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Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes

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A special issue of Catalysts (ISSN 2073-4344). This special issue belongs to the section "Catalytic Materials".

Deadline for manuscript submissions: closed (10 March 2022) | Viewed by 47064

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Prof. Dr. Ioan-Cezar Marcu

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Laboratory of Chemical Technology and Catalysis, University of Bucharest, 4-12, Blv. Regina Elisabeta, 030018 Bucharest, Romania
Interests: heterogeneous catalysis; catalysis by metal oxides; semiconducting metal oxides; layered double hydroxides and related materials; catalytic oxidation
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Dr. Octavian D. Pavel

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Faculty of Chemistry, University of Bucharest, 050663 Bucharest, Romania
Interests: base catalysts; fine chemicals synthesis; ionic liquids
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Dear Colleagues,

Layered double hydroxides (LDHs), also known as two-dimensional anionic clays, as well as the derived materials, including hybrids, nanocomposites, mixed oxides, and supported metals, have been highlighted as outstanding heterogeneous catalysts with unlimited applications in various processes involving both acid-base (addition, alkylation, acylation, decarboxylation, etc.) and redox (oxidation, reduction, dehydrogenation, etc.) mechanisms. This is mainly due to their flexibility in chemical composition allowing finely tuning the nature of the active sites and controlling the balance between them. Additionally, LDHs display a large anion exchange capacity and the possibility to modify their interlayer space, constraining the size and type of reactants entering in the interlamellar space. Further, their easy and economic synthesis, with high levels of purity and efficiency, both at laboratory and industrial scale, make LDH and their derived materials excellent solid catalysts. This Special Issue collects original research papers, reviews, and commentaries focused on the catalytic applications of these remarkable materials.

Prof. Dr. Ioan-Cezar Marcu
Dr. Octavian Dumitru Pavel
Guest Editors

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Keywords

Layered double hydroxide
LDH-based hierarchically structured catalysts
LDH-supported catalysts
Acid-base catalysis
Redox catalysis
Sustainable chemical processes
Fine chemical synthesis
Environmental catalysis

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Layered Double Hydroxide-Based Catalysts for Advanced Chemical Technologies in Catalysts (6 articles)

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Editorial

Jump to: Research, Review

3 pages, 209 KiB

Open AccessEditorial

Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes

by Ioan-Cezar Marcu and Octavian Dumitru Pavel

Catalysts 2022, 12(8), 816; https://doi.org/10.3390/catal12080816 - 25 Jul 2022

Cited by 4 | Viewed by 1581

Abstract

Layered double hydroxides (LDH) or hydrotalcites (HT), together with their corresponding mixed oxides, continue to arouse a great deal of research interest [...] Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

Research

Jump to: Editorial, Review

16 pages, 5913 KiB

Open AccessEditor’s ChoiceArticle

An Advanced Approach for MgZnAl-LDH Catalysts Synthesis Used in Claisen-Schmidt Condensation

by Rodica Zăvoianu, Silvana-Denisa Mihăilă, Bogdan Cojocaru, Mădălina Tudorache, Vasile I. Pârvulescu, Octavian Dumitru Pavel, Solon Oikonomopoulos and Elisabeth Egholm Jacobsen

Catalysts 2022, 12(7), 759; https://doi.org/10.3390/catal12070759 - 8 Jul 2022

Cited by 5 | Viewed by 2769

Abstract

Using organic-base tetramethylammonium hydroxide (TMAH) is a viable, cheap, and fast option for the synthesis of MgZnAl-LDH-type materials by both co-precipitation and mechano-chemical methods. TMAH presents several advantages, such as the smaller quantity of water required in the washing step compared to the use of inorganic alkalis, the prevention of LDH contamination with alkali cations, and its action as a template molecule in texture tailoring. It also has disadvantages, such as its presence in small quantities in the resulting layered materials. Regardless of the use of organic/inorganic bases and co-precipitation/mechano-chemical methods, zincite stable phase was found in all the synthesized solids. The basicity of catalysts followed the trend: mixed oxides > reconstructed > parent LDH. The memory effect of LDH was supported only by the presence of Mg and Al cations, while Zn remained as a zincite stable phase. The catalytic activities for Claisen-Schmidt condensation of benzaldehyde with cyclohexanone provided values higher than 90% after 2 h, with a total selectivity toward 2,6-dibenzylidenecyclohexanone, while self-condensation of cyclohexanone yielded no more than 7.29% after 5 h. These behaviors depended on catalyst basicity as well as on the planar rigidity of the compound. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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24 pages, 5810 KiB

Open AccessEditor’s ChoiceArticle

Electrodeposition of a Li-Al Layered Double Hydroxide (LDH) on a Ball-like Aluminum Lathe Waste Strips in Structured Catalytic Applications: Preparation and Characterization of Ni-Based LDH Catalysts for Hydrogen Evolution

by Song-Hui Huang, Yu-Jia Chen, Wen-Fu Huang and Jun-Yen Uan

Catalysts 2022, 12(5), 520; https://doi.org/10.3390/catal12050520 - 5 May 2022

Cited by 3 | Viewed by 2888

Abstract

A functionally structured catalyst was explored for ethanol steam reforming (ESR) to generate H₂. Aluminum lathe waste strips were employed as the structured catalytic framework. The mixed metal oxide (Li-Al-O) was formed on the surface of Al lathe waste strips through calcination of the Li-Al-CO₃ layered double hydroxide (LDH), working as the support for the formation of Ni catalyst nanoparticles. NaOH and NaHCO₃ titration solutions were, respectively, used for adjusting the pH of the NiCl₂ aqueous solutions at 50 °C when developing the precursors of the Ni-based catalysts forming in-situ on the Li-Al-O oxide support. The Ni precursor on the Al structured framework was reduced in a H₂ atmosphere at 500 °C for 3 h, changing the hydroxide precursor into Ni nanoparticles. The titration agent (NaOH or NaHCO₃) effectively affected the physical and chemical characterizations of the catalyst obtained by the different titrations. The ESR reaction catalyzed by the structured catalysts at a relatively low temperature of 500 °C was studied. The catalyst using NaHCO₃ titration presented good stability for generating H₂ during ESR, achieving a high rate of H₂ volume of about 122.9 L/(g_cat·h). It also had a relatively low acidity on the surface of the Li-Al-O oxide support, leading to low activity for the dehydration of ethanol and high activity to H₂ yield. The interactions of catalysts between the Ni precursors and the Li-Al-O oxide supports were discussed in the processes of the H₂ reduction and the ESR reaction. Mechanisms of carbon formation during the ESR were proposed by the catalysts using NaOH and NaHCO₃ titration agents. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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12 pages, 1531 KiB

Open AccessArticle

Alkali-Free Hydrothermally Reconstructed NiAl Layered Double Hydroxides for Catalytic Transesterification

by Nazrizawati A. Tajuddin, Jinesh C. Manayil, Adam F. Lee and Karen Wilson

Catalysts 2022, 12(3), 286; https://doi.org/10.3390/catal12030286 - 3 Mar 2022

Cited by 13 | Viewed by 3438

Abstract

NiAl layered double hydroxides (LDHs) are promising bifunctional catalysts comprising tunable redox and Lewis acidic sites. However, most studies of NiAl LDH employ alkali hydroxide carbonate precipitants which may contaminate the final LDH catalyst and leach into reaction media. Here, we report an alkali-free route to prepare Ni_xAl LDHs with a composition range x = 1.7 to 4.1 using (NH₄)₂CO₃ and NH₄OH as precipitants. Activation of LDHs by calcination–rehydration protocols reveal Ni_xAl LDHs can be reconstructed under mild hydrothermal treatment (110 °C for 12 h), with the degree of reconstruction increasing with Ni content. Catalyst activity for tributyrin transesterification with methanol was found to increase with Ni content and corresponding base site loadings; TOFs also increased, suggesting that base sites in the reconstructed LDH are more effective for transesterification. Hydrothermally reconstructed Ni_4.1Al LDH was active for the transesterification of C₄–C₁₂ triglycerides with methanol and was stable towards leaching during transesterification. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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14 pages, 4138 KiB

Open AccessArticle

Low-Temperature Oxidation Removal of Formaldehyde Catalyzed by Mn-Containing Mixed-Oxide-Supported Bismuth Oxychloride in Air

by Xiaoli Wang, Gongde Wu and Yanwen Ma

Catalysts 2022, 12(3), 262; https://doi.org/10.3390/catal12030262 - 25 Feb 2022

Cited by 2 | Viewed by 2501

Abstract

The Mn-containing mixed-oxide-supported bismuth oxychloride (BiOCl) catalysts were prepared by calcining their corresponding parent hydrotalcite supported BiOCl. The crystal structure of BiOCl was found to be intact during calcination, while significant differences appeared in the chemical state of Mn and the redox capacities of the catalysts before and after calcination. Compared to the hydrotalcite-supported catalysts, the mixed-oxide-supported BiOCl showed much higher catalytic performance in the oxidation removal of formaldehyde due to the synergetic catalysis of more surface oxygen vacancies and higher surface basicity. The complete removal of formaldehyde could be achieved at 70 °C, and the removal efficiency was maintained more than 90% for 21 h. A possible reaction mechanism was also proposed. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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18 pages, 3411 KiB

Open AccessArticle

Green Epoxidation of Olefins with Zn_xAl/Mg_xAl-LDH Compounds: Influence of the Chemical Composition

by Rodica Zăvoianu, Anca Cruceanu, Octavian Dumitru Pavel, Corina Bradu, Mihaela Florea and Ruxandra Bîrjega

Catalysts 2022, 12(2), 145; https://doi.org/10.3390/catal12020145 - 24 Jan 2022

Cited by 3 | Viewed by 2707

Abstract

This contribution concerns the effect of the chemical composition of the brucite-type layer of bi-cationic LDH materials Zn_xAl and Mg_xAl (x = 2–5) and tri-cationic LDH Mg_yZn_zAl (y + z = 4, y = 1, 2, 3) on their catalytic activity for olefin epoxidation with H₂O₂ in the presence of acetonitrile. LDH materials were prepared by the standard method of co-precipitation at constant pH 10, using an aqueous solution of the corresponding metal nitrates and a basic solution containing NaOH and Na₂CO₃. The fresh LDHs were calcined to yield the corresponding mixed oxides and then the recovery of the LDH structure by hydration of the mixed oxides was performed. The resulting samples were characterized by AAS, XRD, DRIFT, DR-UV–Vis, BET and determination of basic sites. The results of the catalytic tests for olefin epoxidation were well correlated with the basicity of the samples, which was in turn related to the M²⁺/Al³⁺ ratio and the electronegativity of different bivalent metals in the brucite-type layer. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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15 pages, 3744 KiB

Open AccessArticle

MgCr-LDH Nanoplatelets as Effective Oxidation Catalysts for Visible Light-Triggered Rhodamine B Degradation

by Susanginee Nayak and Kulamani Parida

Catalysts 2021, 11(9), 1072; https://doi.org/10.3390/catal11091072 - 3 Sep 2021

Cited by 23 | Viewed by 2501

Abstract

In this work, we successfully exfoliated MgCr-(NO₃⁻) LDH with large purity by a simple formamide method followed by post-hydrothermal treatment and characterized by different physico-chemical techniques. The UV-DRS study persuades the red-shifted absorption band and suitable band gap of MgCr-(NO₃⁻) LDH for optimum light harvestation ability related to the optical properties. Alternatively, the production of elevated photocurrent density of MgCr-(NO₃⁻) LDH (3:1, 80 °C) in the anodic direction was verified by the LSV study, which further revealed their effective charge separation efficacy. These MgCr-LDH nanosheets (3:1, 80 °C) displayed the superior Rhodamine B (RhB) degradation efficiency of 95.0% at 0.80 kW/m² solar light intensity in 2 h. The tremendous catalytic performances of MgCr-LDH (3:1, 80 °C) were typically linked with the formation of surface-active sites for the charge trapping process due to the presence of uncoordinated metallocenters during the exfoliation process. Furthermore, the maximum amount of the active free atoms at the edges of the hexagonal platelet of MgCr-LDH causes severance of the nanosheets, which generates house of platelets of particle size ~20–50 nm for light harvestation, promoting easy charge separation and catalytic efficiency. In addition, radical quenching tests revealed that h⁺ and •OH play as major active species responsible for the RhB degradation. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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17 pages, 2561 KiB

Open AccessFeature PaperArticle

On the Effect of the M³⁺ Origin on the Properties and Aldol Condensation Performance of MgM³⁺ Hydrotalcites and Mixed Oxides

by Valeriia Korolova, Oleg Kikhtyanin, Martin Veselý, Dan Vrtiška, Iva Paterová, Vlastimil Fíla, Libor Čapek and David Kubička

Catalysts 2021, 11(8), 992; https://doi.org/10.3390/catal11080992 - 18 Aug 2021

Cited by 8 | Viewed by 2700

Abstract

Hydrotalcites (HTCs) are promising solid base catalysts to produce advanced biofuels by aldol condensation. Their main potential lies in the tunability of their acid-base properties by varying their composition. However, the relationship between the composition of hydrotalcites, their basicity, and their catalytic performance has not yet been fully revealed. Here, we investigate systematically the preparation of HTCs with the general formula of Mg₆M³⁺₂(OH)₁₆CO₃·4H₂O, where M³⁺ stands for Al, Ga, Fe, and In, while keeping the Mg/M³⁺ equal to 3. We use an array of analytical methods including XRD, N₂ physisorption, CO₂-TPD, TGA-MS, FTIR-ATR, and SEM to assess changes in the properties and concluded that the nature of M³⁺ affected the HTC crystallinity. We show that the basicity of the HTC-derived mixed oxides decreased with the increase in atomic weight of M³⁺, which was reflected by decreased furfural conversion in its aldol condensation with acetone. We demonstrate that all MgM³⁺ mixed oxides can be fully rehydrated, which boosted their activity in aldol condensation. Taking all characterization results together, we conclude that the catalytic performance of the rehydrated HTCs is determined by the “host” MgO component, rather than the nature of M³⁺. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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19 pages, 3828 KiB

Open AccessArticle

Photoelectrocatalytic Degradation of Congo Red Dye with Activated Hydrotalcites and Copper Anode

by Sara Argote-Fuentes, Rossy Feria-Reyes, Esthela Ramos-Ramírez, Norma Gutiérrez-Ortega and Gustavo Cruz-Jiménez

Catalysts 2021, 11(2), 211; https://doi.org/10.3390/catal11020211 - 5 Feb 2021

Cited by 31 | Viewed by 4105

Abstract

Photoelectrocatalysis is a novel technique that combines heterogeneous photocatalysis with the application of an electric field to the system through electrodes for the degradation of organic contaminants in aqueous systems, mainly of toxic dyes. The efficiency of these combined processes depends on the semiconductor properties of the catalysts, as well as on the anodic capacity of the electrode. In this study, we propose the use of active hydrotalcites in the degradation of Congo red dye through processes assisted by ultraviolet (UV) irradiation and electric current. Our research focused on evaluating the degradation capacity of Congo red by means of photolysis, catalysis, photocatalysis, electrocatalysis, and photoelectrocatalysis, as well as identifying the effect of the properties of the active hydrotalcites in these processes. The results show that a maximum degradation was reached with the photoelectrocatalysis process with active hydrotalcites and a copper anode at 6 h with 95% in a half-life of 0.36 h. The degradation is favored by the attack of the OH^• radicals under double bonds in the diazo groups where the electrode produces Cu²⁺ ions, and with the photogenerated electrons, the recombination speed of the electron–hole in the hydrotalcite catalyst is reduced until the complete degradation. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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14 pages, 5472 KiB

Open AccessArticle

CuAlCe Oxides Issued from Layered Double Hydroxide Precursors for Ethanol and Toluene Total Oxidation

by Hadi Dib, Rebecca El Khawaja, Guillaume Rochard, Christophe Poupin, Stéphane Siffert and Renaud Cousin

Catalysts 2020, 10(8), 870; https://doi.org/10.3390/catal10080870 - 3 Aug 2020

Cited by 11 | Viewed by 3931

Abstract

CuAlCe oxides were obtained from hydrotalcite-type precursors by coprecipitation using a M²⁺/M³⁺ ratio of 3. The collapse of the layered double hydroxide structure following the thermal treatment leads to the formation of mixed oxides (CuO and CeO₂). The catalytic performance of the copper-based catalysts was evaluated in the total oxidation of two Volatile Organic Compounds (VOCs): ethanol and toluene. XRD, SEM Energy-Dispersive X-ray Spectrometry (EDX), H₂-temperature programmed reduction (TPR) and XPS were used to characterize the physicochemical properties of the catalysts. A beneficial effect of combining cerium with CuAl-O oxides in terms of redox properties and the abatement of the mentioned VOCs was demonstrated. The sample with the highest content of Ce showed the best catalytic properties, which were mainly related to the improvement of the reducibility of the copper species and their good dispersion on the surface. The presence of a synergetic effect between the copper and cerium elements was also highlighted. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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13 pages, 1748 KiB

Open AccessFeature PaperArticle

Activity in the Photodegradation of 4-Nitrophenol of a Zn,Al Hydrotalcite-Like Solid and the Derived Alumina-Supported ZnO

by Raquel Trujillano, César Nájera and Vicente Rives

Catalysts 2020, 10(6), 702; https://doi.org/10.3390/catal10060702 - 22 Jun 2020

Cited by 16 | Viewed by 3253

Abstract

A Zn,Al layered double hydroxide (LDH), with the hydrotalcite structure and the mixed oxide obtained upon its calcination at 650 °C, was tested in the adsorption and photocatalytic degradation of 4-Nitrophenol in aqueous solution. The Zn,Al LDH was fast and easily obtained by the coprecipitation method. Hydrothermal treatment under microwave irradiation was applied to compare the effect of the ageing treatment on the photocatalytic behavior. The efficiency of the synthetized solids was compared to that of a commercial ZnO. The ageing treatment did not improve the performance of the original samples in the degradation of 4-nitrophenol. The activity of the synthetized solids tested exceeded that observed for the reaction with commercial ZnO. The photocatalytic performance of the original non-calcined hydrotalcite is similar to that of commercial ZnO. The calcined hydrotalcite showed a better performance in the adsorption-degradation of the contaminant than ZnO, and its reusability would be possible as it recovered the hydrotalcite-like structure during the reaction. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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15 pages, 3225 KiB

Open AccessArticle

Ultrasonic-Assisted Michael Addition of Arylhalide to Activated Olefins Utilizing Nanosized CoMgAl-Layered Double Hydroxide Catalysts

by Nada S. Althabaiti, Fawzia M. Al-Nwaiser, Tamer S. Saleh and Mohamed Mokhtar

Catalysts 2020, 10(2), 220; https://doi.org/10.3390/catal10020220 - 11 Feb 2020

Cited by 14 | Viewed by 3187

Abstract

An efficient cobalt-based layered double hydroxide (LDH)-catalyzed Michael addition of an aryl halide compound onto activated olefin as a Michael acceptor is described. The synthesized catalytic materials were characterized using different techniques to investigate their physicochemical, morphological, and textural properties. The partial isomorphic substitution of magnesium by cobalt ions in the cationic sheets of the layered double hydroxide (CoMgAl-LDH) appears to be an appropriate catalyst to cause this reaction. This technique enables compound synthesis resulting from the 1,4-addition in good to excellent yields. Moreover, ultrasound was found to have beneficial effect on this reaction due to the cavitation phenomenon. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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Review

Jump to: Editorial, Research

40 pages, 5220 KiB

Open AccessFeature PaperReview

Highlights on the Catalytic Properties of Polyoxometalate-Intercalated Layered Double Hydroxides: A Review

by Alexandra-Elisabeta Stamate, Octavian Dumitru Pavel, Rodica Zavoianu and Ioan-Cezar Marcu

Catalysts 2020, 10(1), 57; https://doi.org/10.3390/catal10010057 - 1 Jan 2020

Cited by 42 | Viewed by 8689

Abstract

Layered double hydroxides (LDH) are an extended class of two-dimensional anionic materials that are known for their unique lamellar structure, versatile composition, and tunable properties. The layered architecture allows the intercalation between the positively charged sheets of a vast variety of anionic species, including oxometalates and polyoxometalates (POM). The hybrid composites that were developed using POM and LDH show great advantages when compared to both parent materials causing the appearance of new functionalities, which may lead to remarkable contributions in many areas of application, especially in catalysis. The current review paper emphases all of the crucial works already existing in literature that are related to the large group of POM-LDH solids and their use as catalysts for fine organic synthesis. The new trends in the development of the POM-LDH catalysts are highlighted based on the overview of 121 scientific articles that were published between 1984 and 2019. The main topics are focused primarily on the synthesis, characterization, and the catalytic applications of different LDH systems hosting polyoxometalates with low, medium, and high nuclearity. The intense exploration of the POM-LDH field has led to the obtaining of countless effective catalysts used in various types of reactions, from condensation, esterification, halodecarboxylation, to oxidation and epoxidation. Full article

(This article belongs to the Special Issue Layered Double Hydroxide-Based Catalytic Materials for Sustainable Processes)

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