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Synthesis of highly reactive subnano-sized zero-valent iron using smectite clay templates.

ABSTRACT: A novel method was developed for synthesizing subnano-sized zero-valent iron (ZVI) using smectite clay layers as templates. Exchangeable Fe(III) cations compensating the structural negative charges of smectites were reduced with NaBH(4), resulting in the formation of ZVI. The unique structure of smectite clay, in which isolated exchangeable Fe(III) cations reside near the sites of structural negative charges, inhibited the agglomeration of ZVI resulting in the formation of subnanoscale ZVI particles in the smectite interlayer regions. X-ray diffraction revealed an interlayer spacing of approximately 5 A. The non-structural iron content of this clay yields a calculated ratio of two atoms of ZVI per three cation exchange sites, in full agreement with the X-ray diffraction (XRD) results since the diameter of elemental Fe is 2.5 A. The clay-templated ZVI showed superior reactivity and efficiency compared to other previously reported forms of ZVI as indicated by the reduction of nitrobenzene; structural Fe within the aluminosilicate layers was nonreactive. At a 1:3 molar ratio of nitrobenzene/non-structural Fe, a reaction efficiency of 83% was achieved, and over 80% of the nitrobenzene was reduced within one minute. These results confirm that non-structural Fe from Fe(III)-smectite was reduced predominantly to ZVI which was responsible for the reduction of nitrobenzene to aniline. This new form of subnanoscale ZVI may find utility in the development of remediation technologies for persistent environmental contaminants, for example, as components of constructed reactive domains such as reactive caps for contaminated sediments.

SUBMITTER: Gu C

PROVIDER: S-EPMC2892840 | biostudies-literature | 2010 Jun

REPOSITORIES: biostudies-literature

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Synthesis of highly reactive subnano-sized zero-valent iron using smectite clay templates.

Gu Cheng C Jia Hanzhong H Li Hui H Teppen Brian J BJ Boyd Stephen A SA

Environmental science & technology 20100601 11

A novel method was developed for synthesizing subnano-sized zero-valent iron (ZVI) using smectite clay layers as templates. Exchangeable Fe(III) cations compensating the structural negative charges of smectites were reduced with NaBH(4), resulting in the formation of ZVI. The unique structure of smectite clay, in which isolated exchangeable Fe(III) cations reside near the sites of structural negative charges, inhibited the agglomeration of ZVI resulting in the formation of subnanoscale ZVI parti ...[more]

PMID: 20446730

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Project description:Polymer-clay nanocomposites have greater thermal stability compared to the pristine polymer matrix. This can be attributed to the physical barrier provided by the inclusion of 2D clay nanoparticles (especially of the smectite group), together with radical trapping related to the distribution of specific 3d atoms in the inorganic phase. To elucidate the relevance of the Fe3+ distribution in this synergic effect, the iron atoms present in octahedral sheets of natural nontronite clay (Non, 5.6 wt % Fe) or in maghemite (M) nanoparticles (γ-Fe2O3) were incorporated in a poly(methyl methacrylate) (PMMA) matrix. Na-laponite (Lap) clay was used to evaluate the contribution of the diffusion barrier effect to the increased thermal stability of a PMMA-Lap nanocomposite, as evidenced by the upshift of the thermogravimetric (TGA) curve compared to that for PMMA. The contribution of radical trapping to the thermal stability of the PMMA-Non nanocomposite was evidenced by a significant shift of the Fe K-edge rising edge position by -4.5 eV after iron reduction by heating in N2, while similar treatment of pristine nontronite did not lead to a significant rising edge shift in the X-ray absorption spectra (XAS). This downshift demonstrated the reduction of Fe3+ to Fe0, induced by the sequestration of radicals formed by PMMA depolymerization. Raman spectroscopy analysis evidenced the formation of graphitic char deposits above 400 °C, further improving the thermal stability of PMMA-Non by providing an additional physical barrier to mass transport. A fourth contribution of well-dispersed iron was the abstraction of carbon from the char by the iron carburization reaction, which hindered CO2 formation by oxidative coking. In contrast, no relevant contribution of graphitic layer deposition was observed for the PMMA-M-Lap nanocomposite, where its improved thermal stability was only due to the combined contributions of the gas diffusion barrier effect and radical trapping by iron atoms. The maghemite effectively captured the radicals confined by the clay sheets, resulting in significant stabilization of the nanocomposite, with a shift of the mass loss of the PMMA-M-Lap nanocomposite compared to PMMA-Lap.

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Synthesis of highly reactive subnano-sized zero-valent iron using smectite clay templates.

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Synthesis of highly reactive subnano-sized zero-valent iron using smectite clay templates.

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