Application-led, online analysis for the continuous production of Metal-Organic Frameworks (MOFs)

Abstract

Metal-organic frameworks (MOFs) are a class of hybrid functional materials.1 Modular in nature and highly tuneable, they have been used in a wide range of applications such as adsorption,2 gas separation,3 and catalysis.4 Generally, MOFs are solvothermally made in batch-type processes and their analysis and property assessment requires considerable time and chemist intervention. Successful flow synthesis of MOFs with improved space-time yield, enhanced uniformity and quality of crystals have been published in recent years and developed in this work.5-7 However, there is currently no means for the inline characterisation of the MOF product, such that optimisation of in-flow MOF synthesis is complex and labour intensive.
This work investigates a qualitatively distinct approach. Using in-line UV-Vis during continuous production, an application-led focus is implemented whereby the amount of synthesised MOF is assessed based on its performance against a target application. The final system contains a synthetic, application and separation element with a final in-line UV-Vis spectrometer which produces real-time data on the process fluid. The chosen system used was HKUST-1 and the target application was adsorption of organic dye methylene blue.
The work presented in this thesis describes an established set-up that can quantifiably assess HKUST-1s ability to adsorb methylene blue during continuous synthesis. Not only does this prove the concept of ‘application-led’ analysis for the first time, but it helps to bridge the gap within future MOF production. By producing MOFs in flow while gathering in-situ analytical data on their adsorption ability this setup can act as a quality assurance tool for high throughput experimentation.

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Identifiers

ORCID for Adrian Nightingale: orcid.org/0000-0003-2445-4827

ORCID for Darren Bradshaw: orcid.org/0000-0001-5258-6224

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