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Title: Continuous clean etherification
Author: Parrott, Andrew John
Awarding Body: University of Nottingham
Current Institution: University of Nottingham
Date of Award: 2011
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This thesis describes the use of continuous flow reactors as a technology to develop more sus­tainable chemical processes. The particular type of reaction chosen to explore this technology was the heterogeneous acid catalysed formation of ethers using benign alkylating agents with, and without, supercritical carbon dioxide as the solvent. Chapter 1 introduces Green Chemistry and outlines the main aims of this thesis. Chapter 2 describes the continuous flow equipment and analytical techniques used. Chapter 3 de­tails the investigation of several heterogeneous catalysts for the reaction of l-octanol with dimethyl carbonate, an alternative methylating agent. The most effective catalyst tested was y-alumina which was found to give the highest yield of the desired methyl ether over the largest temperature range. Chapter 4 explores this process further; the effect of several reaction parameters was in­vestigated. The scope of the reaction was also extended to include a range of primary and secondary aliphatic alcohols, and to ethylation reactions with diethyl carbonate. It was found that the reaction could be conducted with high yields when using y-alumina as the catalyst. The reaction could be conducted at ambient pressure without the need for a solvent or for a large excess of dialkyl carbonate. If the reaction was conducted at high pressure, the conver­sion of the starting alcohol was greatly reduced. However, when CO-, was used as the solvent, the reaction could be conducted at high pressure without significant reduction in yield. In Chapter 5 the synthesis of several ethers were used as probe reactions for the development of a new reactor system capable of conducting multi-factorial optimisation of continuous re­actions autonomously. This greatly accelerated the rate of optimisation compared to previous techniques. Finally Chapter 6 summarises the thesis and evaluates the progress made towards the aims initially outlined in Chapter I. An Appendix on a CD contains some of the key programs developed during this thesis.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available