Multifunctional Electrochemical Flow Platform for High-Throughput Synthesis & Optimisation of Catalysts

We will develop new technology that greatly accelerates the process of discovering, developing and implementing sustainable organometallic catalysts for industrially-relevant reactions.
Many reactions in pharmaceutical, agrochemical and fine chemicals processes require metal catalysts which rely on platinum group metals (PGMs) such as palladium, platinum and rhodium. PGMs are expensive and are on the European Commission's 2014 list of 20 critical raw materials (http://eur-lex.europa.eu/legal-content/EN/TXT/?uri=CELEX:52014DC0297), which possess serious risk of dwindling supply. Furthermore, PGMs are toxic, hence must be removed from final products to levels that are often difficult/costly to achieve (<5ppm for active pharmaceutical ingredients). The currently increasing use of PGMs in the chemicals industry is therefore untenable in the medium to long-term.
Base-metals such as copper and iron are much more attractive to use as catalysts due to being significantly more abundant and typically having lower toxicity (depending upon speciation). Despite this, the use of base-metals in catalysis is rare in industry; a lack of understanding of the active species and mechanistic profiles of base-metal catalysts, which are more challenging to study than PGMs, means that reactions are unpredictable and often irreproducible. In addition, high catalyst loadings and harsh reaction conditions (when compared to, for example, palladium-catalysed reactions) are usually required.
Catalysts are generally discovered and developed using a linear process, whereby a catalyst is designed and synthesised, tested and optimised in a specific reaction, examined for substrate scope under optimised conditions, and redesigned to try and produce more active and selective (2nd generation) catalysts. In addition to being slow and labour intensive, this process risks overlooking potentially valuable catalysts. For example, due to time constraints, a 2nd generation catalyst may only be tested under conditions that are optimum for the 1st generation catalyst, when alternative and improved conditions could be more suitable.
This proposal seeks to bring together a range of complementary expertise across chemistry and engineering to develop new technology that is capable of rapidly synthesising, screening and self-optimising base-metal catalysts. Both the catalyst synthesis and catalytic reaction stages will be performed in flow cells, which enables online analysis of the output at each stage, and allows modification of the conditions as the reactions are running. Algorithms will be used so that the reactions become self-optimising i.e. conditions are automatically varied in response to the analytical data, enabling several sets of conditions to be screened for a number of catalysts within a relatively short period of time.
Our aim is for the technology to be adopted by both academic and industrial laboratories for the development of catalysts more broadly. We will make all information relating to reactor designs, variables, algorithms etc. open access, so that other researchers can replicate and apply the technology. Data relating to base-metal catalysed reactions will be added to a searchable database; this will provide a valuable resource to others studying these types of reactions, enabling a more knowledge-based and frontier-leading approach to catalyst development.

Organometallic catalysis is an essential area of scientific research, directly impacting on chemical industries worldwide, such as pharmaceuticals, agrochemicals and materials. For these industries to survive and grow, they must work towards a sustainable future, which includes reducing demand on diminishing resources such as platinum group metals (PGMs), or using them in a more efficient manner (e.g. recovering from waste streams and recycling). The proposed research will result in a new flow technology for rapid synthesis, screening and optimisation of catalysts, with a focus on base-metal catalysis. The data generated in this research will benefit chemical industries, as greater understanding of base-metal catalysed processes will be achieved with new and optimised catalysts being discovered. This project will move base-metal catalysed processes towards being 'fit for purpose' for industry. Through working with the industrial advisory board, industrially-relevant processes will be identified and studied. Furthermore, the technology will be developed so that it can be translated into industry for reaction screening (i.e. catalyst discovery and optimisation), or be scaled up for synthesis (i.e. catalyst generation and catalytic reactions on a large scale). It is envisaged that the technology will be adopted for broader use, including making reactions that can only be catalysed by PGMs more efficient, and using the electrochemical technology for metal recovery/recycling.
In providing a technology and generating data and valuable knowledge that will benefit chemical industries, this research will ultimately have a positive impact on society. New and improved pharmaceuticals, agrochemicals and materials will be developed, giving society better healthcare, food security and technology. More efficient and sustainable routes to known compounds will also lead to reduced costs.
This research will have an impact on academics across several areas of the physical sciences. Those working in organometallic chemistry and catalysis will benefit from the technology, as more efficient routes to catalyst synthesis, reaction screening and optimisation will be available. The data generated and searchable databases developed will also be valuable to researchers in these areas, in addition to those working in mechanistic and physical organic chemistry. Information relating to the technology will be valuable to process chemists and chemical engineers, as it can be translated to flow-reactors for similar or different purposes.
All researchers involved will benefit significantly from having the opportunity to carry out this programme of research. The PDRAs will expand their research and technical skills in areas that are of direct relevance to industry, such as organic/organometallic synthesis and analysis, catalysis and chemical engineering. They will benefit from working with a multi-disciplinary team, in addition to liaising with members of the industrial advisory board. They will have ample opportunity to present results to a range of audiences (conference, industrial and departmental meetings) and will be involved in manuscript preparation, thus strengthening skills of importance to future employers. Further training in generic skills such as research management and public engagement will be offered through courses. The PI and CoIs will benefit hugely from having the opportunity to work together and become an internationally-leading team in electrochemical flow technology for metal catalyst screening and optimisation. In addition to the anticipated outputs from this specific research, it is likely to lead to future collaboration with other internationally-leading researchers.