Inverse Liquid Chromatography for reaction catalyst monitoring

Lead Research Organisation: Imperial College London
Department Name: Department of Chemical Engineering

Abstract

The objective of the project is to develop a method for the characterisation of catalysts packed Liquid Chromatography (LC) column, whilst chemical reactions are occurring. Such an approach will expand the Inverse liquid chromatography (ILC) work already being carried out in the group. Such investigations for key catalyst properties, such as microporosity and pore size, have been previously reported via Inverse gas chromatography (IGC). However, a large majority of catalytic reactions occur in a liquid medium and therefore, in these circumstances' interactions between catalyst pores and solvent molecules, for example, are not accounted for.
An ILC based approach to catalyst characterisation would effectively allow simultaneous catalyst characterisation and reaction processes to occur. The unique approach would allow the critical relationship between catalyst performance and catalyst properties to be directly investigated.
Currently, the retrosynthesis and reaction monitoring for heterogenous catalysed reactions is both time consuming and inefficient. The main hypothesis of this proposal is that the ILC column would be an ideal reaction space for the analysis of changes in a catalysts physical and chemical properties, following a reaction, as the process allows both facile condition changes (solvent, temperature, pressure, pH, etc.) and tandem catalyst and product analysis. There are novel opportunities for analysing the changes in the physical properties of the catalyst, i.e. changes in pore / active site availability, surface area, site interaction energies and catalytic leeching into the reaction mixture.
The project aims to investigate whether catalytic reactions can be monitored and optimised using an ILC column, and to develop a reliable and repeatable methodology for catalytic reaction analysis and optimisation. It is theorised that this approach will provide an overall picture of catalyst-reaction material interactions during an optimisation process, while also enabling the rapid assessment of reactions involving molecules in which heteroatoms and functional groups may be changed to effect reaction mechanism and rate. This method will provide much needed information regarding the changes that occur on the catalytic surface when the stoichiometry, reactants or reaction conditions are varied. An initial "proof of concept test" would examine what changes in the catalysts physical and chemical properties might be monitored while also looking at other industrially critical phenomena such as catalytic leaching. The intention is that three different heterogenous catalytic systems would be investigated during the research programme. These systems would be chosen based on their industrial importance, academic interest and technical viability from a chromatographic instrumentation perspective. From each system it should be possible to determine different physical and chemical data and gain a complete picture of the ILC retrosynthetic catalyst analysis technique.
The research would be completed within the time frame of three to three and a half years, in addition to attending various seminars and professional skills courses organised by the chemical engineering department and others to develop communication skills and gain an insight into developing research areas.

Publications

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Studentship Projects

Project Reference Relationship Related To Start End Student Name
EP/R513052/1 01/10/2018 30/09/2023
2194350 Studentship EP/R513052/1 01/10/2018 31/03/2022 Sean McIntyre