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Self-Optimization of Continuous Flow Electrochemical Synthesis Using Fourier Transform Infrared Spectroscopy and Gas Chromatography

Ke, Jie; Gao, Chuang; Folgueiras-Amador, Ana A.; Jolley, Katherine E.; de Frutos, Oscar; Mateos, Carlos; Rincón, Juan A.; Brown, Richard C.D.; Poliakoff, Martyn; George, Michael W.

Self-Optimization of Continuous Flow Electrochemical Synthesis Using Fourier Transform Infrared Spectroscopy and Gas Chromatography Thumbnail


Authors

JIE KE JIE.KE@NOTTINGHAM.AC.UK
Research Fellow

Chuang Gao

Ana A. Folgueiras-Amador

Oscar de Frutos

Carlos Mateos

Juan A. Rincón

Richard C.D. Brown



Abstract

A continuous-flow electrochemical synthesis platform has been developed to enable self-optimization of reaction conditions of organic electrochemical reactions using attenuated total reflection Fourier transform infrared spectroscopy (ATR FT-IR) and gas chromatography (GC) as online real-time monitoring techniques. We have overcome the challenges in using ATR FT-IR as the downstream analytical methods imposed when a large amount of hydrogen gas is produced from the counter electrode by designing two types of gas–liquid separators (GLS) for analysis of the product mixture flowing from the electrochemical reactor. In particular, we report an integrated GLS with an ATR FT-IR probe at the reactor outlet to give a facile and low-cost solution to determining the concentrations of products in gas–liquid two-phase flow. This approach provides a reliable method for quantifying low-volatile analytes, which can be problematic to be monitored by GC. Two electrochemical reactions the methoxylation of 1-formylpyrrolidine and the oxidation of 3-bromobenzyl alcohol were investigated to demonstrate that the optimal conditions can be located within the pre-defined multi-dimensional reaction parameter spaces without intervention of the operator by using the stable noisy optimization by branch and FIT (SNOBFIT) algorithm.

Journal Article Type Article
Acceptance Date Aug 23, 2021
Online Publication Date Dec 15, 2021
Publication Date Jan 1, 2022
Deposit Date Jan 26, 2022
Publicly Available Date Feb 2, 2022
Journal Applied Spectroscopy
Print ISSN 0003-7028
Electronic ISSN 1943-3530
Publisher SAGE Publications
Peer Reviewed Peer Reviewed
Volume 76
Issue 1
Pages 38-50
DOI https://doi.org/10.1177/00037028211059848
Keywords Flow chemistry; self-optimization; electrosynthesis; Fourier transform infrared Spectroscopy; FT-IR; gas separation
Public URL https://nottingham-repository.worktribe.com/output/7340454
Publisher URL https://journals.sagepub.com/doi/10.1177/00037028211059848
Additional Information Ke J, Gao C, Folgueiras-Amador AA, et al. Self-Optimization of Continuous Flow Electrochemical Synthesis Using Fourier Transform Infrared Spectroscopy and Gas Chromatography. Applied Spectroscopy. 2022;76(1):38-50. doi:10.1177/00037028211059848

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