INTEGRATED 3D PRINTED REACTIONWARE FOR CHEMICAL SYNTHESIS AND ANALYSIS PDF

Abstract 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. T he use of three-dimensional 3D printing technologies by individuals promises to bypass sophisticated manufacturing centres and revolutionize every part of the way that materials are turned into functional devices, from design through to oper-ation1,2.

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Richmond1, Geoffrey J. Cooper1, Richard W. 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. Furthermore, solely by modifying reactionware architecture, reaction outcomes can be altered. T he use of three-dimensional 3D printing technologies by parameters regarding the dimensions of these devices could be individuals promises to bypass sophisticated manufacturing adjusted digitally during the computer-aided design process with centres and revolutionize every part of the way that materials great ease, and subsequent printing could be automated effectively.

Hence, we were able to applications of this technology remain limited. Cronin glasgow. All rights reserved. The white area below the printing head is a square of ordinary paper onto which the reactionware was printed.

Protons are omitted for clarity. The device was then printed of the reaction chamber resealed spontaneously, making the using a robust, quick-curing acetoxysilicone polymer Loctite chamber watertight. The subsequent crystallization events were bathroom sealant, LOCTITE as the primary material and monitored through the transparent viewing window incorporated inserting the non-printable components glass frit and microscope into the device see Supplementary Video S1.

When bly. An aqueous solution of CoCl2 was printed that is, dispensed crystals of a suitable size had formed typically within 10—60 by the printer into one solution-holding chamber and an acidic sol- minutes the crystallization device was cut in half with a scalpel ution of the dilacunary polyoxotungstate [Se2W19O67 H2O ] and the crystals were removed and analysed by X-ray crystallogra- prepared using an adapted literature procedure25 was printed phy, Fourier transform infrared spectroscopy, thermogravimetric into the other holding chamber see Supplementary Information.

The two solutions remained in their respective chambers and did The crystal structure of 1 Fig. This the mixing chamber, through the frit and into the lower reaction core contains an octahedral WO6 unit and two CoO6 centres. One chamber at a controlled rate. Grey, black, light blue and pink represent protons, C, N and O, respectively. Relative absorbances are normalized at nm. The active surface area of the ITO working electrode was 2. CoO6 units, and the terminal water ligand on one Co centre is sub- Information for experimental details and full characterization stituted by a chloride.

It is interesting that, in addition to a certain by the reaction of 4-aminophenol, Et3N and 5- 2-bromoethyl number of amines acting as cations and hydrogen bonding to the phenanthridinium bromide in methanol see Supplementary cluster, extra dimethyl ammonium ions are also disordered Information for a discussion of solvent compatibilities in the around the cluster in the crystal structure.

Hence, we speculate as-printed devices. On mixing in the 3D-printed reactionware, that the excess of dimethyl ammonium hydrochloride accelerates the reaction mixture turned an amber colour, and crystals of 3 the crystallization process allowing single crystals to form in only suitable for X-ray diffraction were obtained from the liquor a few minutes , whereas no single crystalline product can be isolated after 96 hours.

The structure thus obtained is shown in after a week if amines are absent. Crystallographic unit-cell checks established that this the ITO-coated surface faced into the reaction chamber. Initially, compound had the same structure as compound 1 see the central chamber of the device was charged with 2 ml of an Supplementary Information. Cycles from Moreover, on termination of the potential cycling at The input light source was provided by a W broad-spectrum Hg arc lamp, which was clamped below the apparatus such that the sample was irradiated from below, through the ITO window, during acqui- sition of the spectra.

Comparison of the spectra obtained before and after the cyclic voltammogram Fig. By equipping the reactionware with a small stir bar, the solution could be stirred mag- netically the stir plate was held to the side of the cell, see Fig. Hence, we were able to perform bulk electrolysis on the sample the c ITO working electrode was poised at —0.

Such studies show that robocast 3D-printed reactionware is suitable for both spectroscopic analyses and bulk synthetic and electrosynthetic processes. In addition to utilizing traditional electrodes within a 3D-printed cell, we were also able to 3D print entire electrochemical cells using the Fab Home platform.

For example, an acetoxysilicone polymer before curing was mixed with toluene to make a thinned gel, which was then mixed with conductive carbon black to produce a conductive paste suitable for loading into the 3D printer see Supplementary Information and Supplementary Fig. S7 for d 0 details. A basic electrochemical cell was then produced, whereby two parallel lines of this conductive paste were printed onto a glass slide, about 0. The glass slide was employed solely to aid visu- Charge mC alization of the ensuing electrochemical reactions, and various func- tional architectures for electrochemical cells can be envisioned using —80 solely printed components.

The two electrodes of the cell were then connected to a three-elec- trode potentiostat, as shown in Fig. Within a few minutes, the yellow polyoxometalate solution had started to turn blue around Figure 5 The 3D-printed electrochemical cell and electrodes. The reaction was followed reactionware used for in situ spectroscopies showing the two conductive visually see Supplementary Video S2, which shows this process at electrodes based on carbon black. The working electrode upper line had an 60 times the normal speed and coulometrically see Fig.

The outcome of the reaction can be switched between these two products by simply altering the reactor architecture. Hence, the dimensions of the reactionware control the outcome of the reaction. No heterocycle 4 was observed in within them and the countless different architectures that could this reaction mixture All other parameters were 3D-printed reactors.

In other words, 3D-printed reactionware kept constant concentrations, solution volumes, etc. This is true in terms of both a ratio of 4-methoxyaniline to 5- 2-bromoethyl phenanthridi- what the reactionware is made from and the types of reactionware nium bromide, with the residual 2 ml of the 5- 2-bromoethyl phe- that can be made. With regard to the latter, this freedom in nanthridinium bromide solution remaining unreacted in the upper 3D-printed reactionware architecture presents the user with holding chamber from which, theoretically, it could be siphoned off both new questions and new solutions when attempting for other reactions.

Using the design Reactor B, the ratio of 4 to 5 chemical discovery. Such concepts could be very useful for tecture. Hence, using this approach, some measure two reactor architectures similar to that shown in Fig. Et3N ref. In the case of Reactor A, the volume of the two to change the way chemistry is performed, we examined the possi- upper solution-holding chambers was 4.

To this end, we thinned acetoxysilicone bathroom sealant Supplementary Information and Supplementary Fig. One holding chamber held the 4-methoxyaniline and tures. As the volume of the lower reaction chamber However, when reactionware made solely from acetoxysilicone 9.

Ahn, B. Science , — Therriault, D. Chaotic mixing in three-dimensional and illustrates the vast scope for invention and discovery that microvascular networks fabricated by direct-write assembly. Nature Mater. Ilievski, F. Soft Conclusions robotics for chemists.

In conclusion, we have demonstrated the production and utility of Hasegawa, T. Multi-directional micro- completely reusable and self-healing bespoke reactionware, which switching valve chip with rotary mechanism. A Phys. Vilbrandt, T. Fabricating nature. Technoetic Arts 7, techniques. Although the chemistry chosen to exemplify this tech- — Pearce, J. Digital technology was used to design and Yager, P. Nature , — Cook, T. Solar energy supply and storage for the legacy and nonlegacy monitor reactions in situ, and so gives an alternative to the tra- worlds.

Hence, we Gratson, G. Microperiodic structures: direct writing of optimized our initial designs to synthesize three previously unre- three-dimensional webs. Nature , Lewis, J. Direct ink writing of 3D functional materials. Moore, J. Fab Home. Malone, E. Fab Home: the personal desktop fabricator kit.

Rapid ity such as printing catalysts into certain parts of the reactionware. Prototyping J. Using such methods, we believe that it should be feasible to create Parenty, A.

Richmond, C. Moreover, the low cost associated with reactionware production Kataria, A. Building around inserts: methods for fabricating complex devices in stereolithography. Rapid Prototyping J.

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Integrated 3D-printed reactionware for chemical synthesis and analysis.

In this section Integrated 3D-printed reactionware for chemical synthesis and analysis Symes, M. Nature Chemistry , 4, pp. 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.

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Integrated 3D-printed reactionware for chemical synthesis and analysis

Nat Chem. Integrated 3D-printed reactionware for chemical synthesis and analysis. Comment in Nat Chem. 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.

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Richmond1, Geoffrey J. Cooper1, Richard W. 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. Furthermore, solely by modifying reactionware architecture, reaction outcomes can be altered.

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