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URN: urn:nbn:de:bsz:25-opus-6914
URL: http://www.freidok.uni-freiburg.de/volltexte/691/

Abu-Shandi, Khalid Hamad

Metal phosphates: From syntheses and structures to applications in sorption, catalysis and teeth erosion protection

Metall-Phosphate: Von der Synthese und Struktur zu Anwendungen bei der Absorption, Katalyse und Zahnerosionsschutz

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Kurzfassung in Deutsch

As a synthetic route a hydrothermal procedure with organic amines as templates. The electronic aspects were investigated in collaboration by using Moessbauer spectroscopy. The synthesized new compounds were structurally analyzed by single crystal X-ray diffraction. The thermal properties and stability were investigated using thermogravimetry (TGA) together with X-ray powder diffractometry (XRPD) to elucidate the loss of guest molecules and the stability of the host framework. Crystals grown from the reaction of piperazinedium phosphate, (C4H12N2)(HPO4)2 with Co(II) or Ni(II) at normal pressure and temperature gave only a hydrogen-bonded framework of composition [M(H2O)6](C4H12N2)(HPO4)2 (M = Co, Ni). Also, the compound [Cu(H2PO4)2(4,4'-bipy)2(H2O)2], prepared by non-hydrothermal routes. Thus, the hydrothermal treatment of 1,3-diaminopropane or 1,4-diaminobutane with iron(III) chloride and phosphoric acid in yielded in both cases the 3-D framework {[NH4][FeIII2(OH)(PO4)2(H2O)]•H2O}n (A). The 3-D mixed-valence iron phosphate {FeII5FeIII2(PO4)2(H0.5PO4)4}n was obtained hydrothermally starting with N-methylpiperazine and FeIICl2. Compounds {[FeII(H2PO4)2(4,4'bipy) (H2O)]•H2O•4,4'-bipy}n and {[FeIII(NO3)2(4,4'-bipy)(H2O)2](OH)(H2O)}n are 1-D coordination polymers. Compounds {[C4H12N2][FeIII3(PO4)3(HPO4)(H2O)]}n (B, 3-D) and mixed-valence {[C4N2H11.6]1.5[FeIIFeIII(PO4)(H0.8PO4)2]•H2O}n (1-D) have been synthesized using a similar hydrothermal method (starting from FeIICl2). The guest species from the open-framework materials A and B together with a gallium analog of B and the literature material {[H3N(CH2)6NH3]4[Ga16(PO4)14 (HPO4)2(OH)2F7]•6H2O}n (C) could be removed (followed by TGA) with the framework proven to remain intact (by XRPD). The resulting guest-depleted open-framework showed sorption activities for different types of organic compounds. Materials B and C but not A exhibited catalytic properties in the regioselective oxidation of n-pentane to 3-pentanol.

SWD-Schlagwörter: Phosphate , Katalyse , Absorption
Institut: Institut für Anorganische und Analytische Chemie
Fakultät: Fakultät für Chemie und Pharmazie (bis Sept. 2002)
DDC-Sachgruppe: Chemie
Dokumentart: Dissertation
Erstgutachter: Janiak, Christoph (Prof. Dr.)
Sprache: Deutsch
Tag der mündlichen Prüfung: 08.05.2003
Erstellungsjahr: 2003
Publikationsdatum: 15.05.2003