Heat on – Calibration of IR Spectroscopy at Process Conditions for Continuous Esterification

• Published in: Chemie ingenieur technik Vol. 92; no. 10; pp. 1467 - 1473
• Main Authors: Schnoor, Johann‐Kilian, Schulte, Lennard D., Liauw, Marcel A.
• Format: Journal Article
• Language: English
• Published: 01.10.2020
• Subjects: Acetic acid esters; Carbon2Chem; Continuous flow; In situ spectroscopy; Inline calibration
• ISSN: 0009-286X; 1522-2640
• DOI: 10.1002/cite.202000050

This work tries to close the gap between continuous synthesis, measurement, calibration, and analysis on R&D scale. By introducing new calibration methods, the full potential of inline ATR‐FTIR spectroscopy in continuous reactor setups is unraveled. A fast, fully automated calibration of the reaction mixtures is carried out at process conditions. The use of different compositions underlines the robustness of this calibration method, which was used for the determination of kinetic parameters. The conversion‐based calibration significantly increased the precision of the analysis. In difference, the new method only requires the preparation of two calibration mixtures. By that, this method can also be applied to large‐scale processes and allows the use of a single measurement setup from R&D to industrial scale. Spectroscopic measurement techniques have found their way into R&D process development. A new calibration method was developed to allow precise measurements using ATR‐FTIR spectroscopy in continuous reactors in R&D and industrial scale. The calibration under process conditions increased precision and avoided temperature‐ and pressure‐related shifts.