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

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

Research output: Journal PublicationArticlepeer-review

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. (Figure presented.).

Original languageEnglish
Pages (from-to)38-50
Number of pages13
JournalApplied Spectroscopy
Volume76
Issue number1
DOIs
Publication statusPublished - Jan 2022

Keywords

  • FT-IR
  • Flow chemistry
  • Fourier transform infrared Spectroscopy
  • electrosynthesis
  • gas separation
  • self-optimization

ASJC Scopus subject areas

  • Instrumentation
  • Spectroscopy

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