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Synthesis and characterization of carbon nanomaterials using BIS(acetylacetonato)oxovanadium(IV), Manganese(III) Acetylacetonate, Co-Zn and CoAI as catalyst precursors.Ndwandwe, Silindile Nomathemba. 07 1900 (has links)
Thesis. (M.Tech. (Chemistry)) -- Vaal University of Technology, 2011. / Bis(acetylacetonato)oxovanadium(IV), Manganese(III) acetylacetonate, Co-Zn and
Co-Al were prepared as catalyst precursors for the synthesis of carbon materials in
a catalytic chemical vapor deposition (CCVD) reactor. The carbon materials
produced were characterized with Raman spectroscopy, Scanning electron
microscope (SEM), Energy dispersive spectroscopy (EDS), X-ray diffraction (XRD),
High resolution transmission electron microscopy (TEM) and Thermogravimetric
analysis, (TGA).
Carbon material prepared from bis(acetylacetonato)oxovanadium(IV) catalyst
precursor showed the presence of carbon spheres with average diameter of 104μm
together with small traces of carbon nanotubes or amorphous carbon. Synthesis of
bis(acetylacetonato)oxovanadium(IV) catalyst precursor yielded approximately 92%
of carbon material. Carbon material prepared from Manganese(III) acetylacetonate
catalyst precursor showed the presence of carbon spheres with diameter of 87.5μm.
Synthesis of Manganese(III) acetylacetonate catalyst precursor yielded
approximately 97% of carbon material.
Carbon material produced from Co-Zn and Co-Al catalyst precursors showed the
presence of carbon nanotubes with small amounts of amorphous carbon. The use of
Co-Zn catalyst precursor yielded approximately 80% of carbon nanotubes, whereas
Co-Al catalyst precursor yielded approximately 98% of carbon nanotubes. / Vaal University of Technology; NRF; SASOL
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Synthesis of Gold Complexes From Diphosphine Ligands and Screening Reactions of Heterocyclic Acetylacetonato (ACAC) Ligands with Transitional Metal ComplexesNyamwihura, Rogers 08 1900 (has links)
Syntheses of diphosphine gold (I) complexes from gold THT and two ligands, 4, 5-bis (diphenylphosphino)-4-cyclopenten-1, 3-dione (BPCD) and 2,3-bis(diphenylphosphino)-N-phenylmaleimide (BPPM), were done separately. The reactions happened under ice conditions followed by room temperature conditions and produced two diphosphine gold (I) complexes in moderated yield. Spectroscopic results including nuclear magnetic resonance (NMR) and X-ray crystallography were used to study and determine the structures of the products formed. Moreover, X-rays of all newly synthesized diphosphine gold (I) complexes were compared with the known X-ray structures of other phosphine and diphosphine gold (I) complexes. There were direct resemblances in terms of bond length and angle between these new diphosphine gold (I) complex structures and those already published. For instance, the bond lengths and angles from the newly prepared diphosphine gold (I) complexes were similar to those already published. Where there were some deviations in bond angles and length between the newly synthesized structures and those already published, appropriate explanation was given to explain the deviation. Heterocyclic ligands bearing acetylacetonate (ACAC) side arm(s) were prepared from ethyl malonyl chloride and the heterocyclic compounds 8-hydroxylquinoline, Syn-2-peridoxyaldoxime, quinoxalinol and 2, 6-dipyridinylmethanol. The products (heterocyclic ACAC ligands) from these reactions were screened with transition metal carbonyl compounds in thermolytic reactions. The complexes formed were studied and investigated using NMR and X-ray crystallography. Furthermore, the X-ray structures of the heterocyclic ACAC ligand or ligand A and that of rhenium complex 1 were compared with similar published X-ray structures. The comparison showed there were some similarities in terms of bond length and bond angles.
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