Real-time feedback control using online attenuated total reflection fourier transform infrared (atr ft-ir) spectroscopy for continuous flow optimization and process knowledge

Ryan A. Skilton, Andrew J. Parrott, Michael W. George, Martyn Poliakoff, Richard A. Bourne

Research output: Journal PublicationArticlepeer-review

52 Citations (Scopus)

Abstract

The use of automated continuous flow reactors is described, with real-time online Fourier transform infrared spectroscopy (FT-IR) analysis to enable rapid optimization of reaction yield using a self-optimizing feedback algorithm. This technique has been applied to the solvent-free methylation of 1-pentanol with dimethyl carbonate using a c-alumina catalyst. Calibration of the FT-IR signal was performed using gas chromatography to enable quantification of yield over a wide variety of flow rates and temperatures. The use of FT-IR as a real-time analytical technique resulted in an order of magnitude reduction in the time and materials required compared to previous studies. This permitted a wide exploration of the parameter space to provide process understanding and validation of the optimization algorithms.

Original languageEnglish
Pages (from-to)1127-1131
Number of pages5
JournalApplied Spectroscopy
Volume67
Issue number10
DOIs
Publication statusPublished - Oct 2013
Externally publishedYes

Keywords

  • Etherification
  • FT-IR spectroscopy
  • Flow chemistry
  • Process optimization

ASJC Scopus subject areas

  • Instrumentation
  • Spectroscopy

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