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1530-1600 Dr. Chris Tighe (Department of Chemical Engineering, Imperial College London)
Scaling Up a Continuous Supercritical Hydrothermal Process for the Manufacture of Inorganic Nanoparticles
Abstract: Inorganic nanoparticles, most commonly in the form of the oxides of metals, but also their nitrides and sulphides, are in increasing demand in applications as diverse as energy storage, healthcare and electronics. Their small size imparts a plethora of desirable (although admittedly in certain cases, undesirable) properties, such as a high specific surface area on which chemical and, or electrochemical reactions can occur, low temperature sintering and colloidal stability. For many decades, such nanoparticles have been synthesised from aqueous metal salts using batch hydrothermal methods i.e. in hot water, usually just a little above its normal boiling point, and therefore under pressure to keep it in liquid form. Stirred autoclaves were used, with reaction times of several hours or sometimes even days required to yield the desirable, crystalline form of the product. In the early 90’s, Adshiri and Arai at Tohuku University in Japan discovered that the same nanoparticles could be made in matter of seconds, by rapidly mixing aqueous metal salts at ambient temperature with water above its critical point (22.1 MPa and 374 °C). Thus the continuous supercritical hydrothermal process was born, imported into the UK by Poliakoff and co-workers at Nottingham University, and subsequently UCL and ICL. In this talk, I will describe the development a new confined jet reactor for the synthesis of nanoparticles at the lab scale, and its subsequent scale up. The advantages of using a continuous process over batch will be discussed, and opportunities for improvement will be highlighted. Finally, a techno-economic analysis will show that for high value materials, the process is very attractive, offered credence by the decision of Hanwha Corporation of South Korea to select this route for the large scale manufacture of lithium iron phosphate, forming the cathode of a rechargeable lithium-ion battery.
About the speaker: Dr Chris Tighe is a Lecturer in the Department of Chemical Engineering at ICL and PI of the High Pressure Industrial Systems Group.
1605-1705 Professor Oliver Kappe (University of Graz)
Going with the Flow – The Use of Continuous Processing in Organic Synthesis
Abstract: Continuous flow processes form the basis of the petrochemical and bulk chemicals industry where strong competition, stringent environmental and safety regulations, and low profit margins drive the need for highly performing, cost effective, safe and atom efficient chemical operations. In contrast to the commodity chemical industry, however, the fine chemical industry primarily relies on its existing infrastructure of multipurpose batch or semi-batch reactors. Fine chemicals, such as drug substances and active pharmaceutical ingredients (APIs), are generally considerably more complex than commodity chemicals and usually require numerous, widely diverse reaction steps for their synthesis. These requirements generally make versatile and reconfigurable multipurpose batch reactors the technology of choice for their preparation. However, the advantages of continuous flow processing are increasingly being appreciated also by the pharmaceutical industry and, thus, a growing number of scientists, from research chemists in academia to process chemists and chemical engineers in pharmaceutical companies, are now starting to employ continuous flow technologies on a more routine basis.1
In this lecture, contributions from our research group in the field of continuous flow processing will be highlighted. Emphasis will be given to highly atom efficient and process intensified chemical transformations useful for the synthesis of APIs or key intermediates that are often too hazardous to be executed in a batch reactor. These involve azide, diazomethane and nitration chemistry, selective precious metal-free olefin and nitrogroup reductions, oxidation reactions involving pure oxygen, and flow photochemistry applications.
1 Review: Gutmann, B.; Cantillo, D.; Kappe, C. O. Angew. Chem. Int. Ed. 2015, 54, 6688.
About the speaker: C. Oliver Kappe received his undergraduate and graduate education at the University of Graz with Professor Gert Kollenz. After periods of postdoctoral research work with Professor Curt Wentrup at the University of Queensland and with Professor Albert Padwa at Emory University, he moved back to the University of Graz in 1996 to start his independent academic career. In 1999 he became Associate Professor and in 2011 was appointed Full Professor for “Technology of Organic Synthesis” at the University of Graz. Professor Kappe has an extensive general experience and a 25-year track record in synthetic and physical organic chemistry, process intensification using batch microwave technology and flow chemistry/microreaction technology, communicated in ~400 scientific publications (h-Index 73). His current research interests involve continuous flow chemistry, API manufacturing, and process intensification technologies. Since 2011 he is Editor-in-Chief of the Journal of Flow Chemistry.