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3D printing of versatile reactionware for chemical synthesis

Nature Protocols volume 11, pages 920–936 (2016)Cite this article

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Abstract

In recent decades, 3D printing (also known as additive manufacturing) techniques have moved beyond their traditional applications in the fields of industrial manufacturing and prototyping to increasingly find roles in scientific research contexts, such as synthetic chemistry. We present a general approach for the production of bespoke chemical reactors, termed reactionware, using two different approaches to extrusion-based 3D printing. This protocol describes the printing of an inert polypropylene (PP) architecture with the concurrent printing of soft material catalyst composites, using two different 3D printer setups. The steps of the PROCEDURE describe the design and preparation of a 3D digital model of the desired reactionware device and the preparation of this model for use with fused deposition modeling (FDM) type 3D printers. The protocol then further describes the preparation of composite catalyst–silicone materials for incorporation into the 3D-printed device and the steps required to fabricate a reactionware device. This combined approach allows versatility in the design and use of reactionware based on the specific needs of the experimental user. To illustrate this, we present a detailed procedure for the production of one such reactionware device that will result in the production of a sealed reactor capable of effecting a multistep organic synthesis. Depending on the design time of the 3D model, and including time for curing and drying of materials, this procedure can be completed in ∼3 d.

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Figure 1: Schematic representation of the concept of 'reactionware'.
Figure 2: Bench-top FDM and extrusion-based 3D printers used by the authors.
Figure 3: Examples of reactionware printed with acetoxy-silicone polymer and composites thereof.
Figure 4: 3D-printed reactionware used for fluidic applications in conjunction with in-line analytics.
Figure 5: 3D-printed reactionware for high-throughput hydrothermal screening applications.
Figure 6: The design and function of the reactionware device for which fabrication is described in this protocol.
Figure 7: Preparation of printer instruction files.
Figure 8: Preparation of acetoxy-silicone composite catalyst 'inks' for printing catalyst beds.
Figure 9: Transfer of semicomplete print between printers for multimaterial printing.
Figure 10: Function of the completed reactionware device and anticipated results.

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Acknowledgements

We gratefully acknowledge financial support from the EPSRC (grants EP/L023652/1, EP/K038885/1, EP/H024107/1, EP/K023004/1, EP/K021966/1, EP/I033459/1, EP/J015156/1, EVOBLISS EC 611640, EVOPROG EC 610730 and MICREAGENTS EC 318671 to L.C.), the Fundamental Research Funds for the Central Universities project (grants buctrc201510 and buctrc201530 to Y.-F.S. and L.C.) and the Royal Society Wolfson Foundation for a Merit Award. We acknowledge the work of M.D. Symes, R.S. Forgan, V. Sans, M.H. Rosnes and V. Dragone for their contributions to the development of the applications of this protocol.

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Authors and Affiliations

  1. International Research Centre for Soft Matter, Beijing University of Chemical Technology, Beijing, P. R. China

    Philip J Kitson, Chang-Gen Lin, Yu-Fei Song & Leroy Cronin

  2. WestCHEM, School of Chemistry, The University of Glasgow, University Avenue, Glasgow, UK

    Philip J Kitson, Stefan Glatzel & Leroy Cronin

  3. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing, P. R. China

    Wei Chen & Yu-Fei Song

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  1. Philip J Kitson
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Contributions

P.J.K. designed and performed the experiments, analyzed data and wrote the paper with guidance from L.C.; S.G. contributed extensively to the editing of the paper and with expertise in 3D printing theory and practice; W.C. and C.-G.L., supervised by Y.-F.S., contributed to the generalization of the protocol; L.C. conceived the idea, supervised the project and designed the experiments.

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Correspondence to Yu-Fei Song or Leroy Cronin.

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Competing interests

L.C. is a director of, and owns some shares in, Cronin Group PLC, set up to commercialize new approaches to design, discovery and digitization in chemistry.

Supplementary information

Supplementary Text and Figures

Supplementary Discussion, Supplementary Data 2 (PDF 9313 kb)

Supplementary Data 1

3D CAD Model Files including; Montmorillonite composite.stl Pd composite.stl Reactionware PP srchitecture.stl Reactionware.dwg Reactionware PP architecture.bfb (ZIP 549 kb)

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Kitson, P., Glatzel, S., Chen, W. et al. 3D printing of versatile reactionware for chemical synthesis. Nat Protoc 11, 920–936 (2016). https://doi.org/10.1038/nprot.2016.041

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