Real-time feedback control using online attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy for continuous flow optimization and process knowledge.
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 γ-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.
School of Chemistry, The University of Nottingham, University Park, Nottingham, NG7 2RD UK.
Ryan A
RA
Skilton
Andrew J
AJ
Parrott
Michael W
MW
George
Martyn
M
Poliakoff
Richard A
RA
Bourne
D000465:Algorithms; D002138:Calibration; D002849:Chromatography, Gas; D005246:Feedback; D005561:Formates; D008956:Models, Chemical; D000439:Pentanols / Q000737:chemistry; D015203:Reproducibility of Results; D012107:Research Design; D012984:Software; D017550:Spectroscopy, Fourier Transform Infrared / Q000379:methods*; D013696:Temperature
D005561:Formates; D000439:Pentanols; C023025:methyl carbonate; C024999:n-pentanol