Synthesis Of Layered Double Hydroxides Research Articles

Hydrothermally Synthesized ZnCr- and NiCr-Layered Double Hydroxides as Hydrogen Evolution Photocatalysts.

The layered double hydroxides (LDHs) of transition metals are of great interest as building blocks for the creation of composite photocatalytic materials for hydrogen production, environmental remediation and other applications. However, the synthesis of most LDHs is reported only by the conventional coprecipitation method, which makes it difficult to control the catalyst's crystallinity. In the present study, ZnCr- and NiCr-LDHs have been successfully prepared using a facile hydrothermal approach. Varying the hydrothermal synthesis conditions allowed us to obtain target products with a controllable crystallite size in the range of 2-26 nm and a specific surface area of 45-83 m2∙g-1. The LDHs synthesized were investigated as photocatalysts of hydrogen generation from aqueous methanol. It was revealed that the photocatalytic activity of ZnCr-LDH samples grows monotonically with the increase in their average crystallite size, while that of NiCr-LDH ones reaches a maximum with intermediate-sized crystallites and then decreases due to the specific surface area reduction. The concentration dependence of the hydrogen evolution activity is generally consistent with the standard Langmuir-Hinshelwood model for heterogeneous catalysis. At a methanol content of 50 mol. %, the rate of hydrogen generation over ZnCr- and NiCr-LDHs reaches 88 and 41 μmol∙h-1∙g-1, respectively. The hydrothermally synthesized LDHs with enhanced crystallinity may be of interest for further fabrication of their nanosheets being promising components of new composite photocatalysts.

Efficient phosphate removal by Mg-La binary layered double hydroxides: synthesis optimization, adsorption performance, and inner mechanism.

Layered double hydroxides (LDH) hold great promise as phosphate adsorbents; however, the conventional binary LDH exhibits low adsorption rate and adsorption capacity. In this study, Mg and La were chosen as binary metals in the synthesis of Mg-La LDH to enhance phosphate efficient adsorption. Different molar ratios of Mg to La (2:1, 3:1, and 4:1) were investigated to further enhance P adsorption. The best performing Mg-La LDH, with Mg to La ratio is 4:1 (LDH-4), presented a larger adsorption capacity and faster adsorption rate than other Mg-La LDH. The maximum adsorption capacity (87.23 mg/g) and the rapid adsorption rate in the initial 25 min of LDH-4 (70 mg/(g·h)) were at least 1.6 times and 1.8 times higher than the others. The kinetics, isotherms, the effect of initial pH and co-existing anions, and the adsorption-desorption cycle experiment were studied. The batch experiment results proved that the chemisorption progress occurred on the single-layered LDH surface and the optimized LDH exhibited strong anti-interference capability. Furthermore, the structural characteristics and adsorption mechanism were further investigated by SEM, BET, FTIR, XRD, and XPS. The characterization results showed that the different metal ratios could lead to changes in the metal hydroxide layer and the main ions inside. At lower Mg/La ratios, distortion occurred in the hydroxide layer, resulting in lower crystallinity and lower performance. The characterization results also proved that the main mechanisms of phosphate adsorption are electrostatic adsorption, ion exchange, and inner-sphere complexation. The results emphasized that the Mg-La LDH was efficient in phosphate removal and could be successfully used for this purpose.

Application of cobalt-cerium-iron ternary layered double hydroxide for extraction of perfluorooctane sulfonate followed by HPLC-MS/MS analysis

Herein, Ce-doped CoFe layered double hydroxide (LDH), noted as CoCeFe ternary LDH, was prepared using the co-precipitation route. Prosperous synthesis of CoFe LDH and successful partial replacement of iron cations with cerium cations in CoCeFe ternary LDH were confirmed by X-ray diffraction patterns, energy-dispersive X-ray spectroscopy, and elemental dot-mapping images. Nanosheet morphology was recognized for both CoFe LDH and CoCeFe ternary LDH from scanning electron microscopy and transmission electron microscopy micrographs. In the following, a dispersive solid phase extraction (DSPE) method was developed using the synthesized CoCeFe ternary LDH as a sorbent for extracting perfluorooctanesulfonic acid (PFOS) from wastewater samples. For the selective analysis of PFOS, high-performance liquid chromatography-tandem mass spectroscopy (HPLC-MS/MS) in multiple reaction monitoring mode was used. Analytical parameters such as the limit of detection equal to 0.02 μg/L, with a linear range of 0.05–300 μg/L, the limit of quantification equal to 0.05 μg/L, and an enrichment factor equal to 23.3 were achieved for PFOS at the optimized condition (sorbent: 5 mg of CoCeFe ternary LDH, eluent type and volume: 150 μL mobile phase, pH: 3, adsorption time: 3 min, and desorption time: 5 min). The developed strategy for the analysis of PFOS was tested in real wastewater samples, including copper mine and petrochemical wastewater. The amount of analytes in real samples was calculated using the standard addition method, and good relative recovery in the range of 86%–105% was obtained. The main novelty of this research is the application of CoCeFe ternary LDH to extract the PFOS from wastewater using the DSPE method for determination by HPLC-MS/MS.

Tailored thymoquinone intercalated Layered Double Hydroxide (LDH) nanocomposites to accelerate mineralization for enhanced osteogenesis

The tunable nature of two-dimensional nanostructured Layered Double Hydroxides [LDH] and their effective intercalation ability with biomolecules make them inevitable functional hybrid materials for versatile biomedical applications. In an attempt to meet the limitations in existing bone reconstruction practice, the present work reports the synthesis of zinc and iron-based LDH [Zn-Fe LDH] and its subsequent intercalation with thymoquinone [TQ-Zn-Fe LDH] to augment osteoblastic differentiation and proliferation for accelerated bone mineralization. Structural studies depicted the polycrystalline and amorphous nature of ZnFe LDH and TQ-Zn-Fe LDH respectively. The biocompatible nature of LDHs was proven by negative cytotoxicity, cell adhesion, and proliferation assays studied in MG-63 cell lines. Gene expression studies of the nanocomposites showed a fold change of 5–10 in osteoblastic differentiation and proliferation. However, TQ-Zn-Fe LDH treated cells showed significantly higher protein translation levels of osteogenesis markers and elevated alkaline phosphatase secretion and calcium deposition on day 21, confirming their osteogenic efficiency. Thus, acquired results speculate the osteogenic potential of thymoquinone intercalated TQ-Zn-Fe-LDH to meet the limitations in bone reconstruction practice.

Heterostructures by Templated Synthesis of Layered Double Hydroxide to Modulate the Electronic Structure of Nickel Sites for a Highly Efficient Oxygen Evolution Reaction

The design and development of highly efficient electrocatalysts for oxygen evolution reaction (OER) are critical for renewable energy generation. Ni‐based electrocatalysts are widely used in the water electrolysis process. In this work, heterostructure consisting of selenides and layered double hydroxides (LDH) named (Co, Ni)Se4@NiFe‐LDH, are prepared by an LDH‐based strategy, in which the electronic structure of Ni active sites is regulated by interfacial electron interaction. The (Co, Ni)Se4@NiFe‐LDH shows an optimized charge distribution of Ni sites and excellent catalytic activity. The effective charge modulation results in lowering the energy barrier of OOH* intermediate formation and adequate adsorption strength of the intermediates on Ni‐active sites, which improves the kinetics of OER. Specifically, the (Co, Ni)Se4@NiFe‐LDH only requires an overpotential of 237 mV to reach the current density of 10 mA cm−2 under alkaline conditions. The results of this work demonstrate that reasonable engineering of heterostructure is an effective strategy to improve the intrinsic property of OER electrocatalysts for water splitting.

Multifunctional Biocompatible Nanoparticles: Surface Modification and Synthesis of Layered Double Hydroxides for Biomedical Applications

Layered Double Hydroxides (LDHs) are considered versatile materials owing to their distinctive features resulting from the isomorphous substitution of metal cations, namely M(II) and M(III), inside their octahedral locations. The LDH layer structure is characterized by a balanced arrangement of exchangeable hydrated or solvated anions within the interlayer and outer regions. This arrangement gives rise to a two-dimensional heterostructure with an ABAB pattern. Various metal cations have a role in LDHs composition, leading to their classification as hydrocalumites and hydrotalcite. Pristine-LDHs that include diverse inorganic anions have shown significant potential in biological applications. These substances have been investigated for their potential use in many applications, including but not limited to antacids, vaccination adjuvants, etc. The attainment of monodispersity in the size of LDHs is of utmost importance for their efficacy in biomedicine. This research emphasizes that the potential of LDHs is contingent upon effectively resolving difficulties, including those associated with size polydispersity. This study suggests using Surface Modified and Synthesized Layered Double Hydroxides for Biomedical Applications (SMS-LDH-BMA). The present study presents a novel approach that incorporates various enhancements, such as a decreased hydrodynamic diameter of 44.6 nm, a zeta potential of -23.86 mV, a high encapsulation efficiency of 91.2%, a substantial drug loading capacity of 14.6%, a favorable cell viability of 96.44%, and a controlled release rate of GLIB at 3.73 μg/mL/min. These findings demonstrate the efficacy of SMS-LDH-BMA in tackling these obstacles and augmenting the drug delivery capabilities and biomedical applications of LDHs.

3D-printed solid phase microextraction fiber based on Co-Al layered double hydroxide nanosheets; application in determination of phenolic acids in fruit juice samples

3D printing technology has attracted great attention in various fields of science and technology. Application of this technology in manufacturing analytical tools is developing fast. High precision in manufacturing designed objects, fast production and low cost also green production approach by using biodegradable materials like polylactic acid is promising bright future in scientific researches. The development of new approaches in improving the functional groups of the surface of 3D printed objects in order to make 3D printed parts more functional with conventional 3D printed materials, causes the entry of many advanced materials in this field. In this study, a novel solid phase microextraction fiber was prepared based on Co-Al layered double hydroxide (LDH) nanosheets in-situ growth on 3D-printed aluminum-polylactic acid (PLA) composite and its application for determination of phenolic acids (PAs) including vanillic acid (VA), ferulic acid (FA), p-coumaric acid (p-CA), p-hydroxybenzoic acid (HBA), protocatechuic acid (PCA) and caffeic acid (CA) in fruit juice samples was investigated. The proposed fiber was prepared via a robust one-step hydrothermal synthesis of Co-Al LDH on an anodized 3D-printed Al-PLA fiber. Factors crucial for the extraction, including pH, extraction and desorption time and ionic strength were explored in detail. Under the optimal experimental conditions, for all PAs except PCA, LOD, LOQ and LDR were obtained as 0.03, 0.1 and 0.1–100.0 µgL−1, respectively. For PCA, LOD, LOQ and LDR were obtained as 0.15, 0.50 and 0.5–100.0 µgL−1, respectively.

Effect of fluorine content in layered double hydroxide catalyzing oxygen evolution

Layered double hydroxides (LDHs) have been extensively studied in OER owing to their unique advantages. The mechanism of the effect of NH4F, a common and essential structural guide in the synthesis of LDH, on LDH is relatively ambiguous. Therefore, the solvothermal process synthesized a series of FeCoNi LDHs with different fluorine contents. Physical and chemical characterizations show that the fluorine content regulates the synthesis process, morphology, and electronic structure of the catalysts. The optimal catalyst required 196 mV overpotential to reach 10 mA cm-2, with a Tafel slope of 22 mV dec-1, and stable operation at a current density of 100 mA cm-2 for more than 120 h. XPS analysis demonstrated that the F- ions leached gradually during the OER reaction, promoting the formation of high-valent intermediates at the Co active site to enhance the catalyst activity. This work contributes to the subsequent study of LDH modification and NH4F.

Metal organic framework derived NiCo layered double hydroxide anode aggregated with biomass derived reduced graphene oxide cathode: A hybrid device configuration for supercapattery applications

Metal-organic frameworks (MOFs), due to its exceptional characteristics like high specific surface area and design diversity, serve as an outstanding sacrificial template in forming layered double hydroxides (LDHs) for highly efficient electrodes in supercapattery devices. In this work, we have prepared bimetallic layered Nickel Cobalt LDH via in-situ etching of Co-ZIF, in different Nickel concentrations directly on Ni foam that enhances the interfacial contact between substrate and the material. The optimised NiCo LDH-2 sample exhibited remarkable electrochemical behaviour with fast electrolyte ion diffusion kinetics ideal for supercapattery device and delivered a high specific capacitance of 2567 Fg−1 at 1 Ag−1. Further, the supercapattery device assembled with Ni-Co LDH as anode and rGO derived from a sustainable source as cathode demonstrated an energy density of 21 Whkg−1, power density of 0.307 kWkg−1 and good cyclic stability with capacitance retention of 88.89 % along with coulombic efficiency of 90.58 % over 1500 cycles. This work proposes an effective approach for designing layered NiCo-LDH that can be further extended to the synthesis of other transition metal-derived LDH for supercapattery devices.

Quintinite: A Mg–Al-layered double hydroxide as an efficient amido black dye adsorbent

Through this work, we show the potency of Quintinite (Mg–Al-Layered Double Hydroxide with Mg/Al ratio ∼2) as an efficient toxic dye (Amido Black 10B) adsorbent. Our strategy involves a facile, scalable synthesis of Layered Double Hydroxide (LDH) with magnesium as divalent and aluminium as trivalent ions in Mg/Al ratio ∼2 that forms a layered structure of metal hydroxides balanced by anions which develops a net positive charge on the surface in an aqueous medium. Adsorption behaviour examined via UV–Visible Spectrometry showed rapid dye adsorption for low dye concentrations (∼99% in 2 min) and displayed a high adsorption capacity of 207 mg/g at higher dye concentrations. These adsorption results were one of the highest reported ever to date with quintinite or any pristine Mg–Al-LDH processed below 100 °C. The mesoporous adsorbent surface together with a net positive charge in an aqueous medium provided an additional advantage in possessing more active adsorbing sites on the adsorbent (Mg–Al-LDH). We attempt to unravel the fact that, the LDH with appropriate preparation conditions can deliver maximum efficiency without any additional modification.

Engineering organic-inorganic frameworks as functionalized coating with remarkable active sites for boosted durability of anti-corrosion protection

In the realm of material engineering, the emergence of layered double hydroxides (LDH) with their exceptional hierarchical arrangements has sparked immense interest, positioning them as promising contenders for avant-garde implementations. However, designing well-defined LDH-based anticorrosion systems with excellent activity and robust stability at the industrial grade remains a serious challenge in practical applications. In this vein, an interface engineering controlled by layer-by-layer protection strategy was applied to construct three-dimensional (3D) hybrid material grown on Mg alloy as a highly efficient functional anti-corrosive coating. The present work unveils a new chitosan (CS) Schiff-base nature-inspired network, crafted to transcend the capabilities of porous MgO coating through the application of pulsed plasma electrolysis (PPE). Moreover, an ingenious strategy is proposed, involving the direct synthesis of LDH, serving as an exemplary foundation to augment the electrochemical proficiency, thereby transforming it into a purposeful film that excels in electron transport. Guided by this fabrication strategy, it is found that the resulting architecture not only exposes enriched active sites with an outstanding performance but also exhibits exceptional stability. This work provides fresh insight into the design of advanced hybrid materials suggesting a promising avenue that is expected to support next-generation anti-corrosion engineering development.

Assessing the Adjuvant Effect of Layered Double Hydroxides (LDH) on BALB/c Mice.

The discovery and validation of new adjuvants are critical areas for vaccinology. Mineral materials (e.g., alum microparticles) have been used for a long time as adjuvants in human vaccine formulations. Nonetheless, the use of nanosized materials is a promising approach to diversify the properties of adjuvants. Nanoclays are potential adjuvants proposed by some research groups. However, their adjuvant mechanisms and safety have not been fully elucidated. Herein, we aimed at expanding the knowledge on the potential adjuvanticity of layered double hydroxide (LDH) nanoparticles by reporting a detailed method for the synthesis and characterization of LDHs and the adsorption of a model antigen (bovine serum albumin, BSA). LDHs varying in diameter (from 56 to 88 nm) were obtained, and an in vitro evaluation revealed that the LDHs are not inherently toxic. BSA was passively adsorbed onto the LDHs, and the immunogenicity in mice of the conjugates obtained was compared to that of free BSA and BSA co-administered with alum (Alum-BSA). The LDH-BSA conjugates induced a higher humoral response that lasted for a longer period compared with that of free BSA and Alum-BSA, confirming that LDH exerts adjuvant effects. The 56 nm LDH particles were deemed as the more efficient carrier since they induced a higher and more balanced Th1/Th2 response than the 88 nm particles. This study is a contribution toward expanding the characterization and use of nanoclays in vaccinology and justifies further studies with pathogen-specific antigens.

Smart Inhibition Action of Amino Acid-Modified Layered Double Hydroxide and Its Application on Carbon Steel.

Surface impregnation of concrete structures with a migrating corrosion inhibitor is a promising and non-invasive technique for increasing the lifetime of existing structures that already show signs of corrosion attack. The main requirement for inhibitors is their ability to diffuse the rebar at a sufficient rate to protect steel. The use of smart nanocontainers such as layered double hydroxides (LDH) to store corrosion inhibitors significantly increases efficiency by providing an active protection from chloride-induced corrosion. The addition of LDH to reinforced mortar can also improve the compactness and mechanical properties of this matrix. Here, we report the synthesis of a magnesium-aluminum LDH storing glutamine amino acid as a green inhibitor (labeled as Mg-Al-Gln), which can be used as a migrating inhibitor on mortar specimens. The corrosion behavior of the specimens was determined via electrochemical techniques based on measurements of corrosion potential and electrochemical impedance spectroscopy. A cell containing a 3.5% NaCl solution was applied to the mortar surface to promote the corrosion of embedded rebars. The specimens treated with Mg-Al-Gln presented an improved corrosion protection performance, exhibiting an increase in polarization resistance (Rp) compared to the reference specimens without an inhibitor (NO INH). This effect is a consequence of a double mechanism of protection/stimuli-responsive release of glutamine and the removal of corrosive chloride species from the medium.

Oriented self-assembly of anisotropic layered double hydroxides (LDHs) with 2D-on-3D hierarchical structure

Layered double hydroxides (LDHs) have been the subject of increasing research due to their unique 2D or 3D structures and promising applications. However, achieving precise control over their morphology and architecture has proven to be a significant challenge. In this work, we present an oriented self-assembly strategy for the synthesis of ultrathin 2D-on-3D CoNi-LDHs nanoflowers (NFs) at ambient temperature. Ex situ and in situ characterization techniques were employed to elucidate the formation process of the 2D-on-3D CoNi-LDHs hierarchical structure. The 2D nanosheets are composed of CoNi(OH)2 seeds that undergo rapid nucleation and growth. Under the influence of oriented attachment and Ostwald ripening, the 2D nanosheets continue to crystallize along the axial and radial directions, resulting in the formation of 2D-on-3D CoNi-LDH NFs. This unique 2D-on-3D LDHs structure possesses an ultrathin thickness of approximately 1.5 nm, nanopores with a diameter of approximately 3.8 nm, and a large surface area of approximately 154 m2/g. These properties manifest excellent energy-storage performance in supercapacitors. Our approach provides important insights into the precise synthesis of LDHs with a 2D-on-3D hierarchical structure. The synthesis of LDHs with well-defined structures is a significant challenge in materials science. Our work contributes to the advancement of this field and has the potential to facilitate the development of new, high-performance energy-storage devices.

Effect of Zn2Cr layered double hydroxide on photocatalytic hydroxylation of terephthalic acid and photodegradation of sodium diclofenac

Titanium dioxide has been widely used in traditional photocatalysis but layered double hydroxides (LDHs) based on Zn/Cr have attracted interest due to their semiconducting properties and tunable bandgap. The typical layered particle morphology of LDHs can result in interesting physicochemical properties, like the properties of traditional bulk semiconductors. The present manuscript describes the synthesis, characterization, and photocatalytic investigation of Zn2Cr LDHs intercalated with Ac-, I-, Br-, F-, Cl- and NO3-. Samples containing SO42-/Na+ were also obtained by coprecipitation at constant and increased pH. The photocatalytic activity was initially investigated using terephthalic acid as a model reaction, and only the LDHs intercalated with SO42-/Na+ could promote the formation of 2-hydroxy terephthalic acid. The two selected photocatalysts intercalated with SO42-/Na+, prepared under different conditions, were investigated regarding photocatalytic degradation of the emerging organic contaminant sodium diclofenac. Promising results were obtained specially after the recycling of the photocatalysts, which kept almost the same catalytic activity after six cycles of use.

Carbonaceous CoCr LDH nanocomposite as a light-responsive sonocatalyst for treatment of a plasticizer-containing water

The carbonous-based nanocomposites of CoCr layered double hydroxide (LDH) with graphene oxide (GO) and reduced graphene oxide (rGO) were prepared. The successful synthesis of the CoCr LDH in hydrotalcite crystalline structure was deduced from the pattern obtained from X-ray diffraction, and the chemical composition of its surface was checked by X-ray photoelectron spectroscopy. The prosperous decorating of LDH on the sheets of rGO and GO was authenticated by the energy dispersive X-ray spectroscopy analysis and micrographs of scanning electron and transmission electron microscopy. The photo-assisted sonocatalytic activity of the prepared nanocomposites was appraised for the decomposition of dimethyl phthalate (DMP) as a plasticizer. The highest decomposition efficiency of 100% was obtained in the existence of CoCr LDH/rGO nanocomposite (0.5 g/L) during 20 min of reaction time via photo-assisted sonocatalysis. The rGO improved the catalytic activity of the CoCr LDH by increasing the specific surface area from 1.2 m2/g to 4.5 m2/g and reducing the band gap from 1.7 eV to 1.3 eV. Moreover, the results of the colony-forming unit method endorsed antibacterial property improvement of the CoCr LDH via hybridizing with rGO. The results of this research provide an optimistic perspective for applying carbonous-based nanocomposites of CoCr LDH as a novel catalyst with antibacterial properties in photo-assisted sonocatalytic processes.

Design of Multicationic Copper‐Bearing Layered Double Hydroxides for Catalytic Application in Biorefinery

AbstractEthanol has been used as a renewable hydrogen‐donor in the conversion of a lignin model molecule in subcritical conditions. Noble metal‐free porous mixed oxides, obtained by activation of Cu−Ni−Al and Cu−Ni−Fe layered double hydroxide (LDH) precursors, have been used as heterogeneous catalysts for Meerwein‐Ponndorf‐Verley (MPV) hydrogen transfer and further hydrogenation by ethanol dehydrogenation products. Both the Cu/(Cu+Ni) ratio and the nature of the trivalent cation (Al or Fe) affect the activity of the catalysts, as well as the selectivity towards the different steps of the hydrogenation reactions and the cleavage of lignin‐like phenylether bonds. Accounting for the peculiar behaviour of Cu2+ and M(III) cations in the synthesis of LDHs, the coprecipitation of the precursors has been monitored by titration experiments. Structural and textural properties of the catalysts are closely related to the composition of the LDH precursors.

Innovative Reuse of Fly Ashes for Treatment of a Contaminated River Sediment: Synthesis of Layered Double Hydroxides (LDH) and Chemical Performance Assessments

Innovative Reuse of Fly Ashes for Treatment of a Contaminated River Sediment: Synthesis of Layered Double Hydroxides (LDH) and Chemical Performance Assessments

An improved method of MgFe-layered double hydroxide/ biochar composite synthesis

Layered double hydroxides (LDHs) and their composites are a promising platform for a wide range of applications, especially in the environmental field. However, the facile and efficient synthesis of high-quality LDHs and their composites remains a challenge. Here, an improved co-pyrolysis method has been developed to synthesize LDH/biochar composites. A composite material was prepared by directly anchoring MgFe-LDH on corn stover by co-precipitation with FeCl3 and Mg(OH)2, and then through pyrolysis. The main features of this improved method are the use of the solubility product Mg(OH)2 to maintain the pH of the mixture at ∼10 (the optimum for LDH precipitation), eliminating the cumbersome pH control steps of the traditional co-precipitation method, and the low rate of solid-liquid reaction to obtain high LDH crystallinity and purity. This produces improved properties of the MgFe-LDH/biochar composite after pyrolysis: higher loading of MgFe-LDH, larger specific surface area of the composite, a more stable layered structure, and a more customizable LDH. The theoretical maximum adsorption capacity of phosphorus for the composite was 379.4 mg L−1 according to an adsorption isotherm study, and the dominant adsorption mechanism is chemical adsorption accompanied by physical adsorption. In actual wastewater applications, >80% of total phosphorus in biogas slurry was removed via adsorption, indicating that the composite is highly efficient in phosphorus selectivity in wastewaters with complex components. Here, a more sustainable synthesis method of LDH/biochar composite has been developed with high application potential.

Сорбционные свойства слоистых двойных гидроксидов, полученных при ультразвуковом воздействии

Layered double hydroxides (LDH) can be classified as promising materials due to the ease of synthesis, as well as their wide scope of application. However, the process of LDH synthesis, depending on the LDH chemical composition, can take from tens of hours to several days. It was previously identified that ultrasound exposure during the LDH production significantly reduces the synthesis time, and LDHs produced in this way are interesting in relation to the study of their physicochemical properties and sorption capacity. In this work, the authors produced Mg/Fe LDHs in nitrate form by the traditional method and by the combined action of ultrasound and increased hydrostatic pressure. The resulting samples are characterized by a complex of physicochemical methods of analysis, including scanning electron microscopy (SEM), infrared spectroscopy (IR), X-ray phase analysis (XRD), and thermal gravimetric analysis (TGA) with differential scanning calorimetry (DSC). Experiments were carried out to study the sorption capacity of the obtained Fe/Mg LDH samples in relation to chromate ions under normal conditions and under the influence of ultrasound, including in combination with increased hydrostatic pressure. A photoelectric photometer was used to obtain and analyze data with quantitative values of the sorption process. Data of comprehensive analysis of the finished product indicate that the synthesized material is a Mg/Fe layered double hydroxide. X-ray phase analysis identified that the LDH synthesis using ultrasound and pressure increases the crystallinity degree of the finished product. It has been found that the sorption properties of LDHs produced by the conventional method and LDHs produced under the influence of ultrasound and pressure are different. In Mg/Fe LDHs synthesized by the conventional method, chromate sorption proceeds better than in samples synthesized using ultrasonic treatment in combination with increased hydrostatic pressure. The study shows that the sorption process of the examined LDH samples is described by different mathematical models.