and 45 minutes). The results showed that the highest cellulose content of 43.61% was achieved with a 1.5% H2SO4 solution for 45 minutes, representing a 90.3% increase from the pre-treatment level of 22.91%. The microwave-assisted pretreatment effectively disrupted the lignocellulosic structure, reduced cellulose crystallinity, and increased biomass surface area, thereby enhancing enzymatic hydrolysis. However, an anomaly was observed in the lignin content, which increased from 14.3% to 36.65% post-treatment, likely due to errors in lignin determination and the formation of pseudo-lignin.

Comparative analysis of bioenergy and mycoprotein production from apple pomace: Strategies for enhancement and environmental benefits

Apple pomace constitutes a major waste stream of the food processing industry that is characterized by high concentrations of free sugars and structural carbohydrates. This study comparatively explored alternative apple pomace valorization strategies. To this regard, the integration of hydrothermal and organic acid pretreatment as a strategy to enhance anaerobic digestion biomethane yield and alternative production of mycoprotein as a valuable secondary product via the use of Aspergillus oryzae and Neurospora intermedia edible fungi were investigated. In scenario 1, both pretreatment liquors and solid residues underwent anaerobic digestion to produce biomethane. In scenario 2, pretreatment liquors and solid residues underwent fungal cultivation and anaerobic digestion, respectively. Additionally, to optimize bioenergy yield and minimize wastewater generation in scenario 2, the fungal growth effluent was also subjected to anaerobic digestion. In scenario 1, employing methane for transportation showed the potential to decrease GHG by 314.8 kt CO2 eq, translating to US$72.4 million in social cost savings. Similarly, in scenario 2, replacing edible fungal biomass in the food market could lead to a substantial reduction in emissions by 824.2 kt CO2 eq and a corresponding US$227.0 million in social cost savings.

Effect of calcium chloride blanching combined with acetic acid soaking pretreatment on oil absorption of fried potato chips

This study investigated the effect of calcium chloride (CaCl2) combined with acetic acid (AA) pretreatment on the oil absorption of potato chips and explored the possible mechanisms influencing oil absorption. Results indicated that compared with hot water blanching, the combination of 0.3% CaCl2 blanching and AA soaking for 2–8 h pretreatment was found to reduce oil content by 10.52%–12.68% and significantly improve the crispness and color of fried potato chips. Microstructural and textural analyses revealed that the main reason for the reduction in oil content was the promotion of pectin gelation in the cell wall by CaCl2 and AA. However, it was observed that prolonged AA soaking time and high-concentration CaCl2 blanching led to an increase in total oil content and decrease in brittleness. Based on the results of surface roughness and moisture content analyses, it was suggested that the CaCl2 and AA pretreatments affected surface roughness and moisture content, thereby increasing oil absorption and reducing brittleness during frying.

Enhancing phenolic and lipid compound production in oat bran via acid pretreatment and solid-state fermentation with Aspergillus niger

Oat (Avena sativa) processing generates a large amount of by-products, especially oat bran. These by-products are excellent sources of bioactive compounds such as polyphenols and essential fatty acids. Therefore, enhancing the extraction of these bioactive substances and incorporating them into the human diet is critical. This study investigates the effect of acid pretreatment on the solid-state fermentation of oat bran with Aspergillus niger, with an emphasis on the bioaccessibility of phenolic acids and lipid profile. The results showed a considerable increase in reducing sugars following acid pretreatment. On the sixth day, there was a notable increase in the total phenolic content, reaching 58.114 ± 0.09 mg GAE/g DW, and the vanillic acid level significantly rose to 77.419 ± 0.27 μg/g DW. The lipid profile study revealed changes ranging from 4.66 % in the control to 7.33 % on the sixth day of SSF. Aside from biochemical alterations, antioxidant activity measurement using the DPPH technique demonstrated the maximum scavenging activity on day 4 (83.33 %). This study highlights acid pretreatment's role in enhancing bioactive compound accessibility in solid-state fermentation and its importance for functional food development.

OPTIMIZATION OF DILUTE SULPHURIC ACID PRETREATMENT OF COTTON STALK THROUGH BOX BEHNKEN DESIGN OF RESPONSE SURFACE METHODOLOGY

The purpose of the current study was to use diluted sulfuric acid to optimize the pretreatment conditions for cotton stalk. Different quantities (w/v) of cotton stalk (5%, 10%, 15%) were pretreated with different concentrations of H2SO4 (0.6%, 0.8%, 1%) for 4, 6 and 8 hours to degrade the crystalline structure of cellulose and to facilitate the hydrolysis of the cellulosic component. Dilute acidic pretreatment was also conducted in steam conditions at 121 °C, 15 psi. A statistical model was created using a three-level Box Behnken design (BBD) to optimize the process variables. Maximum results regarding cellulose exposure (85%) were recorded with 15% substrate loading, 0.8% acid concentration and time period of 8 hours followed by steam. Maximum total phenolic compounds (8.17 mg/mL) were observed under the same conditions, except steam. The effectiveness of the pretreatment was also analyzed by FTIR and XRD techniques. The results were analysed using ANOVA with a second order polynomial equation. The P value 0.05 showed the significance of the model. The pretreatment conditions that allowed obtaining maximum cellulose content can be used for enzymatic hydrolysis to produce maximum sugars.