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Cotton stalks (CS) are lignocellulosic agricultural by-products, a potential source for biogas production, but pretreatment must be considered since hydrolysis is the rate-limiting stage for lignocellulosic biomass substrates. This study investigates the feasibility of mechanical pretreatment of CS to enhance methane production. Batch anaerobic digestion of CS samples with particle sizes ranging from 0.5 to 65 mm was carried out in 1 L eudiometer batch digesters for 48 days at 37°C. Results showed that methane yield was inversely proportional to particle size, and the quality of biogas was good (54.0–55.2% CH4). Significant increases in methane yield were observed with 20.3% and 26% for samples with a particle size of 3 mm and 0.5 mm, respectively, compared to untreated CS. The coefficient of anaerobic energy turnover was relatively low (20.2–25.5%). Reduction of the CS particle size to 3 mm or less is recommended to achieve effective methane conversion and decrease the retention time in an anaerobic digester from 31 to about 25 days. However, to offset the high energy demand required for grinding, further research should be conducted in combining size reduction with chemical and physicochemical pretreatment.

It is urgent to determine suitable municipal sludge treatment solutions to simultaneously minimize the environmental negative impacts and achieve sustainable energy benefits. In this study, different sludge pretreatment techniques were applied and investigated to enhance the sludge solubility and, subsequently, facilitate the anaerobic biodegradation performance of the mixed sludge under different sludge concentrations and pretreatment techniques. The sludge characteristics before and after pretreatment and batch experiments of anaerobic digestion of sludge samples under different conditions were analyzed and discussed. The results showed that the mechanical pretreatment method, alone and in combination with low-temperature heat treatment, significantly improved the sludge solubility, with the highest solubility at 39.23%. The maximum biomethane yield achieved was 0.43 m3/kg after 10 d of anaerobic digestion of a 3% sludge sample subjected to mechanical and thermal pretreatment prior to anaerobic biodegradation. In comparison, it took more than 28 d to achieve the same biomethane production with the unpretreated sludge sample. Mechanical pretreatment and subsequent heat treatment showed a high ability to dissolve sludge and, subsequently, accelerate anaerobic digestion, thereby providing promising prospects for increasing the treatment capacity of existing and new sludge treatment plants.

The potential use of elm wood in lignocellulosic industries has been hindered by the Dutch elm disease (DED) pandemics, which have ravaged European and North American elm groves in the last century. However, the selection of DED-resistant cultivars paves the way for their use as feedstock in lignocellulosic biorefineries. Here, the production of cellulose nanofibers from the resistant Ulmus minor clone Ademuz was evaluated for the first time. Both mechanical (PFI refining) and chemical (TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl radical)-mediated oxidation) pretreatments were assessed prior to microfluidization, observing not only easier fibrillation but also better optical and barrier properties for elm nanopapers compared to eucalyptus ones (used as reference). Furthermore, mechanically pretreated samples showed higher strength for elm nanopapers. Although lower nanofibrillation yields were obtained by mechanical pretreatment, nanofibers showed higher thermal, mechanical and barrier properties, compared to TEMPO-oxidized nanofibers. Furthermore, lignin-containing elm nanofibers presented the most promising characteristics, with slightly lower transparencies.

International audience; Pre-treatments are often applied in anaerobic digestion in order to improve the performance of the process: increased methane yield and rate. Physical pretreatments are the most commonly used for anaerobic digestion of agricultural waste. The main purpose of this work was to evaluate the effects of different lab-scale mechanical pretreatments on cattle manure. Three mechanical pre-treatments were sequentially applied to cattle manure: shredding, mixing and blending. An original set of analytical procedures was performed before and after mechanical pretreatments, in order to assess physical, chemical and biological properties of the feedstock. Thus, shredding and mixing pre-treatments were not significantly efficient in terms of methane production yield and rate. In contrast, methane production rate increased with blending treatment, and methane yield was slightly improved as well. An increase of soluble chemical oxygen demand (COD) was also reported with blending pretreatment. The reduction of particle size was mainly between 31.5 and 4 mm for all pretreatments and it led to an increase of water retention capacity of the cattle manure. Therefore, mechanical pre-treatments do not only affect the biochemical characteristics of agricultural waste. It also influences its structure and reactivity. In this context, blending pretreatment showed as the most performant pretreatment among the evaluated pretreatments with an increase of 18% on methane rate and a higher COD solubilisation. Graphic Abstract Mechanical pre-treatments are present in almost all biogas plants treating organic waste. However they have been far less investigated than thermal chemical or biological pre-treatments. The objective of this work was to characterize different mechanical effects (shredding mixing and blending) on cow manure. An original characterization procedure has been used including biochemical and physical parameters. Our results show that the methane yield and methane production rate was improved by the pre-treatments the most important effect being blending. Shredding mostly reduced the size of the large particles but its effect on the biochemical characteristics was limited.

Methanization is a technology that involves complex biological reactions and it is the subject of several scientific studies. The paper aims to evaluate the effect of the combined mechanical and ultrasonic pretreatment (CMUP) on the anaerobic digestion (AD) of the household organic waste fraction in Morocco (HOWF), using a continuous stirred tank reactor (CSTR) at mesophilic conditions.This article presents and compares a results obtained by operating two experiments in lab scale reactors with mechanical pretreatment (MP) and with CMUP. The experiment with MP was considered in this study as a control. During the handling period, the effect of CMUP on the AD of HOWF was studied. The process was evaluated in terms of methane production and biodegradability. The stability was maintained within correct parameters throughout the process for each experiment, while the methane yield and biodegradability of the control and CMUP experiments were 382 (mL CH4 g−1VS) (0°C, 1 atm), 72%, and 493 (mL CH4 g−1VS) (0°C, 1 atm), 86 % respectively. This shows clearly that the CMUP enhance the methane production and increase the biodegradability, suggesting that this combination pretreatment improve the hydrolysis and methanogenesis phases of the process.A kinetic study on anaerobic digestion results using the first order model was also used. The mathematical model shows a good fit with the experimental data. Keywords: Anaerobic digestion, HOWF, Mechanical pretreatment, Ultrasonic pretreatment, Methane yield, Biodegradability

Experimental results of leaching tests using waste fractions obtained by mechanical pretreatment of lithium ion batteries (LIB) were reported. Two physical pretreatments were performed at pilot scale in order to recover electrodic powders: the first including crushing, milling, and sieving and the second granulation, and sieving. Recovery yield of electrodic powder was significantly influenced by the type of pretreatment. About 50% of initial LIB wastes was recovered by the first treatment (as electrodic powder with size0.5mm, Sample 1), while only 37% of powder with size1mm (Sample 2) can be recovered by the second treatment. Chemical digestion put in evidence the heterogeneity of recovered powders denoting different amounts of Co, Mn, and Ni. Leaching tests of both powders were performed in order to determine optimized conditions for metal extraction. Solid/liquid ratios and sulfuric acid concentrations were changed according to factorial designs at constant temperature (80°C). Optimized conditions for quantitative extraction (99%) of Co and Li from Sample 1 are 1/10g/mL as solid/liquid ratio and +50% stoichiometric excess of acid (1.1M). Using the same solid/liquid ratio, +100% acid excess (1.2M) is necessary to extract 96% of Co and 86% of Li from Sample 2. Best conditions for leaching of Sample 2 using glucose are +200% acid excess (1.7M) and 0.05M glucose concentration. Optimized conditions found in this work are among the most effective reported in the literature in term of Co extraction and reagent consumption.

Essential oils (EOs) are natural and economically valuable aromatic compounds obtained from a variety of crops and trees, including forest trees, which have different therapeutic and biological activities. This project aims to assess the impact of different residual forest biomass pretreatments on the yield and the properties of EOs, including their antibacterial and antioxidant characteristics. Forest biomass from black spruce (BS, Picea mariana Mill.), balsam fir (BF, Abies balsamea), and jack pine (JP, Pinus banksiana Lamb.) was processed mechanically by (i) shredding, (ii) grinding, (iii) pelletizing, and (iv) bundling. EOs were then extracted by hydro- and steam distillation. The densification into bundles was found to improve EOs yield compared to the other residual forest biomass pretreatments. For example, the yield of bundled BF was improved by 68%, 83%, and 93% compared to shredded, ground, and granulated biomass, respectively. The highest yield was obtained when densification into bundles was combined with extraction through hydrodistillation. As for EOs&rsquo, chemical composition, JP had the highest polyphenol content and consequently the greatest antioxidant activity. EOs derived from BS inhibited the growth of Gram-positive Staphylococcus aureus bacteria and Gram-negative Salmonella typhimurium and Escherichia coli bacteria. The densification of forest biomass into bundles did not affect the antioxidant capacity or the antibacterial activity of EOs, thereby preserving both properties. Thus, the pretreatment of forest biomass residue could have an impact on the volume and the transport costs and therefore improve the bioproducts market and the bioeconomy in Canada.

The effect of organosolv pretreatment was investigated using a 30 L bench-scale ball mill reactor that was capable of simultaneously performing physical and chemical pretreatment. Various reaction conditions were tried in order to discover the optimal conditions for the minimal cellulose loss and enhanced enzymatic digestibility of Miscanthus × giganteus (MG), with conditions varying from room temperature to 170 °C for reaction temperature, from 30 to 120 min of reaction time, from 30% to 60% ethanol concentration, and a liquid/solid ratio (L/S) of 10–20 under non-catalyst conditions. The pretreatment effects were evaluated by chemical compositional analysis, enzymatic digestibility test and X-ray diffraction of the treated samples. The pretreatment conditions for the highest glucan digestibility yield were determined as 170 °C, reaction time of 90 min, ethanol concentration of 40% and L/S = 10. With these pretreatment conditions, the XMG (xylan + mannan + galactan) fractionation yield and delignification were 84.4% and 53.2%, respectively. The glucan digestibility of treated MG after the aforementioned pretreatment conditions was 86.0% with 15 filter paper units (FPU) of cellulase (Cellic® CTec2) per g-glucan enzyme loading.

International audience; Mechanical size reduction is considered as a primordial step of current and future lignocellulosic biorefinery. In this sense, it is of high interest to understand who are the biochemical and structural features of the lignocellulosic biomass, which affect the Specific Energy Requirement (SER), and in consequence the cost of mechanical size reduction processes. First, it was shown that the initial moisture content of the lignocellulosic biomass affect the SER and the final particle size distribution. The highest the moisture content gives raise the highest SER. Then, at fixed initial moisture content (≈7% DW), structural and biochemical features of lignocellulosic biomass that can affect the SER were determined. It was noticed that both arabinose/xylose ratio and accessible surface area lead to increasing the SER. On the contrary, the content of cellulose, lignin, crystallinity and p-coumaric acids links were found to have a positive effect on the reduction of the SER.

Cellulose nanofibrils, as a bionanomaterial with many promising properties, have great potential in composite applications. Herein, well-dispersed and uniform-sized cellulose nanofibrils (CNF) was successfully obtained from commercial bleached softwood kraft pulp, with yields of 79.15% via enzyme-assisted hydrolysis and a subsequent homogenization process. Field emission scanning electron microscope (FE-SEM) confirmed the fiber morphology. Water retention value (WRV) was increased from 107.32% of original pulp to 1383.92% of the resulting CNFs, while crystallinity had no significant changes. Fourier transform infrared (FTIR) spectroscopy indicated the addition of enzyme resulted in the removal of hemicelluloses and lignin. CNFs subjected to enzymatic treatment and homogenization had less entangled network, larger aspect ratio and higher transmittance than those from pure mechanical treatment. They exhibited well-dispersed in aqueous solution and uniform-sized in morphology. These advantages revealed enzyme-assisted process had a remarkable effect on the production of CNFs and made CNFs attractive for nanotechnology and nanomaterial.

Animal manure digestion is associated with limited methane production, due to the high content in fibers, which are hardly degradable lignocellulosic compounds. In this study, different mechanical and thermal alkaline pretreatment methods were applied to partially degradable fibers, separated from the effluent stream of biogas reactors. Batch and continuous experiments were conducted to evaluate the efficiency of these pretreatments. In batch experiments, the mechanical pretreatment improved the degradability up to 45%. Even higher efficiency was shown by applying thermal alkaline pretreatments, enhancing fibers degradability by more than 4-fold. In continuous experiments, the thermal alkaline pretreatment, using 6% NaOH at 55°C was proven to be the most efficient pretreatment method as the methane production was increased by 26%. The findings demonstrated that the methane production of the biogas plants can be increased by further exploiting the fraction of the digested manure fibers which are discarded in the post-storage tank.

An innovative process was optimized to recover Co from portable Lithium Ion Batteries (LIB). Pilot scale physical pretreatment was performed to recover electrodic powder from LIB. Co was extracted from electrodic powder by a hydrometallurgical process including the following main stages: leaching (by acid reducing conditions), primary purification (by precipitation of metal impurities), solvent extraction with D2EPHA (for removal of metal impurities), solvent extraction with Cyanex 272 (for separation of cobalt from nickel), cobalt recovery (by precipitation of cobalt carbonate). Tests were separately performed to identify the optimal operating conditions for precipitation (pH 3.8 or 4.8), solvent extraction with D2EHPA (pH 3.8; Mn/D2EHPA = 4; 10% TBP; two sequential extractive steps) and solvent extraction with Cyanex 272 (pH 3.8; Cyanex/Cobalt = 4, 10% TBP, one extractive step). The sequence of optimized process stages was finally performed to obtain cobalt carbonate. Products with different degree of purity were obtained depending on the performed purification steps (precipitation with or without solvent extraction). 95% purity was achieved by implementation of the process including the solvent extraction stages with D2EHPA and Cyanex 272 and final washing for sodium removal.

Modern mechanical-biological waste treatment plants for the stabilization of both the source-separated organic fraction of municipal solid wastes (OFMSW) and the mixed stream of municipal solid wastes (MSW) include a mechanical pretreatment step to separate recyclable materials such as plastics, glass or metals, before biological treatment of the resulting organic material. In this work, the role of storage and mechanical pretreatment steps in the stabilization of organic matter has been studied by means of respiration techniques. Results have shown that a progressive stabilization of organic matter occurs during the pretreatment of the source-separated OFMSW, which is approximately 30% measured by the dynamic respiration index. In the case of mixed MSW, the stabilization occurring during the reception and storage of MSW is compensated by the effect of concentration of organic matter that the pretreatment step provokes on this material. Both results are crucial for the operation of the succeeding biological process. Finally, respiration indices have been shown to be suitable for the monitoring of the pretreatment steps in mechanical-biological waste treatment plants, with a strong positive correlation between the dynamic respiration index and the cumulative respiration index across all samples tested.

A modified twin-screw extruder incorporated with a filtration device was used as a liquid/solid separator for xylose removal from steam exploded corncobs. A face centered central composite design was used to study the combined effects of various enzymatic hydrolysis process variables (enzyme loading, surfactant addition, and hydrolysis time) with two differently extruded corncobs (7% xylose removal, 80% xylose removal) on glucose conversion. The results showed that the extrusion process led to an increase in cellulose crystallinity, while structural changes could also be observed via SEM. A quadratic polynomial model was developed for predicting the glucose conversion and the fitted model provided an adequate approximation of the true response as verified by the analysis of variance (ANOVA).