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Title: Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc-iron layered double hydroxides by one-step coprecipitation route

Abstract

Inorganic sulfate- and organic dodecylbenzenesulfonate (DBS)-intercalated zinc-iron layered double hydroxides (LDHs) materials were prepared by one-step coprecipitation method from a mixed salt solutions containing Zn(II), Fe(II) and Fe(III) salts. The as-prepared samples have been characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), low-temperature nitrogen adsorption, scanning electron microscopy (SEM), inductively coupled plasma emission spectroscopy (ICP), and Moessbauer spectroscopy (MS). The XRD analyses demonstrate the typical LDH-like layered structural characteristics of both products. The room temperature MS results reveal the characteristics of both the Fe(II) and Fe(III) species for SO{sub 4} {sup 2-}-containing product, while only the Fe(III) characteristic for DBS-containing one. The combination characterization results and Rietveld analysis illustrate that the SO{sub 4} {sup 2-}-containing product possesses the Green Rust two (GR2)-like crystal structure with an approximate chemical composition of [Zn{sub 0.435}.Fe{sup II} {sub 0.094}.Fe{sup III} {sub 0.470}.(OH){sub 2}].(SO{sub 4} {sup 2-}){sub 0.235}.1.0H{sub 2}O, while the DBS-containing one exhibits the common LDH compound-like structure. The contact angle measurement indicates the evident hydrophobic properties of DBS-containing nanocomposite, compared with SO{sub 4} {sup 2-}-containing product, due to the modification of the internal and external surface of LDHs by the organic hydrophobic chain of DBS. - Graphical abstract: For Zn{sup 2+}-Fe{supmore » 2+}-Fe{sup 3+} GR2(SO{sub 4} {sup 2-}), according to the derived chemical formula, Fe{sup 3+} was arranged at 1a (0, 0, 0) position, while all Zn{sup 2+} were in 2d position with the occupancy 0.645, and the left part of 2d positions were taken by Fe{sup 2+}/Fe{sup 3+}.« less

Authors:
 [1];  [2];  [3]
  1. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Box 98, Beijing 100029 (China), E-mail: huizhang67@gst21.com
  2. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Box 98, Beijing 100029 (China)
  3. State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871 (China)
Publication Date:
OSTI Identifier:
21015819
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 5; Other Information: DOI: 10.1016/j.jssc.2007.03.016; PII: S0022-4596(07)00117-X; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ADSORPTION; CHEMICAL COMPOSITION; CLATHRATES; COPRECIPITATION; CRYSTAL STRUCTURE; EMISSION SPECTROSCOPY; FOURIER TRANSFORM SPECTROMETERS; FOURIER TRANSFORMATION; HYDROXIDES; INFRARED SPECTRA; IRON COMPOUNDS; IRON IONS; MOESSBAUER EFFECT; NITROGEN; PLASMA; SCANNING ELECTRON MICROSCOPY; SULFATES; SURFACES; SYNTHESIS; TEMPERATURE RANGE 0273-0400 K; X-RAY DIFFRACTION; ZINC COMPOUNDS; ZINC IONS

Citation Formats

Zhang Hui, Wen Xing, and Wang Yingxia. Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc-iron layered double hydroxides by one-step coprecipitation route. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2007.03.016.
Zhang Hui, Wen Xing, & Wang Yingxia. Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc-iron layered double hydroxides by one-step coprecipitation route. United States. doi:10.1016/j.jssc.2007.03.016.
Zhang Hui, Wen Xing, and Wang Yingxia. Tue . "Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc-iron layered double hydroxides by one-step coprecipitation route". United States. doi:10.1016/j.jssc.2007.03.016.
@article{osti_21015819,
title = {Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc-iron layered double hydroxides by one-step coprecipitation route},
author = {Zhang Hui and Wen Xing and Wang Yingxia},
abstractNote = {Inorganic sulfate- and organic dodecylbenzenesulfonate (DBS)-intercalated zinc-iron layered double hydroxides (LDHs) materials were prepared by one-step coprecipitation method from a mixed salt solutions containing Zn(II), Fe(II) and Fe(III) salts. The as-prepared samples have been characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), low-temperature nitrogen adsorption, scanning electron microscopy (SEM), inductively coupled plasma emission spectroscopy (ICP), and Moessbauer spectroscopy (MS). The XRD analyses demonstrate the typical LDH-like layered structural characteristics of both products. The room temperature MS results reveal the characteristics of both the Fe(II) and Fe(III) species for SO{sub 4} {sup 2-}-containing product, while only the Fe(III) characteristic for DBS-containing one. The combination characterization results and Rietveld analysis illustrate that the SO{sub 4} {sup 2-}-containing product possesses the Green Rust two (GR2)-like crystal structure with an approximate chemical composition of [Zn{sub 0.435}.Fe{sup II} {sub 0.094}.Fe{sup III} {sub 0.470}.(OH){sub 2}].(SO{sub 4} {sup 2-}){sub 0.235}.1.0H{sub 2}O, while the DBS-containing one exhibits the common LDH compound-like structure. The contact angle measurement indicates the evident hydrophobic properties of DBS-containing nanocomposite, compared with SO{sub 4} {sup 2-}-containing product, due to the modification of the internal and external surface of LDHs by the organic hydrophobic chain of DBS. - Graphical abstract: For Zn{sup 2+}-Fe{sup 2+}-Fe{sup 3+} GR2(SO{sub 4} {sup 2-}), according to the derived chemical formula, Fe{sup 3+} was arranged at 1a (0, 0, 0) position, while all Zn{sup 2+} were in 2d position with the occupancy 0.645, and the left part of 2d positions were taken by Fe{sup 2+}/Fe{sup 3+}.},
doi = {10.1016/j.jssc.2007.03.016},
journal = {Journal of Solid State Chemistry},
number = 5,
volume = 180,
place = {United States},
year = {Tue May 15 00:00:00 EDT 2007},
month = {Tue May 15 00:00:00 EDT 2007}
}
  • Cd-Cr and Zn-Cd-Cr layered double hydroxides (CdCr-LDH and ZnCdCr-LDH) containing alkyl sulfate as the interlamellar anion have been prepared through a coprecipitation technique. The resulting compounds were characterized using X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, and scanning electron microscopy. Magnetic property measurements indicate that antiferromagnetic interactions occur between the chromium ions in the two compounds at low temperatures. The introduction of zinc influences the ligand field of Cr{sup III} and the Cr{sup III}-Cr{sup III} interactions in the LDH compound. It is found that both CdCr-LDH and ZnCdCr-LDH can be delaminated by dispersion in formamide, leading to translucent and stable colloidalmore » solutions.« less
  • Layered double hydroxides (LDHs) with the hydrotalcite type structure and a Mg:Al ratio of two have been prepared, with salicylate or naproxen in the interlayer. Two synthetic routes have been used: reconstruction from a mildly calcined hydrotalcite-CO{sub 3} precursor, and a coprecipitation method with chlorides of the metals. The solids have been characterized using several physicochemical techniques, i.e., powder X-ray diffraction, FTIR and {sup 13}C CP/MAS NMR spectroscopies and thermal analysis (thermogravimetric and differential thermal analyses). The gallery height determined is in all cases larger than the size of the drug, 11.5A for salicylate and 15.8 and 16.6A for naproxen,more » depending on the specific synthesis route followed. Experimental data suggest the anion molecules form a tilted bilayer, with the carboxylate groups pointing towards the brucite-like layers. The solids are stable up to 230{sup o}C and their evolution from 350{sup o}C upwards is very similar to that observed for a carbonate-containing hydrotalcite, forming mostly amorphous solids with a large specific surface area.« less
  • A core-shell structured magnetic layered organic-inorganic material involving 5-aminosalicylic acid (5-ASA) intercalated Zn-Al layered double hydroxides (LDHs) and magnesium ferrite (MgFe{sub 2}O{sub 4}) is assembled by a coprecipitation method. The powder X-ray diffraction results show the coexistence of the clear but weak diffractions of MgFe{sub 2}O{sub 4} and ordered relatively stronger reflections of 5-ASA intercalated LDHs. The TEM image of magnetic 5-ASA intercalated LDHs reveals that the LDHs layer covers the MgFe{sub 2}O{sub 4} particles or their aggregates with particle size of 50-80 nm. The vibration sample magnetization (VSM) measurements exhibit the increase in saturation magnetization of magnetic 5-ASA intercalatedmore » LDHs samples with increasing amount of magnetic core. The XPS analyses account for a majority of Zn, Al and O atoms on the surface of magnetic particles. It is suggested that the magnetic core MgFe{sub 2}O{sub 4} was coated with LDHs layer probably through Zn-O-Mg and Al-O-Mg linkages, and a core-shell structured model is tentatively proposed.« less
  • Chromate intercalated layered double hydroxides (LDHs) having the formula M{sup II} {sub 6}M'{sup III} {sub 2}(OH){sub 16}CrO{sub 4}.4H{sub 2}O (M{sup II} = Ca, Mg, Co, Ni, Zn with M'{sup III} = Al and M{sup II} = Mg, Co, Ni with M'{sup III} = Fe) have been prepared by coprecipitation. The products obtained are replete with stacking disorders. DIFFaX simulations show that the stacking disorders are of three kinds: (i) turbostratic disorder of an originally single layered hexagonal (1H) crystal (ii) random intergrowth of polytypes with hexagonal (2H) and rhombohedral (3R) symmetries and (iii) translation of randomly chosen layers by (2/3,more » 1/3, z) and (1/3, 2/3, z) leading to stacking faults having a local structure of rhombohedral symmetry. IR spectra show that the CrO{sub 4} {sup 2-} ion is incorporated either in the T {sub d} or in the C {sub 3v} symmetry. The interlayer spacing in the latter case is 7.3 A characteristic of a single atom thick interlayer showing that the CrO{sub 4} {sup 2-} ion is grafted to the metal hydroxide slab. On thermal treatment, the CrO{sub 4} {sup 2-} ion transforms into Cr(III) and is incorporated into the spinel oxide or phase separates as Cr{sub 2}O{sub 3}. In the LDH of Mg with Al, Cr(III) remains in the MgO lattice as a defect and promotes the reconstruction of the LDH on soaking in water. In different LDHs, 18-50% of the CrO{sub 4} {sup 2-} ion is replaceable with carbonate anions showing only partial mineralization of the water-soluble chromate. The extent of replaceable chromates depends upon the solubility of the corresponding LDH, which in turn is determined by the solubility of the MCrO{sub 4}. These studies have profound implications for the possible use of LDHs for chromate amelioration in green chemistry.« less
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