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Title: Polysulfide intercalated layered double hydroxides for metal capture applications

Abstract

Polysulfide intercalated layered double hydroxides and methods for their use in vapor and liquid-phase metal capture applications are provided. The layered double hydroxides comprise a plurality of positively charged host layers of mixed metal hydroxides separated by interlayer spaces. Polysulfide anions are intercalated in the interlayer spaces.

Inventors:
;
Publication Date:
Research Org.:
Idaho National Lab. (INL), Idaho Falls, ID (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1349735
Patent Number(s):
9,610,538
Application Number:
14/715,768
Assignee:
Northwestern University INL
DOE Contract Number:
AC07-05ID14517
Resource Type:
Patent
Resource Relation:
Patent File Date: 2015 May 19
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Kanatzidis, Mercouri G., and Ma, Shulan. Polysulfide intercalated layered double hydroxides for metal capture applications. United States: N. p., 2017. Web.
Kanatzidis, Mercouri G., & Ma, Shulan. Polysulfide intercalated layered double hydroxides for metal capture applications. United States.
Kanatzidis, Mercouri G., and Ma, Shulan. Tue . "Polysulfide intercalated layered double hydroxides for metal capture applications". United States. doi:. https://www.osti.gov/servlets/purl/1349735.
@article{osti_1349735,
title = {Polysulfide intercalated layered double hydroxides for metal capture applications},
author = {Kanatzidis, Mercouri G. and Ma, Shulan},
abstractNote = {Polysulfide intercalated layered double hydroxides and methods for their use in vapor and liquid-phase metal capture applications are provided. The layered double hydroxides comprise a plurality of positively charged host layers of mixed metal hydroxides separated by interlayer spaces. Polysulfide anions are intercalated in the interlayer spaces.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Tue Apr 04 00:00:00 EDT 2017},
month = {Tue Apr 04 00:00:00 EDT 2017}
}

Patent:

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  • We demonstrate strong iodine (I-2) vapor adsorption using Mg/Al layered double hydroxide (MgAl-LDH) nanocomposites intercalated with polysulfide (S-x(2-)) groups (S-x-LDH, x = 2, 4, 6). The as-prepared LDH/polysulfide hybrid materials display highly efficient iodine capture resulting from the reducing property of the intercalated polysulfides. During adsorption, the I-2 molecules are reduced to I-3(-) anions by the intercalated [S-x](2-) groups that simultaneously are oxidized to form S8. In addition to the chemical adsorption, additional molecular I-2 is physically captured by the LDH composites. As a result of these parallel processes, and despite their very low BET surface areas, the iodine capturemore » capacities of S-2-LDH, S-4-LDH, and S-6-LDH are similar to 1.32, 1.52, and 1.43 g/g, respectively, with a maximum adsorption of 152% (wt %). Thermogravimetric and differential thermal analysis (TG-DTA), energy dispersive X-ray spectroscopy (EDS), and temperature-variable powder X-ray diffraction (XRD) measurements show the resulting I-3(-) ions that intercalated into the LDH gallery have high thermal stability (>= 350 degrees C). The excellent iodine adsorption performance combined with the facile preparation points to the S-x-LDH systems as potential superior materials for adsorption of radioactive iodine, a waste product of the nuclear power industry.« 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
  • 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
  • trans-RhCl(CO)(TPPTS){sub 2} (TPPTS=tris(m-sulfonatophenyl)phosphine) has been intercalated into Zn-Al layered double hydroxides (LDHs) by the method of ion exchange. The structure, composition and thermal stability of the composite material have been characterized by powder X-ray diffraction, Fourier transform infrared and {sup 31}P solid-state magic-angle spinning nuclear magnetic resonance spectroscopy, elemental analysis, thermogravimetry, and differential thermal analysis. The geometry of trans-RhCl(CO)(TPPTS){sub 2} was fully optimized using the PM3 semiempirical molecular orbital method, and a schematic model for the intercalated species has been proposed. The thermal stability of trans-RhCl(CO)(TPPTS){sub 2} is significantly enhanced by intercalation, which suggests that such materials may have prospectivemore » application as the basis of a supported catalyst system for the hydroformylation of higher olefins.« 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