Abstracts Chemistry

The application of additive manufacturing in flow chemistry and reaction monitoring

by Adam Price

Methods in which 3D printing can be used to make continuous flow processing more accessible to research groups have been developed. The 3D printing processes used were limited to affordable, desktop fused deposition modelling (FDM) and Stereolithography (SL) as to maintain accessibility and reproducibility of the work described herein. Chapter 1 contains a literature review, intended to give a clear background to the project. The literature review begins with an introduction to 3D printing and computer aided design (CAD) and explores its applications in chemistry research and education. The review then leads into an overview of the design and fabrication of bespoke 3D printed flow reactors with a focus on embedding sensors within reactor architectures for the purpose of in-line reaction monitoring. Methods of automated synthesis, reaction monitoring and the construction of self-optimizing flow systems are then explored with a brief overview of the algorithms that are often used to drive autonomous reaction optimisations and several examples of where unique 3D printed devices have been used to facilitate the integration of process analytical technologies (PAT) with synthetic platforms. Chapter 2 Details the development of an open-access, 3D printable 'toolkit' of common fittings and connectors required for constructing basic flow chemistry configurations. Included, within this toolkit are also several test boards that enable users to rapidly account for tolerances between modes and resulting prints. The toolkit components consist of male threaded nuts, junction connectors and a Luer adapter. The dual extrusion feature of an Ultimaker desktop 3D printer was used to combine the desired properties of multiple materials into single components such that mechanically strong parts could be fabricated that also had chemically resistant wettable flow channels. In addition to the printable toolkit, is the development of an easily customizable 3D printed flow reactor chip, the channel dimensions of which could be easily manipulated by using dimension adjusting slider bars within the user interface of 3D modelling software, Rhino 3D. All files within this chapter have been made freely available from Figshare and can all be printed in a matter of hours for users to begin constructing their own continuous flow reactor configurations. Chapter 3 outlines the development of a low-cost alternative to commercial flow Infra-red spectroscopy and examines its application in automated reaction monitoring. Using stereolithography, a bespoke flow cell was designed and produced that could be attached to a standard FT-IR spectrometer with ATR attachment to enable its installation into a flow process. Continuous spectral acquisition was achieved using a unique Matlab programme that obtained control over the Thermo Fisher IR control software, Omnic, by using scripted DDE commands. The system was used to monitor both the conversion of benzaldehyde to N-benzylideneaniline and its subsequent reduction to N-benzyl phenylamine in a single automated…