Hydrothermal Treatment Research Articles

Chitosan-coated manganese ferrite nanoparticles enhanced Rhodotorula toruloides carotenoid production.

The present study aims to analyze the interaction between Rhodotorula toruloides and magnetic nanoparticles and evaluate their effect on carotenoid production. The manganese ferrite nanoparticles were synthesized without chitosan (MnFe2O4) and chitosan coating (MnFe2O4-CS) by the co-precipitation method assisted by hydrothermal treatment. XRD (X-ray diffraction), Magnetometry, Dynamic Light Scattering (DLS) and FTIR (Fourier-Transform Infrared Spectroscopy), are used to characterize the magnetic nanoparticles. The crystallite size of MnFe2O4 was 16 nm for MnFe2O4 and 20 nm for MnFe2O4-CS. The magnetic saturation of MnFe2O4-CS was lower (39.6 ± 0.6 emu/g) than the same MnFe2O4 nanoparticles (42.7 ± 0.3 emu/g), which was attributed to the chitosan fraction presence. The MnFe2O4-CS FTIR spectra revealed the presence of the characteristic chitosan bands. DLS demonstrated that the average hydrodynamic diameters were 344 nm for MnFe2O4 and 167 nm for MnFe2O4-CS. A kinetic study of cell immobilization performed with their precipitation with a magnet demonstrated that interaction between magnetic nanoparticles and R. toruloides was characterized by an equilibrium time of 2h. The adsorption isotherm models (Langmuir and Freundlich) were fitted to the experimental values. The trypan blue assay was used for cell viability assessment. The carotenoid production increased to 256.2 ± 6.1 µg/g dry mass at 2.0 mg/mL MnFe2O4-CS. The use of MnFe2O4-CS to stimulate carotenoid yeast production and the magnetic separation of biomass are promising nanobiotechnological alternatives. Magnetic cell immobilization is a perspective technique for obtaining cell metabolites.

Preparation of Novel Hierarchical Catalysts by Simultaneous Generation of β-Zeolite and Mesoporous Silica for Catalytic Cracking.

The gel skeletal reinforcement (GSR) method was applied at the preparation stage of β-zeolite to prepare a novel hierarchical catalyst. A solution of hexamethyldisiloxane (HMDS) and acetic anhydride, a GSR reagent, was added to the mixture of colloidal silica, sodium aluminate, tetraethylammonium hydroxide, sodium hydroxide and water, and successive aging and hydrothermal treatment gave microporous β-zeolite surrounded by mesoporous silica like core-shell structure. Its properties were characterized by XRD, nitrogen adsorption and desorption, NH3-TPD, TEM, and TG-DTA measurements, and further characteristics of the catalysts produced were clarified by the catalytic cracking of n-dodecane. The hierarchical structure of microporous zeolite and mesoporous silica was shown from GSR-2.9HS-H-Beta to GSR-3.2HS-H-Beta, where the molar ratio of HMDS and silica source of β-zeolite was 2.9~3.2 : 100. It was found that in the catalytic cracking of n-dodecane, the relative activity (the conversion per the amount of zeolite crystals) increased with the increase in mesopore volume and surface area. The result indicated that the introduction of mesopores was effective even in catalytic cracking of small molecule of n-dodecane.

Micro/Meso‐Porous Double‐Shell Hollow Carbon Spheres through Spatially Confined Pyrolysis for Supercapacitors and Zinc‐Ion Capacitor

AbstractEnergy storage in supercapacitors and hybrid zinc ion capacitors (ZIC) using porous carbon materials offers a promising alternative method for clean energy solutions. The unique combination of hierarchical porous structure and nitrogen doping in these materials has demonstrated significant capacity for energy storage. Nevertheless, the full potential of these materials, particularly the relationship between pore structure configuration and performance, remains underexplored. Herein, a confined pyrolysis strategy based on the polymerization characteristics of polydopamine (PDA) was developed to construction of hollow carbon spheres with microporous/mesoporous dual shell structure. The depth of micropores and cavity can be controlled by adjusting the duration of heat treatment and hydrothermal treatment, in accordance with the decomposition and polymerization characteristics of PDA. Due to the elasticity of this structure, the relationship between the micro/mesoporous depth of the prepared carbon spheres and the energy storage performance in supercapacitors and ZIC is established. Through optimizing the ion transport capacity of carbon spheres and considering the influence of its internal cavity structure on energy storage, the resulting carbon spheres exhibit high specific capacitance of 389 F g−1 in supercapacitor and specific capacitance of 260 F g−1 and excellent stability with 99.3 % retention after 30000 chare/discharge cycles in ZIC.

High removal of volatile organic compounds on hierarchical carbons prepared from agro-industrial waste of banana fruit production for air decontamination.

Activated carbons were prepared from residues from agro-industrial banana production (banana pseudostem) and evaluated in the capture of five different volatile organic compounds (VOCs): dichloromethane, chloroform, ethyl acetate, hexane, and cyclohexane. The biomass was first submitted to a hydrothermal treatment in the presence of KOH or ZnCl2 as activating agents, followed by a dry pyrolysis. This new advance in methodology contributes to producing activated carbons with hierarchical porosity and high surface areas (701-1312 m2g-1), promoting increased interest in managing waste from banana fruit agricultural production. VOC capture studies were performed by thermal analysis, and capture capacities were similar to or higher than those presented in the literature. Higher adsorption capacities were related to the amount of available micropores, and the capture capacity was enhanced by the contribution of small mesopores. As the highest adsorbed amounts of dichloromethane (933mgg-1 at 25°C) were obtained for the material activated with ZnCl2 (1:3), further studies were carried out for this system. The experimental data was fitted using a pseudo-first-order kinetic model. A study was carried out in different atmospheres (He, N2, air), showing that co-adsorption is occurring. Under simulated environmental conditions, the capture capacity decreased slightly at equilibrium, and the new adsorbent was used for up to ten cycles without significantly losing its efficiency, indicating good application in the field.

Nitrogen and Sulfur Co-doped Carbon Dots for Ratiometric Fluorometric Determination of Mercury Ions.

Nitrogen and sulfur co-doped carbon dots (N, S-CDs) were prepared for dual-channel ratiometric fluorescence determination of mercury ions (Hg2+). The dual-emission N, S-CDs were synthesized using a simple one-pot hydrothermal treatment. When excited with visible light, N,S-CDs exhibited two emission peaks at 390 and 500nm. Notably, the presence of Hg2+ caused a considerable decrease in the fluorescence of N, S-CDs at 500nm, mainly due to the static quenching effect. In comparison, the fluorescence at 390nm was almost unchanged. With a limit of detection (LOD) of 0.21 µM for Hg2+, the N, S-CDs were successfully applied to the unlabeled ratiometric fluorescence determination of Hg2+ in actual water samples with good recoveries (94.5-107.8%). In conclusion, this developed ratiometric fluorescent sensor provides a reliable, environmentally friendly, rapid, and efficient platform for detecting Hg2+ in environmental applications.

Screening of agroindustry residues for their usage as oxygen evolution reaction catalysts

The Oxygen Evolution Reaction (OER) is the limiting step of the water splitting process for the attainment of valuable hydrogen. A green and economic catalyst is hereby synthesized to reduce the OER overpotential. For the first time, a set of representative agroindustry residues were used and subjected to pyrolytic and hydrothermal treatments, fitting them into circular economy. Hydrothermally treated potato peels (PP-HC), particularly, reached 10, 50 and 100 mA/cm2 at overpotentials of 353, 408 and 431 mV, respectively. The novel material showed good electron-transfer and small Tafel slope (52.2±0.2 mV/dec) that is explained by the presence of electronic rich bonds as confirmed by physical-chemical and electrochemical characterization. PP-HC showed an astonishingly high stability for 90 h or 8000 cyclic voltammetries, with the hydrochar suffering only slight modifications, as measured by FTIR and XPS. This innovative study opens a path to efficient and environmentally friendly green hydrogen.

Exploring Platinum Thin Films as Electrodes for High‐Temperature and ‐Pressure Electrochemical Studies in Aqueous Systems

ABSTRACTThis work reports a methodology for the fabrication of Pt thin‐film electrodes for electrochemical studies in hydrothermal systems. The research process was meticulous, with particular attention paid to the multilayer Ti/Pt/Ti/Al2O3 film structure and annealing conditions that are expected to impact the morphology of the films, surface composition and electrochemical response. The findings of this study are significant, as they provide valuable insights into the behaviour of Pt thin‐film electrodes in various media and conditions. Two different approaches were adopted for the preparation of the electrodes: in one case, the Ti/Pt/Ti/Al2O3 films deposited on sapphire wafers were exposed to rapid thermal annealing at 900°C under argon for 5 min, followed by argon ion milling to etch the final electrode pattern (Pt‐RA(900)), while in the other case, uncapped Pt films were annealed, after etching, in a tubular oven under argon at specific temperatures between 200°C and 900°C (Pt‐TO). Rapid annealing at 900°C on capped films resulted in the formation of a Pt3Ti intermetallic alloy with remarkable mechanical and chemical stability even after 10 h of immersion in deionised water, acid (0.1 M H2SO4) and alkaline media (0.1 M KOH) conditions at temperatures up to 150°C, despite the dissolution of the Al2O3 top layer at 150°C and long immersion times (> 10 h). In the case of uncapped Pt films, diffusion and oxidation of Ti through the Pt film at high temperature resulted in the formation of TiO2 on the surface of Pt. The results were confirmed by using a comprehensive suite of ex‐situ characterisation techniques to follow changes in the Pt electrode surface morphology and composition before and after immersion in H2O, 0.1 M H2SO4 and 0.1 M KOH solutions under argon. Ex‐situ electrochemical characterisation studies were also conducted to correlate the changes in the electrode surface properties, including the electrochemical surface area, with different annealing conditions and after various hydrothermal treatments in neutral, alkaline and acidic media.

The Paradoxical Influence of Hydrothermally Treated Zeolites on the Hydrocarbon Pool Mechanism.

Understanding the mechanistic intricacies of hydrothermally treated zeolite is crucial for valorizing any oxygen-containing renewable feedstocks (e.g., methanol, carbon dioxide, biomass). Additionally, the regeneration of deactivated zeolite catalysts under oxidative conditions, akin to hydrothermal treatment, is essential in industrial processes. While research in this area has predominantly focused on characterizing steaming-induced physicochemical changes in zeolite, their ultimate impact on the organic reaction mechanism governed by the hydrocarbon pool dual-cycle mechanism remains unclear. To bridge this knowledge gap, this study investigates the effect of steamed zeolite on the organic reaction mechanism during the industrially significant methanol-to-hydrocarbons process. We achieved this objective by strategically integrating catalytic and control experiments over the pristine and steamed zeolites and their advanced characterization, including under operando conditions, XRD structural refinement, and using "mobility-dependent" solid-state NMR spectroscopy. This multimodal characterization approach was instrumental in elucidating elusive mechanistic information in the dual-cycle mechanism, shedding light on phenomena such as the unchanged ethylene selectivity despite decreasing aromatics selectivity, while ethylene could solely be derived from arene-based reaction intermediates. This study could improve the process efficiency in zeolite catalysis by connecting steaming-induced changes in the organic reaction mechanisms with inorganic material aspects.

The Paradoxical Influence of Hydrothermally Treated Zeolites on the Hydrocarbon Pool Mechanism

Understanding the mechanistic intricacies of hydrothermally treated zeolite is crucial for valorizing any oxygen‐containing renewable feedstocks (e.g., methanol, carbon dioxide, biomass). Additionally, the regeneration of deactivated zeolite catalysts under oxidative conditions, akin to hydrothermal treatment, is essential in industrial processes. While research in this area has predominantly focused on characterizing steaming‐induced physicochemical changes in zeolite, their ultimate impact on the organic reaction mechanism governed by the hydrocarbon pool dual‐cycle mechanism remains unclear. To bridge this knowledge gap, this study investigates the effect of steamed zeolite on the organic reaction mechanism during the industrially significant methanol‐to‐hydrocarbons process. We achieved this objective by strategically integrating catalytic and control experiments over the pristine and steamed zeolites and their advanced characterization, including under operando conditions, XRD structural refinement, and using “mobility‐dependent” solid‐state NMR spectroscopy. This multimodal characterization approach was instrumental in elucidating elusive mechanistic information in the dual‐cycle mechanism, shedding light on phenomena such as the unchanged ethylene selectivity despite decreasing aromatics selectivity, while ethylene could solely be derived from arene‐based reaction intermediates. This study could improve the process efficiency in zeolite catalysis by connecting steaming‐induced changes in the organic reaction mechanisms with inorganic material aspects.

Flower-Shaped MnFe2O4@MoS2 Nanocomposite Activated H2O2 for Efficient Degradation of Tetracycline: Performance Evaluation, Mechanism and Degradation Pathway

The limited utilization of H2O2 restricts the practical application of heterogeneous Fenton oxidation technology. In this study, the flower-shaped MnFe2O4@MoS2 nanocomposite was prepared by two-step hydrothermal treatment, constructing MnFe2O4@MoS2/H2O2 system for the degradation of tetracycline (TC). Under optimized conditions, MnFe2O4@MoS2/H2O2 system fully degraded 20 mg·L−1 of TC within 60 min, and the corresponding utilization of H2O2 was also as high as 95.7%. Meanwhile, this system not only exhibited excellent cycling stability for the degradation of TC but also had good anti-interference ability against actual water sources, inorganic cations and anions and natural organic compounds. The efficient activation of H2O2 in MnFe2O4@MoS2/H2O2 system mainly relied on the redox cycling of Fe(II)/Fe(III) and Mn(II)/Mn(III) mediated by MoS2; meanwhile, the oxygen vacancies caused by redox cycling also accelerated activation of H2O2, resulting in the production of a large number of active species (·OH, ·O2− and 1O2) for rapid degradation of pollutants. The vulnerable atomic sites of TC were confirmed through theoretical calculation, and four degradation pathways of TC in MnFe2O4@MoS2/H2O2 system were proposed. Finally, the toxicity analysis confirmed that the toxicity of degradation intermediates was developing towards low toxicity. This study provided new insights into the wide application of heterogeneous Fenton systems in wastewater treatment.

Hydrothermal Valorization of Biosugars with Heterogeneous Catalysts: Advances, Catalyst Deactivation, Mitigation Strategies and Perspectives.

Sustainable production of valuable biochemicals and biofuels from lignocellulosic biomass necessitates the development of durable and high-performance catalysts. To assist the next-stage catalyst design for hydrothermal treatment of biosugars, this paper provides a critical review of (1) recent advances in biosugar hydrothermal valorization using heterogeneous catalysts, (2) the deactivation process of catalysts based on recycling tests of representative biosugar hydrothermal treatments, (3) state-of-the-art understandings of the deactivation mechanisms of heterogeneous catalysts, and (4) strategies for preparing durable catalysts and the regeneration of deactivated catalysts. Based on the review, challenges and perspectives are proposed. Some remarkable achievements in heterogeneous catalysis of biosugars are highlighted. The understanding of catalyst durability needs to be further enhanced based on full examination of the catalytic performance based on the conversion of substrates, the yield, and selectivity of products. Further, a full examination of the physiochemical changes based on multiple characterization techniques is required to eclucidate the relationships between treatment variables and catalyst durability. Collectively, a clear understanding of the relationships between chemical reaction pathways, treatment variables, and the physiochemistry of catalysts is encouraged to be gained to advise the development of heterogeneous catalysts for long-term and efficient hydrothermal upgrading of biosugars.

Regulating the Pore Structure and Heteroatom Doping of Soybean Straw Carbon Based on a Bifunctional Template Method for the High-Performance Carbon Supercapacitor.

The previous research addressed the waste problem of agriculture and forestry residues by exploring the efficient utilization of liquefied soybean straw in supercapacitor. The structures of the liquefied soybean straw were controlled by coupling microwave hydrothermal treatment with carbonization under the influence of a C3N4 bifunctional template. What's more, C3N4 could effectively regulate the pore structures and provide an effective N active site of carbon materials C3N4. The obtained N-SLR Carbon-700 possess a specific surface area of up to 1593.7 m2 g -1, and the pore size is mainly concentrated in the range of 1.8-2.5 nm, providing efficient ions transmission channels and storage space. Its specific capacitance is up to 261.5 F g-1 (current density of 0.5 A g-1), and the capacity retention is 74.04 % when the current density is expanded by 20 times. In the two-electrode system, the energy density of N-SLR Carbon-700 could reach to 31.3 W h kg-1 at a power density of 360 W kg-1, as well as the energy surface density is maintained at 69 % when the power density is increased by a factor of 20. This work enhances effectively the charging and discharging stability and capacitance value of carbon-based supercapacitor.

Effects of Preheating and Alkaline Roasting on Gangue Removal During the Alkaline Hydrothermal Treatment of Low-Grade Iron Ores

Effects of Preheating and Alkaline Roasting on Gangue Removal During the Alkaline Hydrothermal Treatment of Low-Grade Iron Ores

Removal of Methylene Blue from Aqueous Solution through Adsorption and Heterogeneous Fenton Reaction using Iron Oxides Produced by Different Methods

Direct discharge of industrial wastewater containing dyes into water bodies has contributed to the scarcity of drinking water. As environmental legislation becomes stricter, it is increasingly important to develop efficient methods for wastewater treatment. Traditional methods are commonly costly and have limited efficiency. This study aimed to prepare iron oxides via different synthetic routes and evaluate the effect of synthesis method on the efficiency of these materials as adsorbents and heterogeneous Fenton catalysts for the removal of methylene blue from aqueous solution. Iron oxides were synthesized by non-hydrolytic sol–gel (NHSG) and co-precipitation (CP) methods, followed by hydrothermal treatment for different times. CP oxides demonstrated high efficiency in dye adsorption, particularly the sample subjected to hydrothermal treatment for 6 h (CP-R6). This sample achieved 94.04% removal in 120 min. NHSG materials, by contrast, were less effective. The CP series of materials showed superior catalytic performance in heterogeneous Fenton experiments, with CP-R6 reaching 98.79% decolorization in 240 min. X-ray diffraction analysis indicated that iron oxides were composed of crystalline hematite and maghemite. Scanning electron microscopy revealed that CP materials were more porous and homogeneous than NHSG materials. The results demonstrated the efficiency of the developed iron oxides in removing methylene blue via adsorption and heterogeneous Fenton degradation and clarified how synthesis method influences adsorptive and catalytic properties.

Valorization of nopal wastes to produce quantum dots: optimizing synthesis and exploring in smart textile applications

Quantum carbon dots (QCDs) were efficiently synthesized from post-extraction residues generated during nopal fabric production using a hydrothermal treatment. These QCDs were applied to nopal fabrics, enhancing their UV solar radiation absorption. The synthesized QCDs exhibited fluorescence emissions in the 200–300 nm range. An eco-friendly dispersion was created by incorporating QCDs into TiO2 for use in smart textiles, which underlines our commitment to maintaining a sustainable process. Bright and fluorescent patterns were successfully applied to commercial and nopal fabrics using a spray printing technique. Additionally, the QCDs demonstrated pH-sensitive color changes, paving the way for practical applications. This work represents an initial step towards a circular economy by utilizing residues from nopal fabric production to synthesize quantum dots, which may be employed in smart textiles applications with UV absorption capabilities.

Tailoring of Time for Hydrothermal Synthesis of 2D MoSe2 with Enhanced Adsorption and Electro‐Catalytic Efficiency for Applications in Self‐Cleaning and Hydrogen Energy Generation

AbstractMolybdenum diselenide (MoSe2), a 2D layered transition metal dichalcogenide, has garnered significant scientific research interest for its catalytic and electrocatalytic activities. Here, a straightforward hydrothermal procedure is used to synthesize MoSe2 nanosheets (NSs) and focus on their adsorption capabilities and hydrogen evolution reaction (HER) activity. The MoSe2 NSs which are synthesized by 12 h of hydrothermal treatment found to exhibit the highest adsorption capacity of 91.67 mg g−1. The kinetics of the adsorption process have been found to follow the pseudo‐second‐order model, signifying chemisorption and multilayer adsorption as described by the Freundlich isotherm. The thermodynamic analysis further suggests that the adsorption proceeds by endothermic and spontaneous mechanisms. The self‐cleaning property of the adsorbent is demonstrated by degrading the dye on the adsorbent‐coated cotton fabric. The sample created using a 12 h hydrothermal method has been shown to have a minimal Tafel slope of 58 mV dec−1. It also shows excellent HER activity at low over‐potential and possesses long‐term durability. The dual functionality of MoSe2 NSs in both adsorption and electrocatalytic activity highlights their potential for application in environmental remediation and renewable energy production.

UV and blue light cut-off filters using phosphorus doped carbon quantum dots extracted from raw egg yolk

Abstract Using raw egg yolk and phosphoric acid, a simple hydrothermal treatment for synthesizing carbon quantum dots (CQDs) has been developed for the manufacture of UV and blue light-blocking filters. Several samples with different doping ratios of phosphoric acid were prepared. Namely: reference (REF.), 25%, 50%, 75% and 100%. The synthesized CQDs were embedded in polyvinyl alcohol (PVA) to produce blocking-light films with desired optical properties. Six films were prepared, one of which was PVA alone, and the other five samples were the prepared CQDs, with different phosphorus doping levels, mixed with PVA in a 1:1 ratio. We aimed to test the ability of these films to block ultraviolet rays and blue light. The experimental results revealed that the prepared films were able to block the blue light, emitted from a 450 nm blue LED, with blocking ratios of 7%, 17.5%, 27%, 30%, 37% and 70% for the films: PVA alone, REF., 25%, 50%, 75% and 100%, respectively. Moreover, it was found that these phosphorus-doped CQDs films can prevent destructive UV light with substantial value reaching 86%. These results suggest that carbon dots, derived from raw egg yolk, can be effectively applied to block harmful UV and blue lights.

Enhancing black soldier fly larval production from sugarcane bagasse through hydrothermal, enzymatic, and microbial treatment

Enhancing black soldier fly larval production from sugarcane bagasse through hydrothermal, enzymatic, and microbial treatment

Physical, textural, and sensory characteristics of gluten-free cupcakes developed with native and modified by hydrothermal treatment green plantain flours.

Gluten-free diets are characterized by lower nutritional quality. The use of green plantain flour in gluten-free formulations appears as an alternative to overcome this deficiency, considering that green plantains have a relevant content of bioactive compounds, dietary fiber, including resistant starch. The objective of this work was to evaluate the effect of the addition of native and modified by hydrothermal treatment green plantain whole flours in the form of gluten-free cupcakes. The density, yield, and microstructure of the dough, specific volume (SV), height, crumb analysis, color, texture, and sensory acceptability of the cupcakes were evaluated. Partial replacement (40%) of rice flour by native and modified flours produced darker, redder cupcakes, less yellowish and with less color intensity. Sensory analysis revealed higher acceptance for cupcakes with native and modified flours, compared to the control, for appearance, flavor, texture, aroma, and overall acceptance. The native flour was the most viable option, as the cupcake produced with it showed the best values for hardness and chewiness, without changing elasticity and SV, in addition to superior sensory acceptance than the control and similar to cupcakes with other modified flours. PRACTICAL APPLICATION: Pursuing to meet the market demand for gluten-free products, with the cake being one of the most requested products in this market, and taking in account that green banana, from different cultivars, has gained interest for the production of flours. The production of flour and bakery products is of great interest to the food industry, not only because of its flavor and properties but also due to the economic and sustainable viability of producing whole green plantain flour with the potential for application, promoting diversification and innovation in the gluten-free functional products market.

Fluorine-doped carbon dots decorated on iron-cobalt selenide nanosheets as superior electrocatalysts for oxygen evolution in seawater

Developing oxygen evolution reaction (OER) catalysts that can efficiently and stably operate at high current densities in seawater electrolysis is urgently demanded but challenging. In this study, selenium-vacancies-rich iron-cobalt selenide nanosheets (FeCoSe-VSe) decorated with fluorine-doped carbon dots (FCDs) are rationally designed and prepared on nickel foams (NF) through the successive processes of hydrothermal treatment and selenization. Benefiting from the large accessible surface area and abundant active sites provided by FCDs and selenium vacancy defects, as well as the coupled interface between FCDs and FeCoSe-VSe that optimizes the oxygen adsorption energy and accelerates the kinetic process, the FCDs/FeCoSe-VSe/NF composite exhibits excellent OER catalytic activities with a low overpotential of 258 mV at a current density of 200 mA cm−2 in 1 M KOH and a small Tafel slope of 34.7 mV dec–1. In the electrolytes of simulated and natural seawater, the overpotentials of the FCDs/FeCoSe-VSe/NF electrode are slightly higher, measured to be 264 and 297 mV, respectively. More profoundly, the introduction of FCDs enhances the corrosion resistance of the catalyst in alkaline electrolytes, ensuring the long-term stability. This work offers a guidance to improve the electrochemical performances of catalysts for high-efficiency seawater oxidation.