期刊
APPLIED SPECTROSCOPY
卷 67, 期 10, 页码 1127-1131出版社
SAGE PUBLICATIONS INC
DOI: 10.1366/13-06999
关键词
FT-IR spectroscopy; Flow chemistry; Process optimization; Etherification
资金
- Royal Society Wolfson Merit Award
- EU SYNFLOW project
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 gamma-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.
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