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Keywords = vacuum pyrolysis

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25 pages, 6436 KB  
Article
Detoxification and Targeted Conversion of Waste Lithium Battery Electrolyte to Light Hydrocarbons via In Situ Catalytic Pyrolysis: Roles of Li, Ni, Co, and Mn Elements
by Jingyi Wang, Yu Zhang and Lingen Zhang
Separations 2026, 13(6), 163; https://doi.org/10.3390/separations13060163 - 29 May 2026
Viewed by 139
Abstract
Spent lithium-ion battery electrolytes contain fluorine-, sulfur-, and phosphorus-bearing toxins, necessitating deep detoxification and directional conversion into C1–C6 light hydrocarbons. To elucidate the specific catalytic roles and sequential activation of cathode metals (Li, Ni, Co, Mn), this work systematically deconvolutes [...] Read more.
Spent lithium-ion battery electrolytes contain fluorine-, sulfur-, and phosphorus-bearing toxins, necessitating deep detoxification and directional conversion into C1–C6 light hydrocarbons. To elucidate the specific catalytic roles and sequential activation of cathode metals (Li, Ni, Co, Mn), this work systematically deconvolutes their mono- and multi-metallic migration mechanisms over a CaO-ZSM-5* catalyst during vacuum catalytic pyrolysis (530 °C, 100 Pa). Results reveal that Li+ and Ni2+ dominate C–O bond cleavage in carbonates and CaO-ZSM-5*-assisted decarboxylation and oxygen fixation, significantly increasing the relative hydrocarbon content. Conversely, Co2/3+ and Mn4+ release reactive oxygen species, causing deep oxidation of hydrocarbons into CO2 and antagonizing the targeted conversion. In multi-metallic systems, forming composite metal oxides (MxNyOz) increases the energy barrier for releasing active catalytic ions, hindering carbonate cleavage and leaving unreacted carbonate feedstocks. For detoxification, F and P are effectively immobilized as CaF2 and Ca2P2O7. The relative content of detected gas-phase nitriles is minimized to <2% due to the strong antagonistic effect of Ni2+ on Li+-promoted hexanedinitrile cleavage, while sulfur species derived from 1,3-propane sultone are converted to SO2 and ultimately mineralized as calcium and metal-sulfur salts. Mechanistically, product distributions and crystallographic properties suggest a hypothesized sequential activation model—Li+ → Ni2+ → Mn4+—governing reactivity, whereas Co2/3+ does not participate in the synergistic detoxification and selective upgrading process. This migration–reaction coupling framework provides critical insights for cathode-assisted in situ catalytic pyrolysis and closed-loop electrolyte recycling. Full article
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20 pages, 3178 KB  
Article
Resource Utilization of Tea Residue Biomass via Catalytic Vacuum Pyrolysis
by Lifang Li, Mingming Pan, Qing Huang, Yuanyong Yao, Yuhang Xu and Sen Li
Energies 2026, 19(5), 1282; https://doi.org/10.3390/en19051282 - 4 Mar 2026
Viewed by 614
Abstract
Waste biomass represents both an environmental pollutant and a potential renewable energy source. This study examines the feasibility of hydrogen production from tea residue biomass and solid waste, focusing on pyrolysis-based hydrogen generation. Compared to atmospheric pyrolysis, vacuum conditions reduce the saturated vapor [...] Read more.
Waste biomass represents both an environmental pollutant and a potential renewable energy source. This study examines the feasibility of hydrogen production from tea residue biomass and solid waste, focusing on pyrolysis-based hydrogen generation. Compared to atmospheric pyrolysis, vacuum conditions reduce the saturated vapor pressure of biomass volatiles, thereby promoting char gasification, gas-phase interactions, and secondary tar cracking. Utilizing a self-designed vacuum-pyrolysis-catalysis system, we investigated the effects of key parameters—vacuum level, temperature, catalyst-to-feedstock ratio, and retention time on pyrolysis product distribution and formation mechanisms. Results indicate that Ni was successfully and uniformly loaded onto waste calcium oxide desiccant (DC) support via impregnation, thereby significantly increasing the specific surface area of the catalyst. Optimization using response surface methodology identified the following optimal conditions: pressure of 5 kPa, temperature of 835.89 °C, catalyst/feedstock ratio of 110.02%, and retention time of 2.35 h. Under these conditions, a hydrogen yield of 256.39 mL·g−1 was achieved, corresponding to 95.3% of the simulated value. The process not only enabled efficient hydrogen production but also simultaneously yielded bio-oil and biochar, thereby facilitating carbon capture and recycling. These findings provide valuable insights into the resource-oriented application of vacuum pyrolysis-catalysis technology to waste biomass. Full article
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16 pages, 2415 KB  
Review
Recycling Technologies for Extracting Gallium from Light-Emitting Diodes
by Laraib Mustafa, Muhammad Usman, Shazma Ali, Ahmed Ali and Anis Naveed
Photonics 2025, 12(8), 808; https://doi.org/10.3390/photonics12080808 - 12 Aug 2025
Cited by 3 | Viewed by 5578
Abstract
Light-emitting diodes (LEDs) are made up of precious metals, e.g., gallium. These elements can be recovered and reused, reducing the need for new raw materials. Proper recycling prevents harmful substances in LEDs, such as lead and arsenic, from contaminating the environment. Recycling LEDs [...] Read more.
Light-emitting diodes (LEDs) are made up of precious metals, e.g., gallium. These elements can be recovered and reused, reducing the need for new raw materials. Proper recycling prevents harmful substances in LEDs, such as lead and arsenic, from contaminating the environment. Recycling LEDs uses less energy compared to producing new ones, leading to lower carbon emissions. The valuable metal gallium faces the challenge of supply and demand due to the surge in its demand, the difficulty of separating it from minerals, and processing issues during extraction. In this review, we describe the methods for recycling gallium from LEDs by using different techniques such as pyrolysis (95% recovery), oxalic acid leaching (83.2% recovery), HCL acid leaching of coal fly ash (90–95% recovery), subcritical water treatment (80.5% recovery), supercritical ethanol (93.10% recovery), oxidation and subsequent leaching (91.4% recovery), and vacuum metallurgy separation (90% recovery). Based on our analysis, hydrometallurgy is the best approach for recovering gallium. It is reported that approximately 5% of the waste from LEDs is adequately recycled, whereas the total gallium potential wasted throughout production is over 93%. By recycling LEDs, we can minimize waste, conserve resources, and promote sustainable practices. Thus, recycling LEDs is essential for strengthening a circular economy. Full article
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14 pages, 9154 KB  
Article
Evaluation of the Mechanical Properties of Highly Oriented Recycled Carbon Fiber Composites Using the Vacuum-Assisted Resin Transfer Molding, Wet-Layup, and Resin Transfer Molding Methods
by Mio Sato, Yuki Kataoka, Masumi Higashide, Yuichi Ishida and Sunao Sugimoto
Polymers 2025, 17(10), 1293; https://doi.org/10.3390/polym17101293 - 8 May 2025
Cited by 9 | Viewed by 1902
Abstract
Recycling carbon-fiber-reinforced plastics (CFRPs) is crucial for sustainable material utilization, particularly in aerospace applications, where large quantities of prepreg waste are generated. This study investigated the mechanical properties of highly oriented recycled CFRP (rCFRP) molded using vacuum-assisted resin transfer molding (VaRTM), wet-layup, and [...] Read more.
Recycling carbon-fiber-reinforced plastics (CFRPs) is crucial for sustainable material utilization, particularly in aerospace applications, where large quantities of prepreg waste are generated. This study investigated the mechanical properties of highly oriented recycled CFRP (rCFRP) molded using vacuum-assisted resin transfer molding (VaRTM), wet-layup, and traditional RTM methods. Recycled carbon fibers (rCFs) obtained via solvolysis and pyrolysis were processed into nonwoven preforms to ensure fiber alignment through carding. The influence of molding methods, fiber recycling techniques, and fiber orientation on mechanical performance was examined through tensile tests, fiber volume fraction (Vf) analysis, and scanning electron microscopy observations. The results indicated that the solvolysis-recycled rCF exhibited superior interfacial adhesion with the resin, leading to a higher tensile strength and stiffness, particularly in the RTM process, where a high Vf was achieved. Wet-layup molding effectively reduced the void content owing to autoclave curing, maintaining stable properties even with pyrolyzed rCF. VaRTM, while enabling vacuum-assisted resin infusion, exhibited a higher void content, limiting improvements in mechanical performance. This study highlights that tailoring the molding method according to the desired performance, such as increasing stiffness potential by enhancing Vf in RTM or improving tensile strength by improving fiber–matrix adhesion in wet-layup molding, is critical for optimizing rCFRP properties, providing important insights into sustainable CFRP recycling and high-performance material design. Full article
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16 pages, 8231 KB  
Article
A Study on the Effect of an Oxidizing Atmosphere During the Recycling of CFRP by Pyrolysis
by Cynthie Dega, Ali Jadidinia and Rachid Boukhili
Fibers 2025, 13(5), 58; https://doi.org/10.3390/fib13050058 - 7 May 2025
Cited by 4 | Viewed by 2950
Abstract
Composite materials are increasingly in demand. However, challenges such as high raw-material costs and complicated waste management impede their adoption. Overcoming these obstacles requires efficient recycling methods. Pyrolysis effectively recycles carbon fiber-reinforced polymers (CFRPs). This study proposes a cost-effective CFRP recovery approach utilizing [...] Read more.
Composite materials are increasingly in demand. However, challenges such as high raw-material costs and complicated waste management impede their adoption. Overcoming these obstacles requires efficient recycling methods. Pyrolysis effectively recycles carbon fiber-reinforced polymers (CFRPs). This study proposes a cost-effective CFRP recovery approach utilizing conventional ovens to minimize recycling expenses and maximize reclaimed-product value. Pyrolysis was conducted under atmospheric conditions at 450–600 °C, lasting 1–6 h at each temperature. It was optimal at 2.5 h and 500 °C. Higher temperatures caused fiber degradation, and lower temperatures excessively prolonged duration. After determining the optimal conditions, composite plates were produced using recycled carbon fibers and a vacuum-assisted resin infusion process. Subsequent physical characterization and mechanical tests were conducted on these plates to assess the recycled-CFRP properties. The recovered tensile strength and tensile modulus were 88% and 97% that of virgin carbon fibers (vCF), respectively. Full article
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12 pages, 2310 KB  
Article
[3+2] Cycloaddition to a Chiral 5-Methylene-1,3-dioxolan-4-one and Pyrolysis of the Spiro Adducts
by R. Alan Aitken, Lynn A. Power and Alexandra M. Z. Slawin
Molecules 2025, 30(6), 1246; https://doi.org/10.3390/molecules30061246 - 10 Mar 2025
Viewed by 1459
Abstract
The [3+2] cycloaddition chemistry of (2S)-5-methylene-2-t-butyl-1,3-dioxolan-4-one, derived from lactic acid, has been examined, and spiro adducts have been obtained with benzonitrile oxide, acetonitrile oxide, diazomethane and diphenyldiazomethane. The structure and absolute stereochemistry of the benzonitrile oxide adduct has been [...] Read more.
The [3+2] cycloaddition chemistry of (2S)-5-methylene-2-t-butyl-1,3-dioxolan-4-one, derived from lactic acid, has been examined, and spiro adducts have been obtained with benzonitrile oxide, acetonitrile oxide, diazomethane and diphenyldiazomethane. The structure and absolute stereochemistry of the benzonitrile oxide adduct has been confirmed by X-ray diffraction, and all the adducts have been fully characterised by 1H and 13C NMR. Attempted cycloaddition with a nitrile sulfide, a nitrile imine and azides failed. Pyrolysis results in a range of novel gas-phase reactions, with the nitrile oxide adducts giving pivalaldehyde, CO2, the nitrile and ketene, the diazomethane adduct losing only N2 to give a cyclopropane-fused dioxolanone, and the diphenylcyclopropane derived from diphenyldiazomethane giving mainly benzophenone in a sequence involving the loss of pivalaldehyde and methyleneketene. Full article
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21 pages, 1095 KB  
Review
Effects of Calcium-Oxide-Modified Biochar on the Anaerobic Digestion of Vacuum Blackwater
by Ping Fa Chiang, Teng Ling Zhang, Abdulmoseen Segun Giwa, Ndungutse Jean Maurice, Mugabekazi Joie Claire, Nasir Ali, Ehtisham Shafique and Mohammadtaghi Vakili
Molecules 2025, 30(2), 215; https://doi.org/10.3390/molecules30020215 - 7 Jan 2025
Cited by 13 | Viewed by 4152
Abstract
The increasing global population and urbanization have led to significant challenges in waste management, particularly concerning vacuum blackwater (VBW), which is the wastewater generated from vacuum toilets. Traditional treatment methods, such as landfilling and composting, often fall short in terms of efficiency and [...] Read more.
The increasing global population and urbanization have led to significant challenges in waste management, particularly concerning vacuum blackwater (VBW), which is the wastewater generated from vacuum toilets. Traditional treatment methods, such as landfilling and composting, often fall short in terms of efficiency and sustainability. Anaerobic digestion (AD) has emerged as a promising alternative, offering benefits such as biogas production and digestate generation. However, the performance of AD can be influenced by various factors, including the composition of the feedstock, pH levels, and the presence of inhibitors. This review investigates the effects of calcium oxide (CaO)-modified biochar (BC) as an additive in AD of VBW. Modifying BC with CaO enhances its alkalinity, nutrient retention, and adsorption capacity, creating a more favorable environment for microorganisms and promoting biogas production, which serves as a valuable source of heat, fuel and electricity. Additionally, the digestate can be processed through plasma pyrolysis to ensure the complete destruction of pathogens while promoting resource utilization. Plasma pyrolysis operates at extremely high temperatures, effectively sterilizing the digestate and eliminating both pathogens and harmful contaminants. This process not only guarantees the safety of the end products, but also transforms organic materials into valuable outputs such as syngas and slag. The syngas produced is a versatile energy carrier that can be utilized as a source of hydrogen, electricity, and heat, making it a valuable resource for various applications, including fuel cells and power generation. Furthermore, the slag has potential for reuse as an additive in the AD process or as a biofertilizer to enhance soil properties. This study aims to provide insights into the benefits of using modified BC as a co-substrate in AD systems. The findings will contribute to the development of more sustainable and efficient waste management strategies, addressing the challenges associated with VBW treatment while promoting renewable energy production. Full article
(This article belongs to the Topic Advances in Organic Solid Waste and Wastewater Management)
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13 pages, 3498 KB  
Article
Effects of Preformed Composition and Pore Size on Microstructure and Properties of SiCf/SiC Composites via Reactive Melt Infiltration
by Haifeng Nie, Pingzhan Si, Quanxing Ren, Ziqiang Yin, Tihao Cao, Zhengren Huang, Qing Huang and Yinsheng Li
Materials 2024, 17(23), 5765; https://doi.org/10.3390/ma17235765 - 25 Nov 2024
Cited by 8 | Viewed by 3097
Abstract
This study investigated the influence of preformed composition and pore size on the microstructure and properties of SiCf/SiC composites fabricated via reactive melt infiltration (RMI). The process began with the impregnation of SiC fiber cloth with phenolic resin, followed by lamination [...] Read more.
This study investigated the influence of preformed composition and pore size on the microstructure and properties of SiCf/SiC composites fabricated via reactive melt infiltration (RMI). The process began with the impregnation of SiC fiber cloth with phenolic resin, followed by lamination and pyrolysis. Subsequent steps included further impregnations with phenolic resin, SiC slurry, and carbon black slurry, each followed by additional pyrolysis. This process resulted in three types of preforms, designated as PP, PS, and PC. These preforms exhibited a multimodal distribution of pore size, with peak pore diameters around 5 μm for PP, ranging from 200 nm to 4 μm for PS, and approximately 150 nm for PC. The preforms were then subjected to molten silicon infiltration at 1600 °C under vacuum for 1 h to create SiCf/SiC composites. The PP preform contained only pyrolytic carbon, leading to a composite with high closed porosity and unreacted carbon, resulting in poor mechanical properties. The PS preform, which was impregnated with SiC particles, displayed an optimized pore size distribution but retained significant amounts of residual silicon and carbon in the final composite. In contrast, the PC preform featured both an ideal pore size distribution and an adequate amount of carbon, achieving high density and low porosity with reduced residual phases in the final composite. This optimization led to a flexural strength of 152.4 ± 15.4 MPa, an elastic modulus of about 181.1 ± 0.1 GPa, and a thermal conductivity of 27.7 W/mK in the SiCf/SiC composites product. These findings underscore the importance of preform optimization in enhancing the performance of SiCf/SiC composites, potentially paving the way for more reliable nuclear fuel cladding solutions. Full article
(This article belongs to the Section Advanced Composites)
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19 pages, 15782 KB  
Article
Recycled Carbon Black/High-Density Polyethylene Composite from Waste Tires: Manufacturing, Testing, and Aging Characterization
by Catherine Billotte, Laurence Romana, Anny Flory, Serge Kaliaguine and Edu Ruiz
Recycling 2024, 9(6), 107; https://doi.org/10.3390/recycling9060107 - 5 Nov 2024
Cited by 6 | Viewed by 6212
Abstract
This study addresses the global issue of recycling used vehicle tires, typically burned out or trimmed to be reused in playground floors or road banks. In this study, we explore a novel environmentally responsive approach to decomposing and recovering the carbon black particles [...] Read more.
This study addresses the global issue of recycling used vehicle tires, typically burned out or trimmed to be reused in playground floors or road banks. In this study, we explore a novel environmentally responsive approach to decomposing and recovering the carbon black particles contained in tires (25–30 wt.%) by vacuum pyrolysis. Given that carbon black is well known for its UV protection in plastics, the objective of this research is to provide an ecological alternative to commercial carbon black of fossil origin by recycling the carbon black (rCB) from used tires. In our research, we create a composite material using rCB and high-density polyethylene (HDPE). In this article, we present the environmental aging studies carried out on this composite material. The topographic evolution of the samples with aging and the oxidation kinetics of the surface and through the thickness were studied. The Beer–Lambert law is used to relate the oxidative index to the characteristic depth of the samples. The UV photons are observed to penetrate up to 54% less with the addition of 6 wt.% of rCB compared to virgin HDPE. In this work, the addition of rCB as filler for HDPE used for outdoor applications has demonstrated to be an antioxidant for UV protection and a good substitute for commercial carbon black for industrial goods. Full article
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17 pages, 5350 KB  
Article
High-Speed Removal Process for Organic Polymers by Non-Thermal Atmospheric-Pressure Spark Discharge at Room Temperature and Its Mechanism
by Yoshihiro Sakamoto, Takayoshi Tsutsumi, Hiromasa Tanaka, Kenji Ishikawa, Hiroshi Hashizume and Masaru Hori
Coatings 2024, 14(10), 1339; https://doi.org/10.3390/coatings14101339 - 18 Oct 2024
Viewed by 1508
Abstract
Heel marks (HMs) are a type of dirt stain consisting of polyester-based urethane rubber on polyvinyl chloride (PVC) floor surfaces. The rapid removal of HMs was achieved by using non-thermal atmospheric-pressure plasma technology. Mimetic HMs were prepared by coating PVC floor samples with [...] Read more.
Heel marks (HMs) are a type of dirt stain consisting of polyester-based urethane rubber on polyvinyl chloride (PVC) floor surfaces. The rapid removal of HMs was achieved by using non-thermal atmospheric-pressure plasma technology. Mimetic HMs were prepared by coating PVC floor samples with HMs to a thickness of 13.9 μm. The removal area, thickness, and volume were measured after applying spark discharges at high voltage and a repetition rate of 50 kHz. The treated surfaces were analyzed by using X-ray photoelectron spectroscopy (XPS) and pyrolysis–gas chromatography with time-of-flight mass spectrometry (Py-GC/TOFMS). Removal rates of 20 mm2/min in area, 52 mm3/min in volume, and 7 μm/min in depth were achieved with an inter-electrode distance of 10.0 mm and an air flow rate of 20 standard liters per minute. A removal depth of 10 μm/min was achieved without air supply. The mechanism of stain removal by spark discharge was modeled by decomposing the original high-molecular-weight molecules in polyester-based urethane rubber into low-molecular-weight molecules, such as methylene diisocyanate (MDI) components. The results of this study may facilitate the development of a novel electric vacuum cleaner capable of removing floor stains. Full article
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19 pages, 5194 KB  
Article
Effect of Polyethylene Glycol with Different Molecular Weights on the Properties of Mytilaria laosensis Timber
by Linhan He, Xiaoling Liu, Yin Kuang, Liuliu Wang, Songwu Chen, Yufen Luo and Yao Chen
Forests 2024, 15(8), 1401; https://doi.org/10.3390/f15081401 - 10 Aug 2024
Cited by 3 | Viewed by 2501
Abstract
Mytilaria laosensis, a common fast-growing tree species in southern China, boasts excellent growth speed and attractive color and texture. However, due to its short growth cycle and high proportion of juvenile wood, it typically exhibits poor dimensional stability and low strength, which [...] Read more.
Mytilaria laosensis, a common fast-growing tree species in southern China, boasts excellent growth speed and attractive color and texture. However, due to its short growth cycle and high proportion of juvenile wood, it typically exhibits poor dimensional stability and low strength, which significantly limits its practical applications. This study uses vacuum impregnation to modify M. laosensis wood with polyethylene glycol (PEG), focusing on the effects and mechanisms of PEG with different molecular weights on wood properties. The results indicate that PEG enters the wood cell walls through capillary action and diffusion, forming hydrogen bonds with the free hydroxyl groups on cellulose and hemicellulose, which keeps the cell walls swollen and enhances dimensional stability. Post modification, the dimensional stability of M. laosensis wood improved, with an anti-swelling efficiency ranging from 61.43% to 71.22%, showing an initial increase followed by a decrease with increasing PEG molecular weight. The optimal PEG molecular weight for anti-swelling efficiency was 1500 Da, achieving 71.22%. The flexural modulus of elasticity and flexural strength of the treated wood also first decreased and then increased with increasing PEG molecular weight. Among them, the PEG1000-treated material showed the best performance, with the flexural modulus of elasticity increased by about 29% and the flexural strength increased by about 5% compared to untreated wood. Additionally, PEG, having a higher pyrolysis temperature than wood, raised the initial pyrolysis temperature and maximum pyrolysis rate temperature of M. laosensis wood, thus improving its thermal stability. These findings provide scientific evidence and technical support for the efficient utilization and industrialization of M. laosensis wood, promoting its widespread application and industrial development. Full article
(This article belongs to the Section Wood Science and Forest Products)
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20 pages, 2890 KB  
Article
Variety and Site Drive Salix Mixture Effects on Soil Organic Matter Chemistry and Soil Carbon Accumulation
by Joel Jensen, Petra Fransson, Christel Baum, Peter Leinweber, Kai-Uwe Eckhardt and Martin Weih
Forests 2024, 15(8), 1339; https://doi.org/10.3390/f15081339 - 1 Aug 2024
Viewed by 1710
Abstract
Soil organic matter (SOM) is essential for nutrient cycling and soil carbon (C) accumulation, both of which are heavily influenced by the quality and quantity of plant litter. Since SOM dynamics in relation to plant diversity are poorly understood, we investigated the effects [...] Read more.
Soil organic matter (SOM) is essential for nutrient cycling and soil carbon (C) accumulation, both of which are heavily influenced by the quality and quantity of plant litter. Since SOM dynamics in relation to plant diversity are poorly understood, we investigated the effects of willow variety and mixture, and site on the soil C stocks, SOM chemical composition and thermal stability. Using pyrolysis-field ionization mass spectrometry (Py-FIMS), a method of stepwise thermal degradation in ultrahigh vacuum combined with soft ionization in a high electric field, followed by mass-spectrometric separation and detection of molecular ions, we analyzed SOM in the top 10 cm of soil from two 7-year-old experimental sites in Germany and Sweden. Monocultures and mixtures of two willow varieties (Salix spp.) belonging to different species were grown at the experimental plots. Overall, site had the strongest effect on SOM quality. The results showed significant variability across sites for willow identity and mixture effects on C accumulation and SOM chemistry. In the German site (Rostock), yearly soil C accumulation was higher (p < 0.05) for variety ‘Loden’ (1.0 Mg C ha−1 year−1) compared to ‘Tora’ (0.5 Mg C ha−1 year−1), whilst in the Swedish site (Uppsala), both varieties exhibited similar soil C accumulation rates of around 0.6 Mg C ha−1 year−1. Willow variety identity significantly affected SOM quality at both sites, while mixing had minor effects. Our findings emphasize the significance of site-specific context and variety and species identity in shaping soil C accumulation in willow plantations. Full article
(This article belongs to the Section Forest Soil)
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14 pages, 2562 KB  
Article
Utilizing Date Palm Leaf Biochar for Simultaneous Adsorption of Pb(II) and Iodine from Aqueous Solutions
by Essam R. I. Mahmoud, Hesham M. Aly, Noura A. Hassan, Abdulrahman Aljabri, Asim Laeeq Khan and Hashem F. El-Labban
Processes 2024, 12(7), 1370; https://doi.org/10.3390/pr12071370 - 1 Jul 2024
Cited by 8 | Viewed by 2693
Abstract
This study addresses the environmental and health hazards posed by Pb(II) and iodine, two significant contaminants. The objective was to explore the adsorption of these substances from aqueous solutions using biochar derived from the leaf midribs of the date palm through a slow [...] Read more.
This study addresses the environmental and health hazards posed by Pb(II) and iodine, two significant contaminants. The objective was to explore the adsorption of these substances from aqueous solutions using biochar derived from the leaf midribs of the date palm through a slow pyrolysis process. The pyrolysis was conducted in two stages within a vacuum furnace: initially at 300 °C for 1 h followed by overnight cooling, and then at 600 °C with a similar cooling process. The resulting biochar was characterized for its microstructural features and functional groups using scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy. It exhibited a porous structure with large numbers of pores (20 to 50 μm in size) and functional groups including O-H, C-H, and C=C, which are integral to its adsorption capabilities. For the adsorption studies, a 100 ppm Pb(II) ion solution was treated with varying amounts of biochar (20, 40, 60, and 80 mg) for 24 h. In parallel, iodine adsorption was tested, with biochar quantities ranging from 0.1 to 0.4 g/50 mL. Both treatments were followed by filtration and analysis using atomic absorption spectroscopy to determine the remaining concentrations of Pb(II) and iodine. The study also explored the effect of varying incubation periods (up to 30 h) on iodine adsorption. The results were significant; 100% adsorption of Pb(II) was achieved with the addition of 60 mg of biochar per 10 mL of solution. In contrast, for iodine, a maximum adsorption of 39.7% was observed with 30 mg or 40 mg of biochar per 50 mL. These findings demonstrate the potential of date palm-derived biochar as an effective and sustainable material for the removal of Pb(II) and iodine from contaminated water, offering valuable insights for environmental remediation strategies. Full article
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12 pages, 1943 KB  
Article
Rearrangement of Arylsulfamates and Sulfates to Para-Sulfonyl Anilines and Phenols
by Yifei Zhou and Alan M. Jones
Molecules 2024, 29(7), 1445; https://doi.org/10.3390/molecules29071445 - 23 Mar 2024
Cited by 3 | Viewed by 3361
Abstract
The C(sp2)-aryl sulfonate functional group is found in bioactive molecules, but their synthesis can involve extreme temperatures (>190 °C or flash vacuum pyrolysis) and strongly acidic reaction conditions. Inspired by the 1917 Tyrer industrial process for a sulfa dye that [...] Read more.
The C(sp2)-aryl sulfonate functional group is found in bioactive molecules, but their synthesis can involve extreme temperatures (>190 °C or flash vacuum pyrolysis) and strongly acidic reaction conditions. Inspired by the 1917 Tyrer industrial process for a sulfa dye that involved an aniline N(sp2)-SO3 intermediate en route to a C(sp2)-SO3 rearranged product, we investigated tributylsulfoammonium betaine (TBSAB) as a milder N-sulfamation to C-sulfonate relay reagent. Initial investigations of a stepwise route involving TBSAB on selected anilines at room temperature enabled the isolation of N(sp2)-sulfamate. Subsequent thermal rearrangement demonstrated the intermediary of a sulfamate en route to the sulfonate; however, it was low-yielding. Investigation of the N-sulfamate to C--sulfonate mechanism through control experiments with variation at the heteroatom positions and kinetic isotope experiments (KIEH/D) confirmed the formation of a key N(sp2)-SO3 intermediate and further confirmed an intermolecular mechanism. Furthermore, compounds without an accessible nitrogen (or oxygen) lone pair did not undergo sulfamation- (or sulfation) -to-sulfonation under these conditions. A one-pot sulfamation and thermal sulfonation reaction was ultimately developed and explored on a range of aniline and heterocyclic scaffolds with high conversions, including N(sp2)-sulfamates (O(sp2)-sulfates) and C(sp2)-sulfonates, in up to 99 and 80% (and 88% for a phenolic example) isolated yield, respectively. Encouragingly, the ability to modulate the ortho-para selectivity of the products obtained was observed under thermal control. A sulfonated analog of the intravenous anesthetic propofol was isolated (88% yield), demonstrating a proof-of-concept modification of a licensed drug alongside a range of nitrogen- and sulfur-containing heterocyclic fragments used in drug discovery. Full article
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16 pages, 12142 KB  
Article
Response Surface Methodology—Central Composite Design Optimization Sugarcane Bagasse Activated Carbon under Varying Microwave-Assisted Pyrolysis Conditions
by Xuexue Chen, Yunji Pei, Xinran Wang, Wenlin Zhou and Li Jiang
Processes 2024, 12(3), 497; https://doi.org/10.3390/pr12030497 - 28 Feb 2024
Cited by 5 | Viewed by 3253
Abstract
Sugarcane bagasse (SB) is a widely available agro-industrial waste residue in China that has the potential to be converted into a cost-effective and renewable adsorbent. In this study, activated carbon (AC) was prepared from SB by microwave vacuum pyrolysis using H3PO [...] Read more.
Sugarcane bagasse (SB) is a widely available agro-industrial waste residue in China that has the potential to be converted into a cost-effective and renewable adsorbent. In this study, activated carbon (AC) was prepared from SB by microwave vacuum pyrolysis using H3PO4 as the activator. To enhance the sorption selectivity and yield, the pyrolysis process of SB-activated carbon (SBAC) should be well-designed. Central composite design was employed as an optimized experiment design, and response surface methodology was used to optimize the process parameters for maximized SBAC yield and its iodine number. The results showed that the optimized parameters obtained for the SBAC are 2.47 for the impregnation ratio (IR), 479.07 W for microwave power (MP), 23.86 mm for biomass bed depth, and 12.96 min for irradiation time, with responses of 868.7 mg/g iodine number and 43.88% yield. The anticipated outcomes were substantiated, revealing a marginal 5.4% variance in yield and a mere 1.9% discrepancy in iodine number from the forecasted values. The synthesized adsorbents underwent comprehensive characterization through instrumental methodologies, including FT-IR, BET, and SEM. The SBAC produced by the pyrolysis method contained a regular and homogeneous porous structure with a specific surface area of up to 1697.37 m2/g and a total 1.20 cm 3/g volume, which has favorable adsorption of toxic and harmful substances in the environment. Full article
(This article belongs to the Special Issue Advances in Recycling and Utilization of Agricultural Wastes)
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