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schulzediss - Ni/Mg/Al catalysts derived from...

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Ni/Mg/Al catalysts derived from hydrotalcite-type precursors for the partial oxidation of propane. Synthesis and characterisation of physicochemical and catalytic properties Vom Fachbereich 6 (Chemie-Geographie) der Gerhard-Mercator-Universität – Gesamthochschule Duisburg zur Erlangung des akademischen Grades eines Doktors der Naturwissenschaften (Dr. rer. nat.) genehmigte Dissertation von Kai Schulze aus Duisburg Referent: Prof. Dr. Roman Dziembaj Korreferent: Prof. Dr. Günter Geismar Tag der mündlichen Prüfung: 11. Juli 2001
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Die vorliegende Arbeit entstand in der Zeit vom 4. März bis 14. August 1997 im Fachbereich 6 an der Gerhard-Merctor-Universität – Gesamthochschule Duisburg (Deutschland) unter Betreuung von Prof. Dr. Günter Geismar und vom 15. August 1997 bis 8. Juni 2001 an der Chemischen Fakultät der Jagiellonischen Universität in Krakau (Polen) unter Betreuung von Prof. Dr. Roman Dziembaj.
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Acknowledgements I would like to thank Prof. Dr. Roman Dziembaj for allowing me to work on this very interesting project, his invaluable assistance and all his support. I would also like to thank Prof. Dr. Günter Geismar for all his cooperation and his kind support. willingness to share his ideas on various issues and his constant support. Above all, I would like to recognise all the people that were involved in this work at the Jagiellonian University and the Gerhard-Mercator-University Duisburg. Without their support this work would have not been possible.
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For my mother
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Ni/Mg/Al catalysts derived from hydrotalcite-type precursors for the partial oxidation of propane. Synthesis and characterisation of physicochemical and catalytic properties Ph.D. thesis by Kai Schulze from Duisburg (Germany) submitted to the Gerhard-Mercator- University, Duisburg, Germany in June 2001 The work was performed from 4 th March 1997 to 14 th August 1997 at the Department of Inorganic Chemistry, Gerhard-Mercator-University, Duisburg, Germany, supervisor Prof. Dr. Günter Geismar and from 15 th August 1997 to 8 th June 2001 at the Faculty of Chemistry, Jagiellonian University, Krakow, Poland, supervisor Prof. Dr. Roman Dziembaj. Abstract Anionic clays of hydrotalcite-type structure of the approximate formula [Ni x Mg 72-x Al 28 (OH) 200 ][(NO 3 ) y (CO 3 ) (28-y)/2 ]· 50H 2 O (x = 0, 5, 10, 15, 30, 50, 72 and 11 y 16) were synthesised by coprecipitation at low supersaturation at pH 8 ± 0.2. Their composition and structure was determined by elemental analysis, XRD, TG-MS and DSC. Their calcination at temperature of well crystallised divalent metal oxide phases with periclase structure and spinel phases. At lower temperatures poorly crystallised divalent metal oxides and amorphous Al 2 O 3 phases with poorly crystallised spinel at their interfaces were formed. The degree of crystallinity increased with increasing calcination temperature. Catalysts with a lower nickel content exhibited remarkably high surface areas. This suggests that the fast removal of the gases formed during the calcination process combined with a slow heating rate had a beneficial influence on the catalysts’ preparation.
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