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  • B-N polymer embedded iron(0) nanoparticles as highly active and long lived catalyst in the dehydrogenation of ammonia borane.

B-N polymer embedded iron(0) nanoparticles as highly active and long lived catalyst in the dehydrogenation of ammonia borane.

Journal of nanoscience and nanotechnology (2013-08-02)
Sibel Duman, Onder Metin, Saim Ozkar
摘要

B-N polymer embedded iron(0) nanoparticles (NPs) were in-situ generated from the reduction of iron(III) acetylacetonate during the dehydrogenation of ammonia borane (AB) in THF solution at 40.0 +/- 0.5 degrees C. The iron(0) NPs could be isolated as powder from the reaction solution by centrifugation and characterized by UV-Vis, TEM, and XRD. They are redispersible in polar solvent such as THF and yet highly active catalysts in the dehydrogenation of AB providing a TOF value of 202 h(-1) at 40.0 +/- 0.5 degrees C. The catalytic activity of iron(0) NPs compare well with those of the known homogenous and heterogeneous precious metal catalysts reported so far. They are also long-life catalysts in the dehydrogenation of AB providing 1410 turnovers over 18 h at 40.0 +/- 0.5 degrees C. The poisoning experiments using carbon disulfide show that the dehydrogenation of AB catalyzed by iron(0) NPs is a heterogeneous catalysis. The catalytic dehydrogenation of AB in the presence of iron(0) NPs was followed by measuring the volume of hydrogen generated and by 11B-NMR spectroscopy. Our report also includes the results of a detailed kinetic study on the catalytic dehydrogenation of AB depending on the catalyst concentration, substrate concentration, and temperature. The dehydrogenation of AB produces sparingly soluble B-N polymers which provide just enough stability to the iron(0) NPs. The co-precipitation of some iron(0) NPs with the sparingly soluble polymers causes a slight decrease in the catalytic activity toward the end of dehydrogenation. However, iron(0) NPs embedded in B-N polymers appear to be an efficient catalyst in hydrogen generation from ammonia borane at moderate temperature.

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氨 溶液, 7 N in methanol
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氨, anhydrous, ≥99.98%
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铁, ≥99%, reduced, powder (fine)
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氮化硼试剂, powder, ~1 μm, 98%
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Hydrogen, ≥99.99%
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氨 溶液, 2.0 M in ethanol
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羰基铁, ≥97% Fe basis
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铁, powder, −325 mesh, 97%
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氨 溶液, 0.4 M in THF
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氨 溶液, 0.4 M in dioxane
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氨 溶液, 2.0 M in methanol
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铁, powder, <10 μm, ≥99.9% trace metals basis
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氨 溶液, 4 M in methanol
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铁, puriss. p.a., carbonyl-Iron powder, low in magnesium and manganese compounds, ≥99.5% (RT)
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氨 溶液, 2.0 M in isopropanol
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铁, chips, 99.98% trace metals basis
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铁, granular, 10-40 mesh, >99.99% trace metals basis
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铁, foil, thickness 0.1 mm, ≥99.9% trace metals basis
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铁, foil, thickness 0.25 mm, ≥99.99% trace metals basis
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铁, wire, diam. 1.0 mm, ≥99.9% trace metals basis
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铁, wire, diam. 1.0 mm, ≥99.99% trace metals basis
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铁, rod, diam. 6.3 mm, 99.98% trace metals basis
铁, IRMM®, certified reference material, 0.5 mm wire
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铁, wire, diam. 0.5 mm, ≥99.9% trace metals basis