Integrated 3D-printed reactionware for chemical synthesis and analysis

Abstract

Three-dimensional (3D) printing has the potential to transform science and technology by creating bespoke, low-cost appliances that previously required dedicated facilities to make. An attractive, but unexplored, application is to use a 3D printer to initiate chemical reactions by printing the reagents directly into a 3D reactionware matrix, and so put reactionware design, construction and operation under digital control. Here, using a low-cost 3D printer and open-source design software we produced reactionware for organic and inorganic synthesis, which included printed-in catalysts and other architectures with printed-in components for electrochemical and spectroscopic analysis. This enabled reactions to be monitored in situ so that different reactionware architectures could be screened for their efficacy for a given process, with a digital feedback mechanism for device optimization. Furthermore, solely by modifying reactionware architecture, reaction outcomes can be altered. Taken together, this approach constitutes a relatively cheap, automated and reconfigurable chemical discovery platform that makes techniques from chemical engineering accessible to typical synthetic laboratories.

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Figure 1: The Fab@Home Version 0.24 RC6 freeform fabricator.
Figure 2: The synthesis and crystallization of polyoxometalates in the 3D-printed reactionware.
Figure 3: The synthesis of heterocycle 3 in 3D-printed reactionware.
Figure 4: The 3D-printed reactionware used for in situ spectroscopies.
Figure 5: The 3D-printed electrochemical cell and electrodes.
Figure 6: The 3D-printed reactionware-assisted selective syntheses of C22H20N2O (4) and C22H19BrN2O (5).

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Acknowledgements

This work was supported by the Engineering and Physical Sciences Research Council UK via Creativity@HOME. L.C. thanks the Royal Society/Wolfson Foundation for a Merit Award. We thank R.M. Eadie (University of Glasgow) for samples of 2-bromoethylphenanthridinium bromide and E. Malone and K. Kondo (NextFab Studio, Philadelphia) for assistance with building the fabricator.

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Authors

Contributions

L.C. conceived the idea and the organized the fabricator assembly, M.D.S., P.J.K., T.V., G.J.T.C. and R.W.B. designed the reactionware, M.D.S. and P.J.K. printed the devices, M.D.S., P.J.K., J.Y. and C.J.R. performed the experiments, L.C., M.D.S, P.J.K., J.Y. and C.J.R. analysed the results and M.D.S. and L.C. co-wrote the paper.

Corresponding author

Correspondence to Leroy Cronin.

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The authors declare no competing financial interests.

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Supplementary Movie 1 (MOV 15090 kb)

Supplementary Movie 2

Supplementary Movie 2 (MOV 9654 kb)

Supplementary information

Crystallographic data for compound 1 (CIF 37 kb)

Supplementary information

Crystallographic data for compound 2 (CIF 27 kb)

Supplementary information

Crystallographic data for compound 3 (CIF 15 kb)

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Symes, M., Kitson, P., Yan, J. et al. Integrated 3D-printed reactionware for chemical synthesis and analysis. Nature Chem 4, 349–354 (2012). https://doi.org/10.1038/nchem.1313

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