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Title: Novel routes to potential packed bed absorbents for the desulphiding reaction
Author: Pringle, Tom
Awarding Body: University of Edinburgh
Current Institution: University of Edinburgh
Date of Award: 1999
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Three interdependent areas of investigation were conducted in order to formulate a repeatable, reliable and simple set of procedures to synthesize, characterize and assess the potential desulphiding ability of the synthesized materials. The exclusion of atmospheric carbon dioxide throughout the sequence of preparation, characterization and assessment and the transfer processes between these stages was a key component of the design strategy and final success of these procedures. The three areas of investigation were: (i) synthesis of precursor materials; (ii) development of air-free apparatus and regimes for the hydrolysis of precursors and the collection and transfer of hydrolysis products to air-free apparatus for analysis and; (iii) investigation of the properties of the products using purpose built equipment. The aim of the syntheses was to prepare contaminant free samples of ZnO, Zn(OH)2 or any other structurally modified compounds of zinc which may have activity as desulphiding reagents. The hydrolysis of zinc-based complexes containing oxygen-donor ligands was found to be a productive route to generating such structurally modified compounds of zinc. Basic zinc carboxylates (in particular hexakis(μ-2-acetato-O-O')-(μ-4-oxo)-tetrazinc, Zn4O(O2CCH3)6) were found to be the simplest to prepare, with good yields and high levels of purity (ascertained by the absence of surface carbonate contaminants). These offered a rich source of structurally novel materials. The preparation of these materials led to the crystallographic determination of the structure of hexakis[μ-(propanato-O:O')]-μ4-oxotetrazinc, Zn4O(O2CCH2CH3)6. Two novel acetates of zinc were also discovered by sublimation of the neutral acetate. These have been assigned as the novel acetates Zn8O3(O2CCH3)10 and Zn2(O2CCH3)4. In addition, mass spectral evidence supports the proposed existence of related multi-nuclear propionates.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available