Systematic Preparation Of Polyoxometalate Pillared Layered Double Hydroxides Via Direct Aqueous Reaction

1991 ◽  
Vol 233 ◽  
Author(s):  
Jiandang Wang ◽  
Ying Tian ◽  
Ren-Chain Wang ◽  
Jorge L. Colón ◽  
Abraham Clearfield
Keyword(s):  
Layered Double Hydroxides ◽  
Extended Period ◽  
Interlayer Spacing ◽  
X Ray ◽  
Keggin Ion ◽  
Keggin Ions ◽  
Great Ease ◽  
Key Factor ◽  
Double Hydroxides ◽  
The Ideal

ABSTRACTThe series of layered double hydroxides, MgnAl(OH)2n+2X (n = 2–5, X = NO3− or Cl−) and NinAl(OH) 2n+2X (n = 2–4, X = NO3− or Cl−), were pillared with polyoxometalate ions of the Keggin structure, ranging from [PW12O40]3− to [PV4W8O40]7−, in aqueous solution. Full exchange of the Keggin ions into the layers is achieved as evidenced by X-ray powder diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. Also, partial exchange was observed for Ni5Al(OH)12NO3 The key factor that effects these reactions is the pre-swelling step. Thus, when the layered double hydroxides are thoroughly wet either by preparing wet solids or by soaking the dried products for an extended period, pillaring reactions proceed with great ease. Relations can be extracted between the water content and the separation between the layers, as well as between layer charge density and the charge of the Keggin ion. The pillared layered double hydroxides were found generally to have interlayer distances ranging from 11.0 to 13.5 Å, which is smaller than the numerical sum of the Keggin ion diameter and the ideal thickness of the hydroxide layer. This fact and the low crystallinity are attributed to strong interaction between the basic layered double hydroxides and the acidic Keggin ions. A more crystalline phase with the expected 14.5 Å interlayer spacing was also obtained as a mixture with the lower spaced products.

scholarly journals Photocatalytic Degradation of 2,4,6-Trichlorophenol by MgO–MgFe2O4 Derived from Layered Double Hydroxide Structures

Catalysts ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 454 ◽  
Author(s):  
Esthela Ramos-Ramírez ◽  
Francisco Tzompantzi-Morales ◽  
Norma Gutiérrez-Ortega ◽  
Héctor G. Mojica-Calvillo ◽  
Julio Castillo-Rodríguez
Keyword(s):  
Photocatalytic Degradation ◽  
Layered Double Hydroxides ◽  
X Ray Diffraction ◽  
Application Study ◽  
Toxic Compounds ◽  
X Ray ◽  
Thermally Activated ◽  
Double Hydroxide ◽  
Double Hydroxides ◽  
Scanning Electron

In recent years, the search for solutions for the treatment of water pollution by toxic compounds such as phenols and chlorophenols has been increasing. Phenols and their derivatives are widely used in the manufacture of pesticides, insecticides, paper, and wood preservers, among other things. Chlorophenols are partially biodegradable but not directly photodegradable by sunlight and are extremely toxic—especially 2,4,6-trichlorophenol, which is considered to be potentially carcinogenic. As a viable proposal to be applied in the treatment of water contaminated with 2,4,6-trichlorophenol, this paper presents an application study of the thermally activated Mg/Fe layered double hydroxides as photocatalysts for the mineralization of this contaminant. Activated Mg/Fe layered double hydroxides were characterized by X-ray diffraction, thermal analysis, N2 physisorption, and scanning electron microscopy with X-ray dispersive energy. The results of the photocatalytic degradation of 2,4,6-trichlorophenol in aqueous solution showed good photocatalytic activity, with an efficiency of degradation of up to 93% and mineralization of 82%; degradation values which are higher than that of TiO2-P25, which only reached 18% degradation. The degradation capacity is attributed to the structure of the MgO–MgFe2O4 oxides derived from double laminate hydroxide Mg/Fe. A path of degradation based on a mechanism of superoxide and hollow radicals is proposed.

scholarly journals Mn-Fe Layered Double Hydroxide Intercalated with Ethylene-Diaminetetraacetate Anion: Synthesis and Removal of As(III) from Aqueous Solution around pH 2–11

2020 ◽  
Vol 17 (24) ◽  
pp. 9341
Author(s):  
Guifeng Liu ◽  
Zongqiang Zhu ◽  
Ningning Zhao ◽  
Yali Fang ◽  
Yingying Gao ◽  
...  
Keyword(s):  
Adsorption Capacity ◽  
Layered Double Hydroxides ◽  
Interlayer Spacing ◽  
Maximum Adsorption Capacity ◽  
Hydroxyl Groups ◽  
Surface Hydroxyl ◽  
Xps Characterization ◽  
Ph Range ◽  
Double Hydroxide ◽  
Double Hydroxides

A novel adsorbent Mn-Fe layered double hydroxides intercalated with ethylenediaminete-traacetic (EDTA@MF-LDHs) was synthesized by a low saturation coprecipitation method. The behavior and mechanism of As(III) removed by EDTA@MF-LDHs were investigated in detail in comparison with the carbonate intercalated Mn-Fe layered double hydroxides (CO3@MF-LDHs). The results showed that EDTA@MF-LDHs had a higher removal efficiency for As(III) than As(V) with a broader pH range than CO3@MF-LDH. The large adsorption capacity of EDTA@MF-LDHs is related to its large interlayer spacing and the high affinity of its surface hydroxyl groups. The maximum adsorption capacity for As(III) is 66.76 mg/g at pH 7. The FT-IR and XPS characterization indicated that the removal mechanism of the As(III) on EDTA@MF-LDHs include surface complexation, redox, and ion exchange.

scholarly journals Potential Sustainable Slow-Release Fertilizers Obtained by Mechanochemical Activation of MgAl and MgFe Layered Double Hydroxides and K2HPO4

Nanomaterials ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 183 ◽  
Author(s):  
Roger Borges ◽  
Fernando Wypych ◽  
Elodie Petit ◽  
Claude Forano ◽  
Vanessa Prevot
Keyword(s):  
Layered Double Hydroxides ◽  
Slow Release ◽  
Mechanochemical Activation ◽  
Molar Ratio ◽  
X Ray ◽  
Dipotassium Hydrogen Phosphate ◽  
Before And After ◽  
Noticeable Improvement ◽  
Slow Release Fertilizers ◽  
Double Hydroxides

This study describes the behavior of potential slow-release fertilizers (SRF), prepared by the mechanochemical activation of calcined Mg2Al-CO3 or Mg2Fe-CO3 layered double hydroxides (LDH) mixed with dipotassium hydrogen phosphate (K2HPO4). The effects of LDH thermal treatment on P/K release behavior were investigated. Characterizations of the inorganic composites before and after release experiments combined X-Ray diffraction (XRD), Fourier-transform infra-red spectroscopy (FTIR), solid-state nuclear magnetic resonance (NMR), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The best release profile (<75% in 28 days and at least 75% release) was obtained for MgAl/K2HPO4 (9 h milling, 2:1 molar ratio, MR). Compared to readily used K2HPO4, milling orthophosphate into LDH matrices decreases its solubility and slows down its release, with 60% and 5.4% release after 168 h for MgAl/K2HPO4 and MgFe/K2HPO4 composites, respectively. Mechanochemical addition of carboxymethylcellulose to the LDH/K2HPO4 composites leads to a noticeable improvement of P release properties.

scholarly journals High efficient photocatalytic activity of Zn-Al-Ti layered double hydroxides nanocomposite

2018 ◽  
Vol 149 ◽  
pp. 01087 ◽  
Author(s):  
F. Amor ◽  
A. Diouri ◽  
I. Ellouzi ◽  
F. Ouanji ◽  
M. Kacimi
Keyword(s):  
Methylene Blue ◽  
Photocatalytic Activity ◽  
Uv Irradiation ◽  
Layered Double Hydroxides ◽  
Removal Rate ◽  
X Ray Diffraction ◽  
Simple Method ◽  
X Ray ◽  
High Efficient ◽  
Double Hydroxides

This work establishes a simple method for synthesising layered double hydroxides (LDHs) powders with coprecipitation. The characteristics of the samples were investigated y X-ray diffraction (XRD), scanning electron microscopy (SEM) and spectrophotometer UV–Vis (DRS). Non-uniform distribution was shown for LDHs samples by SEM. Photocatalytic efficiencies were tested using methylene blue (MB) dye as a model contaminant under UV irradiation. In particular, Zn–Al-Ti LDH exhibited an excellent performance towards MB degradation compared with commercial TiO2 nanoparticles. Methylene blue removal percentage was reached at almost 100%, whereas commercial TiO2 reached a removal rate of only 66% under the same conditions within 20 min. The aim of the current work is to prepare Zn-Al-Ti layered double hydroxides nanocomposite and to evaluate their photocatalytic activity in the removal of methylene blue under UV irradiation.

scholarly journals Designing Magnetic Layered Double Hydroxides and Two-Dimensional Magnetic Nano-Nets of Cobalt Ferrite through a Novel Approach

2018 ◽  
Vol 8 (11) ◽  
pp. 2099 ◽  
Author(s):  
Osama Saber ◽  
Abdullah Aljaafari ◽  
Sarah Asiri ◽  
Khalid Batoo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Layered Double Hydroxides ◽  
Cobalt Ferrite ◽  
High Coercivity ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Double Hydroxides

The present study has a dual aim of supporting magnetic nanoparticles over the nanolayers of LDHs and designing two-dimensional magnetic nano-nets of cobalt ferrite. In this trend, nanoparticles of CoFe2O4 were prepared and supported by Co-Fe LDH through urea hydrolysis. The nanolayered structures of Co-Fe LDH were confirmed by X-ray diffraction, energy-dispersive X-ray spectrometry, FT-IR spectra, thermal analyses, and transmission electron microscopy. In addition, they indicated that 13.2% CoFe2O4 were supported over Co-Fe LDH. Transformation of the nanolayered structures of Co-Fe LDH to nano-nets was achieved by the catalytic effect of the supported CoFe2O4 nanoparticles through solvent thermal technique. X-ray diffraction patterns and transmission electron microscopy images confirmed the transformation of the supported Co-Fe LDH to nano-nets of cobalt ferrite. In order to indicate the effect of the LDH for designing the nano-nets, nanoparticles of cobalt ferrite were prepared by the same technique without LDH. The magnetic behavior of the nano-nets and the supported Co-Fe LDH were measured and compared with the nanoparticles through vibrating sample magnetometer technique. The magnetic parameters indicated that the prepared nano-nets have ferromagnetic behavior and high coercivity. However, the prepared nanoparticles revealed a superparamagnetic state and low coercivity. The experimental results concluded that the incorporation of nanoparticles with nanowires into nano-net structures has been found to be an efficient way to improve their magnetic properties and prevent their agglomerations. Finally, layered double hydroxides are an important source for constructing magnetic nanolayered structures and nano-nets.

scholarly journals Gas-Phase Hydrogenation of Furfural to Furfuryl Alcohol over Cu-ZnO-Al2O3 Catalysts Prepared from Layered Double Hydroxides

Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 486
Author(s):  
Guillermo R. Bertolini ◽  
Carmen P. Jiménez-Gómez ◽  
Juan Antonio Cecilia ◽  
Pedro Maireles-Torres
Keyword(s):  
Gas Phase ◽  
Aging Time ◽  
Layered Double Hydroxides ◽  
Furfuryl Alcohol ◽  
Precipitation Method ◽  
Molar Ratio ◽  
X Ray ◽  
General Chemical ◽  
Co Precipitation ◽  
Double Hydroxides

Several layered double hydroxides (LDHs) with general chemical composition (Cu,Zn)1−xAlx(OH)2(CO3)x/2·mH2O have been synthesized by the co-precipitation method, maintaining a (M2+/M3+) molar ratio of 3, and varying the Cu2+/Zn2+ molar ratio between 0.2 and 6.0. After calcination and reduction steps, Cu/ZnO/Al2O3 catalysts were synthesized. These catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), H2 thermoprogrammed reduction (H2-TPR), N2 adsorption-desorption at −196 °C, N2O titration, X-ray photoelectron miscroscopy (XPS), NH3-thermoprogramed desorption (NH3-TPD) and CO2- thermoprogrammed desorption (CO2-TPD). The characterization data revealed that these catalysts are mainly meso-and macroporous, where Cu, ZnO and Al2O3 are well dispersed. The catalytic results show that these catalysts are active in the gas-phase hydrogenation of furfural, being highly selective to furfuryl alcohol (FOL) and reaching the highest FOL yield for the catalyst with a Cu2+/Zn2+ molar ratio of 1. In an additional study, the influence of the aging time on the synthesis of the LDHs was also evaluated. The catalytic data revealed that the use of shorter aging time in the formation of the LDH has a beneficial effect on the catalytic behavior, since more disordered structures with a higher amount of available Cu sites is obtained, leading to a higher yield towards FOL (71% after 5 h of time-on-stream at 210 °C).

Preparation of hydroxy double salts exchanged by organic compounds

1998 ◽  
Vol 13 (4) ◽  
pp. 848-851 ◽  
Author(s):  
Hiroyuki Morioka ◽  
Hideyuki Tagaya ◽  
Masa Karasu ◽  
Jun-ichi Kadokawa ◽  
Koji Chiba
Keyword(s):  
Carboxylic Acid ◽  
Carboxylic Acids ◽  
Layered Double Hydroxides ◽  
Interlayer Spacing ◽  
Layered Materials ◽  
Exchange Reactions ◽  
Double Salts ◽  
Hydroxy Double Salts ◽  
Double Hydroxides ◽  
Positively Charged

Hydroxy double salts (HDS's) comprise a class of layered materials that are similar to layered double hydroxides (LDH's) and show a comparable intracrystalline reactivity. Their anion exchange reactions occur with preincorporated anions in the hydroxide layer and with anions bound as gegenions of the positively charged layers, respectively. In this study, nitrate and acetate anions of HDS's were exchanged with anionic monoand di-carboxylic acids, and we confirmed that interlayer spacing of HDS's increased depending on the size of mono- and di-carboxylic acids. Moreover, we have prepared photofunctional materials by exchange reaction with azobenzene-p-carboxylic acid and 4–4′-azobenzenedicarboxylic acid.

Probing the thermal decomposition process of layered double hydroxides through in situ 57Fe Mössbauer and in situ X-ray diffraction experiments

2006 ◽  
Vol 42 (2) ◽  
pp. 534-538 ◽  
Author(s):  
Daniel X. Gouveia ◽  
Odair P. Ferreira ◽  
Antonio G. Souza Filho ◽  
M. G. da Silva ◽  
J. A. C. de Paiva ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Layered Double Hydroxides ◽  
Decomposition Process ◽  
X Ray Diffraction ◽  
Thermal Decomposition Process ◽  
X Ray ◽  
57Fe Mössbauer ◽  
Double Hydroxides

scholarly journals Interlayer Structure of Bioactive Molecule, 2-Aminoethanesulfonate, Intercalated into Calcium-Containing Layered Double Hydroxides

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Tae-Hyun Kim ◽  
Hyoung Jun Kim ◽  
Jae-Min Oh
Keyword(s):  
Layered Double Hydroxides ◽  
Solid Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Calcium Cation ◽  
Particle Size And Morphology ◽  
Interlayer Structure ◽  
Diffraction Patterns ◽  
Size And Morphology ◽  
Double Hydroxides

We have successfully intercalated 2-aminoethanesulfonate, a well-known biomolecule taurine, into calcium-containing layered double hydroxides via optimized solid phase intercalation. According to X-ray diffraction patterns and infrared spectroscopy, it was revealed that the intercalated taurine molecules were each directly coordinated to other calcium cation and arranged in a zig-zag pattern. Scanning electron microscopy showed that the particle size and morphology of the LDHs were not affected by the solid phase intercalation, and the surface of intercalates was covered by organic moieties. From ninhydrin amine detection tests, we confirmed that most of the taurine molecules were well stabilized between the calcium-containing LDH layers.

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