Search Results (118)

A facile and versatile strategy to obtain NPs@ZnAlO nanocomposite materials, comprising controlled-size nanoparticles (NPs) within a ZnAlO matrix is reported. The mono-(Au, Ni) and bimetallic (Ni-Au) NPs serving as an active phase were prepared by the polyol-alkaline method, while the ZnAlO support was obtained via the thermal decomposition of its corresponding layered double hydroxide (LDH) precursors. X-ray diffraction (XRD) patterns confirmed the successful fabrication of the nanocomposites, including the synthesis of the metallic NPs, the formation of LDH-like structure, and the subsequent transformation to ZnO phase upon LDH calcination. The obtained nanostructures confirmed the nanoplate-like morphology inherited from the original LDH precursors, which tended to aggregate after the addition of gold NPs. According to the UV-Vis spectroscopy, loading NPs onto the ZnAlO support enhanced the light absorption and reduced the band gap energy. ATR-DRIFT spectroscopy, H₂-TPR measurements, and XPS analysis provided information about the functional groups, surface composition, and reducibility of the materials. The catalytic performance of the developed nanostructures was evaluated by the photodegradation of bisphenol A (BPA), under simulated solar irradiation. The conversion of BPA over the bimetallic Ni-Au@ZnAlO reached up to 95% after 180 min of irradiation, exceeding the monometallic Ni@ZnAlO and Au@ZnAlO catalysts. Its enhanced activity was correlated with good dispersion of the bimetals, narrower band gap, and efficient charge carrier separation of the photo-induced e⁻/h⁺ pairs. Full article

Maritime corrosion is a global problem often retarded through protective coatings containing corrosion inhibitors (CIs). ZnAl layered double hydroxides (LDH) have been used to immobilize CIs, which can reduce their early leaching and, thus, foster long-term corrosion protection. However, the environmental behavior of these nanomaterials remains largely unknown, particularly in the context of global changes. The present study aims to assess the environmental behavior of four anti-corrosion nanomaterials in an ocean acidification scenario (IPCC SSP3-7.0). Three different concentrations of the nanostructured CIs (1.23, 11.11, and 100 mg L⁻¹) were prepared and maintained at 20 °C and 30 °C in artificial salt water (ASW) at two pH values, with and without the presence of organic matter. The nanomaterials’ particle size and the release profiles of Al³⁺, Zn²⁺, and anions were monitored over time. In all conditions, the hydrodynamic size of the dispersed nanomaterials confirmed that the high ionic strength favors their aggregation/agglomeration. In the presence of organic matter, dissolved Al³⁺ increased, while Zn²⁺ decreased, and increased in the ocean acidification scenario at both temperatures. CIs were more released in the presence of humic acid. These findings demonstrate the influence of the tested parameters in the nanomaterials’ environmental behavior, leading to the release of metals and CIs. Full article

In this study, a novel adsorbent was developed by synthesizing Zn-Al layered double hydroxide (LDH) incorporated with silver nanoparticles (Ag-NPs), and its effectiveness in bromide removal from aqueous solutions was systematically evaluated. The X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) analyses confirmed the integration of Ag-NPs within the LDH, ensuring uniform chemical composition and structural integrity. A series of controlled batch trials, each varying a single parameter (adsorbent dose, contact time, or temperature) confirmed that over 95% of bromide (initially 5320 μg/L) was removed under optimized conditions. LDH/Ag-NPs exhibited superior performance, with kinetics well described by a second-order reaction model. Thermodynamic analysis confirmed the spontaneous and exothermic nature of bromide adsorption, with ΔG° values ranging from −2.03 to −0.73 kJ/mol as the temperature increased from 22 °C to 52 °C. In continuous-flow experiments, packed-bed column tests illustrated that LDH/Ag-NPs maintained more effective bromide removal than LDH alone over extended periods. Conductivity measurements further supported this enhancement, with LDH/Ag-NPs reducing final conductivity to 139 µS/cm, compared to 212 µS/cm for LDH. Furthermore, this study revealed the notable antimicrobial activity of LDH/Ag-NPs, as evidenced by a significant reduction in bacterial growth compared to LDH alone, highlighting its dual functionality for both bromide adsorption and water disinfection. Overall, the incorporation of Ag-NPs into LDH offers a promising strategy for developing multifunctional and sustainable water treatment systems. Full article

The rapid pace of industrialization has led to widespread heavy metal contamination in water and soil, highlighting the need for efficient remediation strategies. Among various approaches, adsorption has proven to be an effective method for treating contaminated environments. Layered double hydroxide (LDH) is frequently used in such applications. However, its adsorption efficiency remains limited. In this study, glutamic acid diacetate tetrasodium salt (GLDA) was incorporated into ZnAl LDH via a straightforward co-precipitation and ion exchange method, yielding a modified material, GLDA-LDH, which was subsequently applied for the adsorption of Pb(II) and Cd(II). Adsorption behavior was investigated through kinetic and isothermal models, with results indicating that the process followed pseudo-second-order kinetics and fit well with the Langmuir isotherm, suggesting chemisorption onto monolayer surface. The maximum adsorption capacities reached 219.2 mg/g for Pb(II) and 121.9 mg/g for Cd(II). Furthermore, GLDA-LDH exhibited a strong retention capability for metal ions with minimal desorption and remained effective in the presence of hard water and contaminated soils. XPS analysis revealed distinct interaction mechanisms; surface oxygen and carboxyl groups played a key role in Pb(II) adsorption, whereas nitrogen coordination was involved in Cd(II) uptake. These results point to the potential of GLDA-LDH as a reliable material for addressing heavy metal pollution and provide insights into the design of enhanced LDH-based adsorbents. Full article

Layered double hydroxide (LDH)-derived mixed oxides offer a promising approach for CO₂ hydrogenation to light hydrocarbons. Herein, we explore the impact of various transition metals (X = Mn, Co, Cu, and Zn) incorporated into the M-Al or M-(Al+Fe) LDH structures, with the aim of exploring possible synergistic effects. Structural and compositional analyses reveal that an abundance of Fe over Al (Fe/Al ratio ~4) leads to the formation of mixed oxide crystalline phases attributed to CoFe₂O₄, CuFe₂O₄, and ZnFe₂O₄. Catalytic evaluation results demonstrate that the X-Al LDH-derived oxides exhibit high CO₂ conversion yet are selective to CH₄ or CO. In contrast, Fe incorporation shifts selectivity toward higher hydrocarbons. Specifically, the yield to higher hydrocarbons (C₂⁺) follows the order Ζn-Al-Fe > Cu-Al-Fe > Mn-Al-Fe > Co-Al-Fe >> Mn-Al, Co-Al, Zn-Al, Cu-Al, highlighting the pivotal role of Fe. Moreover, Zn-Al-Fe and Mn-Al-Fe catalysts have been shown to be the most selective towards light olefins. Zn-based systems also exhibit high thermal and structural stability with minimal coke formation, whereas Co-, Cu-, and Mn-based catalysts, when modified with Fe, experience increased carbon deposition or structural changes that may impact long-term stability. This work provides insights into the combined role of Fe and a second transition metal in LDHs for modulating catalytic activity, phase transformations, and stability, underscoring the need for further optimization to balance selectivity and catalyst durability in CO₂ hydrogenation applications. Full article

This study aimed to synthesize a multicationic hydrotalcite and transform it into mixed oxide nanostructures (ZnO/TiO₂/CeO₂/Al₂O₃, referred to as MixO) to serve as a heterogeneous photocatalyst for degrading various pollutants, including methylene blue (MB), methyl orange (MO), paracetamol (PA), and paraquat (PQ). The hydrotalcite was synthesized via an ultrasound-assisted method and calcined at 700 °C to obtain the corresponding mixed metal oxide. A comprehensive characterization of both the multicationic hydrotalcite (MC-LDH) and the mixed metal oxides (MixO) was performed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), N₂ adsorption–desorption, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and pH_PZC analysis. The MixO sample exhibited an optical bandgap of 3.19 eV. Photocatalytic performance was evaluated during 240 min of UV irradiation, demonstrating high degradation efficiencies attributable to the synergistic interactions among ZnO, TiO₂, and CeO₂. Degradation efficiencies reached 99.3% for MO and 95.2% for MB, while PA and PQ showed moderate degradation rates of 60% and 15%, respectively. The degradation kinetics of all pollutant compounds followed the Langmuir–Hinshelwood model. Additionally, the MixO catalyst maintained consistent performance over four consecutive degradation cycles, highlighting its reusability and stability. These findings underscore the potential of MixO mixed oxide nanostructures as practical and recyclable photocatalysts for environmental remediation, particularly in wastewater treatment applications. Full article

Heavy metal cations such as Ag⁺, Pb²⁺, and Hg²⁺ can accumulate in living organisms, posing severe risks to biological systems, including humans. Therefore, removing heavy metal cations from wastewater is crucial before discharging them to the environment. However, trace levels and high-capacity removal of the heavy metals remain a critical challenge. This work demonstrates the synthesis and characterization of [Mo₂S₁₂]²⁻ intercalated cobalt aluminum-layered double hydroxide, CoAl―Mo₂S₁₂―LDH (CoAl―Mo₂S₁₂), and its remarkable sorption properties for heavy metals. This material shows high efficiency for removing over 99.9% of Ag⁺, Cu²⁺, Hg²⁺, and Pb²⁺ from 10 ppm aqueous solutions with a distribution constant, K_d, as high as 10⁷ mL/g. The selectivity order for removing these ions, determined from the mixed ion state experiment, was Pb²⁺ < Cu²⁺ ≪ Hg²⁺ < Ag⁺. This study also suggests that CoAl―Mo₂S₁₂ is not selective for Ni²⁺, Cd²⁺, and Zn²⁺ cations. CoAl―Mo₂S₁₂ is an efficient sorbent for Ag⁺, Cu²⁺, Hg²⁺, and Pb²⁺ ions at pH~12, with the removal performance of both Ag⁺ and Hg²⁺ cations retaining > 99.7% across the pH range of ~2 to 12. Our study also shows that the CoAl―Mo₂S₁₂ is a highly competent silver cation adsorbent exhibiting removal capacity (q_m) as high as ~918 mg/g compared with the reported data. A detailed mechanistic analysis of the post-treated solid samples with Ag⁺, Hg²⁺, and Pb²⁺ reveals the formation of Ag₂S, HgS, and PbMoO₄, respectively, suggesting the precipitation reaction mechanism. Full article

Converting CO₂ and green hydrogen into products such as methane and methanol not only has a negative carbon effect, but also stores renewable energy into energy chemicals. This represents a promising route for hydrogen energy storage technologies. The hydrogenation of CO₂ to methane and methanol, which represent strongly exothermic reactions, are thermodynamically favored at low temperatures. However, the inherent inertness of CO₂ makes it difficult to activate CO₂ at low temperatures. Both reactions face the challenge of activating CO₂ at low temperature, so catalysts exhibiting high activity under such conditions are a critical need. Layered double hydroxides (LDHs) have attracted considerable interest owing to their regular layered structure and uniform dispersion of multiple metallic components. However, there are few studies on the same effects of promoters over LDHs-derived catalysts. Here, we investigated the same effects of promoters on two LDHs-derived catalysts in different CO₂ hydrogenation reactions to illustrate the effects of promoters on facilitating low-temperature CO₂ activation in LDHs-derived catalysts. By adding promoters Fe and Mn to the catalysts NiAl-Fe and CuZnAl-Mn, the crystal lattices were expanded, surface areas were increased 38% and 25%, and the reduction temperatures were decreased to 97 °C and 10 °C, respectively. These promoters significantly enhanced the CO₂ adsorption and activation of the catalysts NiAl-Fe and CuZnAl-Mn. The methanation catalyst NiAl-Fe achieved a CO₂ conversion of 80.8% at 200 °C and 2 MPa, while the methanol synthesis catalyst CuZnAl-Mn exhibited a CO₂ conversion of 21.3% and a methanol selectivity of 61.8% under the conditions of 250 °C and 3 MPa. The influence of the LDHs precursors’ structure and the addition of promoters Fe and Mn on the catalytic performance were studied by XRD, N₂ adsorption–desorption, H₂-TPR, H₂-TPD, and CO₂-TPD. Full article

In this work, the coprecipitation approach was successfully used to create Mg-Al hydrotalcite-like inhibitors modified with varying amounts of Zn, and their characteristics were assessed. The findings indicate that the flame retardancy of Mg-Al hydrotalcite (MgAl-LDHs) is not significantly affected by Zn content. By adding MgAl-LDHs, the temperature at which the exothermic reaction started to occur was raised from 146.2 °C to 193.6 °C, according to the test of spontaneous combustion tendency. In the excavation route, the utility model can serve as a temporary fire prevention and extinguishment tool. Furthermore, the analysis of the functional group changes during the reaction was conducted using FTIR. After applying MgAl-LDHs, the oxidation of organic groups on the coal surface was clearly prevented, indicating that the inhibitor had a substantial flame-retardant effect on coal. In conclusion, this work creates a material that resembles hydrotalcite and is easy to use, inexpensive, and effective in preventing coal from spontaneously combusting. Full article

This study focuses on the synthesis of a novel layered double hydroxide and its application in two environmental remediation processes. Graphene oxide, a two-dimensional material, has potential applications in this field. However, its tendency to agglomerate restricts its usability. Our objective was to increase the morphology and performance of layered double hydroxide (LDH) by combining GO with hydrotalcite. The LDH/GO nanohybrids were utilized as photocatalysts for the degradation of methylene blue (MB) dye and were investigated as sorbents for acid red (A.R) dye in water. In order to achieve this objective, ZnAl-NO₃ LDH was synthesized using the co-precipitation method, with a Zn:Al ratio of ~3. Subsequently, the LDH was intercalated with varying ratios of as-received graphene oxide. An array of analytical techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) measurements, N₂ physisorption, scanning electron microscopy–energy-dispersive X-ray analysis (SEM-EDX), and diffuse reflectance UV–vis spectra (DR UV-vis), were employed to examine the physicochemical properties of the synthesized LDH. These techniques confirmed that the obtained material is zinc-aluminum hydrotalcite intercalated with GO. The addition of graphene oxide (GO) to the layered double hydroxide (LDH) structure improved the performance of the hydrotalcite. As a result, the composite ZnAl-LDH-10 shows significant potential in the field of photocatalytic degradation of MB. Additionally, the incorporation of GO enhanced the absorption of light in the visible region of the spectra, leading to improved elimination of A.R compared to LDH without GO or other ratios of GO. Full article

In this study, the synthesis of hybrid photocatalysts of Zn-Al-In mixed metal oxides were activated by using visible light, derived from Zn-Al-In layered double hydroxide (ZnAlIn-LDH), and these nanocomposites demonstrated high efficiency for photocatalytic H₂ production under UV light when using methanol as a sacrificial agent. The most active photocatalytic material produced 372 μmol h⁻¹ g⁻¹ of H₂. The characterization of these materials included X-ray diffraction (DRX), infrared spectroscopy (FTIR), X-ray fluorescence spectroscopy (XRF), X-ray spectroscopy (XEDS), scanning electron microscopy analysis (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy, and N₂- physisorption. In addition, the materials were characterized by photoelectrochemical techniques to explain the photocatalytic behavior. Subsequently, the photocatalytic performance for the water-splitting reactions under visible irradiation was evaluated. The ZnAlIn-MMOs with an In/(Al + In) molar ratio of 0.45 exhibited the highest photocatalytic activity in tests under visible light, attributed to the efficient separation and transport of photogenerated charge carriers originating from the new nanocomposite. This discovery indicates a method for developing new types of heteronanostructured photocatalysts which are activated by visible light. Full article

Layered double hydroxides (LDHs) and their derived mixed oxides are emerging as a promising class of biocompatible inorganic lamellar nanomaterials. The detailed structure and textural characteristics of the synthesized LDH-based materials were examined using X-ray diffraction, Fourier transform infrared spectroscopy, and N₂ adsorption/desorption isotherm. This study explored the removal efficiency of pharmaceutical tolperisone hydrochloride (TLP), as well as the herbicides quinmerac (QUI) and clomazone (CLO) from water, using dried and calcined LDH-based photocatalysts under simulated solar irradiation and UV irradiation. A higher removal efficiency was observed using UV irradiation, for all substrates. The most effective removal was achieved using ZnAl photocatalysts thermally treated at 100 °C (ZnAl 100) and 500 °C (ZnAl 500). The highest removal rates were observed in the TLP/ZnAl 100 and QUI/ZnAl 100 systems, achieving ~79% and ~86% removal after 75 min of treatment under UV. In contrast, the CLO/ZnAl 100 and CLO/ZnAl 500 systems achieved ~47% removal of CLO. Furthermore, this study investigated the role of reactive species to elucidate the mechanisms of photodegradation under UV. It was found that in the degradation of TLP and QUI in the presence of ZnAl 100 and ZnAl 500, the superoxide anion radical played the most important role. Full article

This study presents a vanadate-exchanged Zn-Al layered double hydroxide (LDH) coating on a ZX21 Mg alloy (Mg-2.15 wt%Zn-0.97 wt%Ca) by electrodeposition and immersion anion-exchange post-treatment. With the prepared vanadate-exchanged electrodeposited Zn-Al LDH coating, the corrosion resistance of the ZX21 Mg alloy improves with a decrease in the corrosion current density from 62.4 μA/cm² to 3.32 μA/cm². The fabricated vanadate-exchanged electrodeposited Zn-Al LDH coating contains complex anions in the interlayers, including mainly nitrate (NO₃⁻), carbonate (CO₃²⁻), and different vanadates. The coating not only serves as a physical barrier on the ZX21 Mg alloy but also absorbs chloride ions in the environment through anion exchange and inhibits corrosion with the reduction of the interlayer vanadates. Furthermore, the vanadates can also be released into the damaged area of the coating. Full article

This article presents the results of research on the growth kinetics, microstructure (SEM/EDS/XRD), and corrosion behavior of Zn-5Al coatings obtained using a high-temperature hot dip process on B500B reinforcing steel. The corrosion resistance of the coatings was determined using the neutral salt spray (NSS) test (EN ISO 9227). Based on chemical composition tests in micro-areas (EDS) and phase composition tests (XRD), corrosion products formed on the coating surface after exposure to a corrosive environment containing chlorides were identified. In the outer layer of the coating, areas rich in Zn and Al were found, which were solid solutions of Al in Zn (α), while the diffusion layer was formed by a layer of Fe(Al,Zn)₃ intermetallics. The growth kinetics of the coatings indicate the sequential growth of the diffusion layer, controlled by diffusion in the initial phase of growth, and the formation of a periodic layered structure with a longer immersion time. The NSS test showed an improved corrosion resistance of reinforcing bars with Zn-5Al coatings compared to a conventional hot-dip-galvanized zinc coating. The increase in corrosion resistance was caused by the formation of beneficial corrosion products: layered double hydroxides (LDH) based on Zn²⁺ and Al³⁺ cations and Cl⁻ anions and simonkolleite—Zn₅(OH)₈Cl₂·H₂O. Full article

Acid–base M²⁺MgAlO and M²⁺AlO mixed oxides (where M²⁺ = Mg, Cu, Co, Zn, and Ni) were obtained by thermal decomposition of the corresponding layered double hydroxide (LDH) precursors and used as catalysts for cyclohexanol and benzaldehyde condensation under solvent-free conditions. The catalysts were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), and temperature-programmed desorption of CO₂ (TPD-CO₂). Gas chromatography–mass spectroscopy (GC/MS) was used for the identification and quantification of the product mixtures. In the reaction of cyclohexanol and benzaldehyde on M²⁺MgAlO and MgAlO catalysts, a 2,6-dibenzylidene-cyclohexanone was obtained as the main product as a result of consecutive one-pot dehydrogenation of cyclohexanol to cyclohexanone and subsequent Claisen–Schmidt condensation. In the reaction mixture obtained in the presence of NiAlO, CoAlO, and ZnAlO catalysts, a cyclohexyl ester of 6-hydroxyhexanoic acid was detected together with the main product. This is most likely a by-product obtained after the oxidation, ring opening, and subsequent esterification of the cyclohexanol. Full article