3D Printed Reactors and Kessil Lamp Holders for Flow Photochemistry: Design and System Standardization

Abstract

A low-cost 3D printed standardized flow-photochemistry setup has been designed and developed for use with a pressure-driven flow system using photochemistry lamps available in most laboratories. In this research, photochemical reactors were 3D printed from polypropylene which facilitated rapid optimization of both reactor geometry and experimental setup of the lamp housing system. To exemplify the rapidity of this approach to optimization, a Kessil LED lamp was used in the bromination of a range of toluenes in the 3D printed reactors in good yields with residence times as low as 27 seconds. The reaction compared favorably with the batch photochemical procedure and was able to be scaled up to a productivity of 75 mmol h-1.

Digitisation of a modular plug and play 3D printed continuous flow system for chemical synthesis

“…The scale up synthesis of 1,2-bis(4-methoxyphenyl)-1,2-diphenylethane-1,2-diol ( 5 ) (Table 2, Scheme 2) 29 and methyl 3-bromo-3-phenylpropanoate ( 8 ) (Table 3, Scheme 3) 24 were successfully obtained using the phototemperature module. Both reactions were performed with one CDR placed 30 mm below a blue light lamp while being air cooled.…”

“…The phototemperature module was designed to hold a Kessil lamp to perform photochemical reactions, record temperature measurements, whilst cooling the system with compressed air and the last module was designed to measure the flow rate of the system using an SLF3C-1300F liquid flow sensor. 23,24 Conventional liquid sensors such as these are frequently calibrated with water only and as such, the sensor was calibrated with a range of other solvents to accurately monitor their specific flow rate (ESI†). The calibrated solvents were selected based on which ones were most probable to be used in reactions and were compatible with the sensor, including isopropanol (IPA), methanol, ethanol, acetone, and acetonitrile.…”