3D printing of versatile reactionware for chemical synthesis

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.

Frontal Conversion and Uniformity in 3D Printing by Photopolymerisation

“…Current 3D applications include automotive, aerospace, medical and dental, as well as design, jewellery and increasingly domestic use. Numerous high-tech and specialist industries are actively piloting and already employing 3D printing technologies [2,3] in emerging applications in medical and analytical sciences [4], including tissue engineering [5,6,7], drug delivery [8], and reaction ware [9,10], but also device fabrication and microfluidics [11,12], materials for energy [13,14], low-density, high-strength materials [15,16], electronics [17,18,19]. …”

Digital Control of Multistep Hydrothermal Synthesis by Using 3D Printed Reactionware for the Synthesis of Metal–Organic Frameworks

“…[9] Despite these advances,c onventional hydrothermal syntheses are still usually carried out under one-pot, single step conditions,w hich precludes the exploration of multi-step reactions or more complex reaction conditions.T his limits the ability to introduce synthetic complexity,whereby the composition of the reaction mixture can be changed under the reaction conditions without interruption. [11][12][13][14][15] This is because we wanted to see if the production of bespoke hydrothermal reactors,with partitioned chambers,w as possible.T raditional "one-pot" hydrothermal techniques are limited to using asingle reaction composition (c)w hich encompasses the sum of starting materials introduced at the start of the experiment, and this evolves through the course of the reaction. [10] We hypothesized that sequential hydrothermal syntheses could be achieved by creating reactors with internal geometries that allow the compartmentalization of different reaction mixtures,p reventing their mixing until defined points in the synthesis.T his approach leads to the possibility of "trapping" otherwise inaccessible reaction intermediates or unstable building blocks.W ith this in mind, we opted to build upon our recent work that used 3D printing to give architectural control of the reactor with the design and fabrication of reactionware.…”

Advanced reactor engineering with 3D printing for the continuous-flow synthesis of silver nanoparticles

“…Cronin and co-workers reported for the first time the application of 3D printing to chemical synthesis, coining the term "reactionware", 22,23 including the development of fluidic devices for continuous-flow synthesis. [24][25][26] This work has led to a new area of research, mostly in the development of 3D printed microfluidic devices for analytical applications.…”