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Synthesis and Twin Polymerization of Si(OCH2py)4 for Nitrogen-containing Carbon Materials

Scharf, S.; Notz, S.; Pfefferkorn, K.; Rüffer, T.; Formánek, P.; Hübner, R.; Selyshchev, O.; Madeira, T. I.; Zahn, D. R. T.; Lang, H.


The synthesis and twin polymerization (TP) of Si(OCH2py)4 (3a, py=2-cC5H4N; 3b, py=3-cC5H4N; 3c, py=4-cC5H4N) is discussed. The solid state structures of 3b, c were confirmed by single-crystal X-ray crystallography showing non-conventional H-bonding, forming 2D chains (3b) or 3D networks (3c). Thermally induced TP of 3a–c and their simultaneous polymerization with 2,2‘-spiro-bi[4H-1,3,2-benzodioxasiline] (4) is described. The resulting hybrid materials were characterized by 1H, 13C{1H}, and 29Si{1H} CP MAS NMR spectroscopy confirming the transformation of the SiOCH2 moieties into CH2 groups enabling the formation of the respective polymers. These results were supported by HAADF-STEM studies, displaying micro-structuring. Nitrogen-containing porous carbon materials C_1–C_3 show surface areas of 1300 and 1700 m2g-1, large pore volumes between 0.6–1.2 cm3g-1, and nitrogen contents of up to 3.1 at-%. X-ray photoemission spectroscopy reveal that pyrrolic, pyridine, and pyridone nitrogen atoms are present. If equimolar amounts of 3a–c and 4 are simultaneously polymerized in the presence of [Pd(OAc)2] (5), then the Pd nanoparticle-decorated material Pd@C_3 (900 m2g-1) was obtained, which showed k values of -0.083 and -0.066 min-1 in the reduction of methylene blue and methyl orange, proving the accessibility of the Pd NPs.

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