Hydrotalcite Materials Research Articles

Blocking endogenous phosphorus release in sediments by a hydrotalcite mixture synthesized with natural sepiolite and discarded cans

Pure hydrotalcite (LDH) materials prepared from chemical reagents have been investigated as solid-phase phosphorus (P) inactivation materials (SPIM) to manage endogenous P loading in sediments. However, the efficacy and mechanism of LDH mixtures prepared by natural minerals and solid wastes in controlling sediment P release are unclear. Therefore, a Ca/Mg-Al-LDH (CMA-LDH) material was synthesized using sepiolite and cans, and its efficacy, mechanism, and ecological impact in controlling sediment P release were investigated. CMA-LDH-p was prepared as a control material using pure chemical reagents. The CMA-LDH and CMA-LDH-p were both composed of hydrotalcite and hydrocalumite. The maximum P adsorption capacity of CMA-LDH was 123.01 mg/g, comparable to that of CMA-LDH-p. The adsorbed P by CMA-LDH was mostly in the stable P form, accounting for 87.2 % of the total P. The adsorption capacity and immobilization ability of CMA-LDH for P were superior to other reported LDH-based SPIM. Both the CMA-LDH addition and capping successfully blocked sediment P release under anaerobic conditions. Passivation of mobile P in the sediment and DGT-labile P in the interstitial water was critical to preventing sediment P release by the CMA-LDH addition. The CMA-LDH capping inhibited sediment P release through the effective adsorption of CMA-LDH on DGT-labile P at the sediment/overlying water interface. The CMA-LDH addition and capping affected the abundance of microbial communities associated with iron and sulfur cycling, which might affect the stability of endogenous P. These results confirmed that CMA-LDH addition and capping treatments were effective methods for managing sediment P loading.

Revisiting hydrotalcite synthesis: Efficient combined mechanochemical/coprecipitation synthesis to design advanced tunable basic catalysts

Abstract Hydrotalcite materials (HTs) were synthesized by a facile and swift combined mechanochemistry/coprecipitation approach, and their catalytic activity was evaluated and compared with conventionally synthesized hydrotalcites (co-precipitation method) in the Knoevenagel condensation between furfural and ethyl cyanoacetate/malononitrile. Characterization and catalytic activity results clearly demonstrate that the proposed combined mechanochemical/coprecipitation approach provides an improvement in crystallinity, morphology, tunable basicity, and textural properties (higher surface area and enhanced surface properties) as compared to HTs obtained via conventional coprecipitation methods. In addition, mechanochemically synthesized HTs largely improve catalytic activities, including conversion and product selectivity to Knoevenagel condensation products under solventless conditions, short reaction times, or reaction at room temperature as compared to conventional counterparts (e.g., 30–40 vs > 99% product yields).

Three dimensional porous magnesium aluminum hydrotalcite material doped with TiO2 and Al2O3 for fluoride removal

At present, the increasingly serious fluorine pollution in water is an enormous threat to human health, therefore, a three-dimensional porous magnesium aluminum hydrotalcite material doped with TiO2 and Al2O3 that can be used as defluorination material was synthesized by a green hydrothermal method and a series of comprehensive fluoride adsorption experiments were conducted in this study. The adsorption material has an ideal adsorption effect on fluoride due to its porous structure and various strong interactions with fluoride. The results of batch adsorption experiments indicate that the maximum adsorption capacity can reach up to 100.69 mg·g−1. Meanwhile, it can be applied in a wide pH range (3–10) and has strong resistance to the effect of coexisting anions. In addition, we explored the adsorption mechanism through DFT calculation, and found that electrostatic attraction, ion exchange, hydrogen bonding and chemisorption were the main adsorption mechanisms. Based on the above advantages, the adsorbent has a good application potential.

Preparation of intercalated hydrotalcite materials and its effect on thermal stability properties of polyvinyl chloride

In this study, ZnAlLa-maleate-LDHs was synthesized using the co-precipitation-hydrothermal method. The effects of aluminum-lanthanum ratio, co-precipitation time, hydrothermal time, and hydrothermal temperature on the crystal structure were investigated. As indicated by the result, the optimal condition was n (Al3+): n (La3+) = 10:1, the co-precipitation time reached 24 h, the hydrothermal time was 8 h, and the hydrothermal temperature reached 180°C. The effect of hydrotalcite on the thermal stability properties and plasticizing properties of PVC was analyzed. The result suggested that ZnAlLa-maleate-LDHs enhanced the thermal stability, plasticizing properties, and mechanical properties of PVC compared with ZnAlLa-CO3-LDHs. The layer spacing of hydrotalcite was increased with the introduction of maleic acid, such that the entry of Cl− into the interlayer guest was facilitated, and the decomposition of PVC was inhibited. Moreover, the long-term thermal stability mechanism was analyzed using FTIR before and after hydrochloric acid treatment. As revealed by the above result, the thermal stabilizer ZnAlLa-maleate-LDHs are capable of hindering the breakage of C-Cl bonds in PVC, inhibiting the formation of HCl, and playing a certain role in thermal stabilization.

Insights into acid-base properties of hydrotalcite materials during hydrothermal carbonization of sewage sludge

Based on proteins hydrolysis requiring alkaline conditions while polysaccharide hydrolysis requiring acidic conditions during hydrothermal carbonization (HTC) of sewage sludge (SS), different types of layered double oxides (LDOs) were introduced as catalysts to understand their role and structural alterations due to its containing acidic and basic sites. Results indicated that the structure of LDOs changes during HTC of SS with structural reconstruction influenced by properties of the aqueous phase, including anions and organic matter. As a result, the properties of the resulting hydrochar are also altered. Structural reconstruction of LDOs is a key factor that influences the HTC of SS. Basic sites of Mg/Al/Zn LDOs are slightly reduced, while acidic sites are remarkably enhanced, leading to an improvement in nitrogen removal and the recovery of organic matter from the HTC aqueous phase.

Preparation and mechanism of tartaric acid-intercalated hydrotalcite retarder for oil-well cement

In view of the existing problems of retarding agents, such as abnormal cementing of cement slurry, slow development of cement strength, low strength, poor thermal stability and excessive retarding, etc. In this study, tartaric acid-intercalated hydrotalcite (Mg/Al-TA-LDH) was prepared by ion exchange between tartaric acid and magnesium–aluminium hydrotalcite (Mg/Al-CO3-LDH). The results show that Mg/Al-CO3-LDH and Mg/Al-TA-LDH have typical structural characteristics of hydrotalcite. The interlayer spacing of Mg/Al-TA-LDH after intercalation is larger than that of Mg/Al-CO3-LDH prior to intercalation. Measurements of the thickening time and thickening curve of oil-well cement show that the slow release of tartaric acid has a retarding effect on the oil-well cement slurry mixed with the tartaric acid-intercalated hydrotalcite retarder, the effect is stable, and the thickening curve is stable and shows right-angle thickening. Based on the compressive strength test of oil-well cement, the strength increases gradually with the addition of 0.3%–1.0 % Mg/Al-TA-LDH promoting the development of 1 d and 3 d strength of stone cement. When the dosage of Mg/Al-TA-LDH is 1.0%, the 1 d and 3 d strength of stone cement is higher than that of pure cement, and the 3 d strength of stone cement is increased by 99.6%. The development of 7 d strength was inhibited, but the late strength development was still higher than that of pure cement, and the 14 d strength was 33.3% higher than that of pure cement. Tartaric acid-intercalated hydrotalcite can increase the thickening time of oil well cement through the release of tartaric acid, and can significantly improve the compressive strength of oil well cement through the seed promotion effect of hydrotalcite material.

Porous Hierarchical Ni/Mg/Al Layered Double Hydroxide for Adsorption of Methyl Orange from Aqueous Solution.

A basic urea technique was successfully used to synthesize Mg/Al-Layered double hydroxides (Mg/Al LDHs), which were then calcined at 400 °C to form Mg/Al-Layered double oxides (Mg/Al LDOs). To reconstruct LDHs, Mg/Al LDOs were fabricated with different feeding ratios of Ni by the co-precipitation method. After synthesis, the Ni/Mg/Al-layered double hydroxides (NMA-LDHs) with 20% and 30% Ni (S1 and S2) were roasted at 400 °C and transformed into corresponding Ni/Mg/Al-layered double oxides (NMA-LDOs) (S1a and S2b, respectively). The physiochemical properties of synthesized samples were also evaluated by various characterization techniques, such as X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDS), Fourier transform infrared (FTIR), and Brunauer, Emmett, and Teller (BET). The adsorption behavior of methyl orange (MO) onto the synthesized samples was evaluated in batch adsorption mode under varying conditions of contact time, adsorbent quantity, and solution pH. As the dosage amount increased from 0.01-0.04 g, the removal percentage of MO dye also increased from 83% to 90% for S1, 84% to 92% for S1a, 77% to 87% for S2, and 93% to 98% for S2b, respectively. For all of the samples, the adsorption kinetics were well described by the pseudo-second-order kinetic model. The equilibrium adsorption data were well fitted to both Langmuir and Freundlich models for methyl orange (MO). Finally, three adsorption-desorption cycles show that NMA-LDHs and NMA-LDOs have greater adsorption and reusability performance for MO dye, signifying that the design and fabrication strategy can facilitate the application of the natural hydrotalcite material in water remediation.

Kinetics of furfural aldol condensation with acetone

Furfural condensation with acetone has been studied over hydrotalcite materials exploring the influence of temperature, furfural to acetone ratio and catalyst loading. Concentration profiles exhibiting limiting conversion values depending on the catalyst amounts along with thermodynamic calculations clearly demonstrating absence of any thermodynamic restrictions point out on catalyst deactivation, which is more pronounced at lower catalyst concentrations. Deactivation is more likely influencing the first step of aldol condensation, rather than subsequent dehydration. A kinetic model has been developed which included catalyst deactivation. Kinetic modelling confirmed an adequate description of the experimental data with the advanced model.

Interfacial Modification to Nanoflower-Like NiV-Layered Double Hydroxide for Enhancing Supercapacitor Performance

Vanadium-based hydrotalcite materials have attracted much attention in supercapacitor electrodes due to their polyvalent properties. Nevertheless, the weak electrical conductivity of hydrotalcite limits its further development. In order to overcome this problem, nanoflowers P-NiV-LDHs-8 and Se-NiV-LDHs-1 were obtained by ingenious modification on the surface of nanoflower microlamellae of NiV-LDHs. Compared with Se-NiV-LDHs-x (x = 0.5, 2), P-NiV-LDHs-x (x = 4, 12), NiV-LDHs, Ni2P, and NiSe2, nanoflowers P-NiV-LDHs-8 and Se-NiV-LDHs-1 have better mass-specific capacity and corresponding rate performances. The self-assembled P-NiV-LDHs-8//AC and Se-NiV-LDHs-1//AC (AC = activated carbon) soft package devices have relatively superior energy density and power density. Moreover, the specific capacitance retention also maintains a relatively impressive level. It is proven that the interfacial modification has a positive effect on the energy storage performance of NiV-LDHs from the perspectives of phosphating and selenizing.

Gold and Ceria Modified NiAl Hydrotalcite Materials as Catalyst Precursors for Dry Reforming of Methane

Structured hydrotalcite NiAl-HT material with Ni/Al atomic ratio of 2.5 was prepared by co-precipitation of Ni and Al nitrate precursors and then modified by the addition of 1 wt% Ce and/or 3 wt% Au species. The obtained materials, after calcination at 600 °C, were characterized by XRD, XPS and TPR. Their catalytic performance was tested through dry reforming of methane (DRM) and by the temperature-programmed surface reaction of methane (TPSR-CH4). Thermal gravimetry analysis (TGA) of the spent catalysts was performed to determine the amount of carbon accumulated during the reaction. The effects of the addition of cerium as a support promoter and gold as nickel promoter and the sequential addition of cerium and gold on the structural properties and on the catalytic efficiency were investigated. Under the severe condition of high space velocity (600,000 mL g−1 h−1), all the catalysts were quite active, with values of CH4 conversion between 67% and 74% at 700 °C. In particular, the combination of cerium and gold enhanced the CH4 conversion up to 74%. Both additives, individually and simultaneously, enhanced the nickel dispersion with respect to the unpromoted NiAl and favored the reducibility of the nickel. During DRM all the catalysts formed graphitic carbon, contributing to their deactivation. The lower carbon gasification temperature of the promoted catalysts confirmed a positive effect played by Ce and Au in assisting the formation of an easier-to-remove carbon. The positive effect was testified by the better stability of the Ce/NiAl with respect to the other catalysts. In the gold-containing samples, this effect was neutralized by Au diffusing towards the catalyst surface during DRM, masking the nickel active sites. TPSR-CH4 test highlighted different CH4 activation capability of the catalysts. Furthermore, the comparison of the deposited carbon features (amount and removal temperature) of the DRM and TPSR spent catalysts indicated a superior activation of CO2 by the Au/Ce/NiAl, to be related to the close interaction of gold and ceria enhancing the oxygen mobility in the catalyst lattice.

Conversion of xylose into furfural over Cr/Mg hydrotalcite catalysts

In this study, the coprecipitation method was used to synthesize a series of chromium-magnesium hydrotalcite materials. The trivalent and alkali metals in the materials acted as Lewis acid and Bronsted base catalysts, respectively. Its specific surface area was increased by calcining the chromium-magnesium hydrotalcite catalyst material. When dehydration of xylose to synthesize furfural was conducted at a temperature of 393 K for 16 h using a catalyst load of 100 mg and xylose substrate of 30 mg, a 50.3% yield was obtained at an optimal M3+/M2+ ratio of 13:20. The catalyst exhibited good stability, with 85.3% activity retained after being used for five cycles.

Interfaces and Oxygen Vacancies-Enriched Catalysts Derived from Cu-Mn-Al Hydrotalcite towards High-Efficient Water-Gas Shift Reaction.

The water-gas shift (WGS) reaction is an important process in the hydrogen industry, and its catalysts are of vital importance for this process. However, it is still a great challenge to develop catalysts with both high activity and high stability. Herein, a series of high-purity Cu-Mn-Al hydrotalcites with high Cu content have been prepared, and the WGS performance of the Cu-Mn-Al catalysts derived from these hydrotalcites have been studied. The results show that the Cu-Mn-Al catalysts have both outstanding catalytic activity and excellent stability. The optimized Cu-Mn-Al catalyst has displayed a superior reaction rate of 42.6 μmolCO-1⋅gcat-1⋅s-1, while the CO conversion was as high as 96.1% simultaneously. The outstanding catalytic activities of the Cu-Mn-Al catalysts could be ascribed to the enriched interfaces between Cu-containing particles and manganese oxide particles, and/or abundant oxygen vacancies. The excellent catalytic stability of the Cu-Mn-Al catalysts may be benefitting from the low valence state of the manganese of manganese oxides, because the low valence manganese oxides have good anti-sintering properties and can stabilize oxygen vacancies. This study provides an example for the construction of high-performance catalysts by using two-dimensional hydrotalcite materials as precursors.

Mô hình hấp phụ đẳng nhiệt và động học hấp phụ phosphat trên vật liệu hydrotalcit Mg-Al/CO3

In this paper, the hydrotalcite Mg-Al/CO3 material was synthesized successfully with an Mg/Al molar ratio of 2:1 by the co-precipitation method. SEM images, XRD patterns and FTIR Spectra and Energy Dispersive X-ray Spectra (EDX) of the material were analyzed. Equilibrium adsorption isotherms and kinetic models of the phosphate adsorption process on the hydrotalcite material Mg-Al/CO3 were investigated. The experimental data were analyzed by Langmuir and Freundlich models of adsorption. The phosphate adsorption on the material was well fitted to both Langmuir and Freundlich isotherms, and the maximum adsorption capacity was found to be 46.95 mg/g with the material sample was calcined at 600oC. The kinetic data obtained at different concentrations have been analyzed using a pseudo-first-order and a pseudo-second-order equation. The experimental data fitted very well with the pseudo-second-order kinetic model.

Hydrodeoxygenation of Anisole by Using a Ruthenium‐Containing Nickel‐Iron Hydrotalcite‐Based Catalyst

AbstractRuthenium‐loaded nickel‐iron (Ni−Fe) hydrotalcite materials were synthesized via the co‐precipitation method. The physicochemical properties of the synthesized materials were characterized by spectroscopic and analytical methods. The highly crystalline nature of Ni−Fe HT (NiFe‐0.5) hydrotalcite material was evident from powder XRD studies. The presence of uniformly dispersed ruthenium in its NiRu alloy form was evident from the TPR studies. The synthesized materials show promising catalytic performance for the hydrodeoxygenation (HDO) of anisole under ambient reaction conditions (190 °C, 20 bar H2). The catalyst prepared with a nickel‐to‐iron molar ratio of 2 : 1 (NF0.5 A) exhibited a good hydrotalcite structure and moderate catalytic activity for the hydrotreatment of anisole. The catalytic activity was improved by the introduction of 4 wt. % ruthenium on the surface of Ni−Fe hydrotalcite (NF0.5Ru), which shows 98 % anisole conversion with the selective formation of toluene as the major product. Catalytic activity remained for several consecutive runs. The recycled catalyst showed a similar conversion with the formation of toluene and methylcyclohexane as the major products. The variation in the selectivity might be due to the re‐dispersion of Ni−Ru active sites.

Removal of Pb (II) from aqueous solutions by new layered double hydroxides adsorbent MgCuCaAl-LDH: Free Gibbs energy, entropy and internal energy studies

• MgCuCaAl-LDH adsorbent showed a high removal capacity for Pb (II). • Experimental results were described by Sips and PSO models. • MgCuCaAl-LDH showed an removal efficiency of 84.62 %. • The prepared material can be reused even after five cycles. • Statistical physics models results in short form. The aim of this study is the removal of Pb (II) from aqueous solutions using a new hydrotalcite material, MgCuCaAl-LDH. The clay was synthesized from a co-precipitation method, at constant pH and with a molar ratio M 2+ /M 3+ of 2. The physico-chemical characterization of the material was carried out using various techniques such as: infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and isoelectric point (pHpzc) measurements. The adsorption behaviour of the Pb (II) on the adsorbent was studied by varying the contact time, the initial pH, the ionic strength of the aqueous solution, the adsorbent doses, the temperature of adsorption and the presence of humic acid substances. The experimental results of kinetic adsorption fit well a pseudo-second order model and that the adsorption isotherm correlates best with the Sips equation. The maximum adsorption capacity was found to be 345.77 mg/g at 25 °C at an initial pH of 5.5 and a contact time of 5 h. The thermodynamic parameters (ΔH°, ΔS°, ΔG°) indicated that the adsorption process was endothermic and spontaneous. Finally, to better understand the adsorption mechanism, a statistical method was used to clarify the number of adsorbed Pb (II) ions per site, the attachment number, the density of the receptor sites, the adsorbed quantity at saturation, the concentration at half saturation and the molar adsorption energy. For the purpose of our study, a statistical physics model, with two binding sites, was used to describe the removal of Pb (II) ions by the adsorbent LDH.

Highly thermally stable multi-porous calcium aluminum hydrotalcite catalyst for efficient carbonate synthesis

In the context of a carbon–neutral era, conversion of greenhouse gas CO2via chemical catalysis is a powerful means. Using CO2and petroleum-derived alkylene oxide as the raw materials to produce high-value carbonate substances has been considered a green and economic path for carbon reduction and energy transition. We discovered a multi-porous calcium aluminum hydrotalcite material (Ca-Al HT), and found that it performs excellent catalytic ability on transesterification (an important reaction in the synthesis of carbonates). Being different from homogeneous basic catalysts such as soluble metal hydroxides and organic halide salts, and well-known solid basic catalyst CaO, which are difficult to recycle and suffer severe deactivation in long-term catalytic process, the robust Ca12Al14O33crystal phase in Ca-Al HT catalyst behaves much more stable catalytic performance during 4000 min efficient catalysis (63 % conversion and 100 % selectivity). The special crystal phase structure of Ca12Al14O33remains stable at even a very high temperature of 900 °C. In contrast, CaO as the reference catalyst is very sensitive to trace H2O in catalytic system, and deactivates immediately. The outstanding catalytic ability of Ca-Al HT is attributed to its super-strong alkali strength, large alkali amount, and quick mass transfer originating from the hierarchical pore system.

Enhanced Adsorption, Photocatalytic Degradation Efficiency of Phenol Red Using CuZnAl Hydrotalcite Synthesized by Co-Precipitation Technique

ZnAlCO3 hydrotalcite materials modified by Cu2+ ions were synthesized by the co-precipitation method according to the molar ratios of (Cu2+ + Zn2+):Al3+ as 7:3. Thus, the modified materials contain various molar ratios of Cu2+ from 0–3.5 in the samples. The synthesized materials were characterized by X-ray diffraction pattern (XRD), FT–IR, EDS, SEM, the N2 adsorption/desorption isotherm (BET), and UV–Vis DRS spectrum. The synthesized materials were characterized by a layered double hydroxide structure—such as hydrotalcite. The specific surface area BET increases slightly, corresponding to the increasing Cu2+ molar ratios, and the bandgap energy Eg decreases accordingly. Especially, these material samples have a high phenol red (PR) adsorption capacity at a concentration of 100 ppm and PR was degraded under a 30 W LED light with over 90% of conversion efficiency in the presence of 1.2 mL of 30% H2O2 solution. In addition, the CuH–3.5 material sample maintained stability after four times catalytic reuse. Therefore, this material can be used as an effective treatment for the wastewater of the sedge mat weaving village.

Highly thermally stable multi-porous calcium aluminum hydrotalcite catalyst for efficient carbonate synthesis

<h2>Abstract</h2> In the context of a carbon-neutral era, conversion of greenhouse gas CO₂ via chemical catalysis is a powerful means. Using CO₂ and petroleum-derived alkylene oxide as the raw materials to produce high-value carbonate substances has been considered a green and economic path for carbon reduction and energy transition. We discovered a multi-porous calcium aluminum hydrotalcite material (Ca-Al HT), and found that it performs excellent catalytic ability on transesterification (an important reaction in the synthesis of carbonates). Being different from homogeneous basic catalysts such as soluble metal hydroxides and organic halide salts, and well-known solid basic catalyst CaO, which are difficult to recycle and suffer severe deactivation in long-term catalytic process, the robust Ca₁₂Al₁₄O₃₃ crystal phase in Ca-Al HT catalyst behaves much more stable catalytic performance during 4000 min efficient catalysis (63% conversion and 100% selectivity). The special crystal phase structure of Ca₁₂Al₁₄O₃₃ maintains stability at even a very high temperature of 900 °C. In contrast, CaO as the reference catalyst is very sensitive to trace H₂O in catalytic system, and deactivates immediately. The outstanding catalytic ability of Ca-Al HT is attributed to its super-strong alkali strength, large alkali amount, and quick mass transfer originating from the hierarchical pore system.

Enhanced Photocatalytic Degradation of Rhodamine-B under Led Light Using CuZnAl Hydrotalcite Synthesized by Co-Precipitation Technique

The co-precipitation method was employed to synthesize a set of ZnAl hydrotalcite materials modified by Cu2+. The synthesized materials have a similar lamellar structure to that of hydrotalcite. The distance between layers is in the range of 7.73–8.56 Å. The network parameters a and c ranged from 3.058 to 3.074 Å and from 23.01 to 24.44, respectively. According to the IUPAC classification, the composites possess a mesoporous structure which belongs to class IV, type H 3. Particularly, the absorption edge shifts strongly to the visible light region when increasing the molar ratio of Cu2+ in the samples from 0 to 3.5. The photocatalytic activity of the synthetic materials was evaluated through the degradation efficiency of rhodamine-B (Rh-B) in the water and colorants in textile wastewater. The present study was the first to synthesize a material sample that contains a molar ratio of Cu2+ in the range of 2.5–3.5 and has high catalytic activities. They were able to degrade Rh-B at a high concentration (100 ppm) with a conversion rate of approximately 90% after 240 min of irradiation using a 30 W LED light. The catalytic activity of the composites depends on the molar ratio of modified Cu2+, the value of environmental pH, the H2O2 concentration and the irradiation time.

Facile water-free synthesis of noble metal-containing hydrotalcites-derived materials and their application for hydrotreatment of anisole

A novel, solvent-free, atom-efficient, and environmentally friendly method for preparing nickel-based hydrotalcite (HT) materials containing group VIII metals was established. A series of nickel-based (NiRu, NiRh, NiIr, NiSn, NiFe, NiCo, NiIn, and NiAl) HT-type materials were successfully synthesized using a facile water-free solid-state grinding method. The precursor-gel obtained by solid-state grinding facilitates efficient hydrolysis of metal salts by the use of ammonium hydroxide and results in the formation of layered HT materials. The presence of layered HT structure was evident from the powder X-ray diffraction (XRD) analysis. The method provides the complete conversion of metal precursors into the corresponding HT materials in an atom-efficient manner. The developed nickel-based HT materials were highly efficient and reusable catalysts for the hydrotreatment of the lignin-derived model compound, anisole. Among the several catalysts prepared, the one based on nickel-ruthenium catalysts showed complete conversion of anisole with 86% selectivity toward cyclohexane under optimum reaction conditions. The presence of in-situ generated metallic nickel‒ruthenium species on the surface of the catalyst, as evident from XPS, TEM, and XRD analysis of the spent catalyst, was responsible for the observed superior catalytic activity.