Application of quantitative inline NMR spectroscopy for investigation of a fixed-bed chromatographic reactor process

Alexander Brächer; Lisa Maria Kreußer; Shamsul Qamar; Andreas Seidel-Morgenstern; Erik von Harbou

doi:10.1016/j.cej.2017.12.004

Application of quantitative inline NMR spectroscopy for investigation of a fixed-bed chromatographic reactor process

Alexander Brächer, Lisa Maria Kreußer, Shamsul Qamar, Andreas Seidel-Morgenstern, Erik von Harbou

Department of Mathematical Sciences

Research output: Contribution to journal › Article › peer-review

9 Citations (SciVal)

Abstract

A Nuclear Magnetic Resonance (NMR) spectroscopy method is presented that facilitates inline analysis of dynamic processes. Compared to other commonly used optical inline analysis methods, NMR spectroscopy has the advantage that it can resolve different species in complex multicomponent mixtures. An inline NMR spectroscopy method was optimized to enable analysis with high temporal resolution. The method was applied to study the dynamic behavior of a fixed-bed chromatographic reactor (FBCR) by monitoring the composition at the reactor outlet. The heterogeneously catalyzed hydrolysis reactions of methyl acetate and methyl formate were chosen as test systems. The influence of different process parameters such as the concentration of reactants, reactor temperature and flow rate of the mobile phase (water) were systematically studied with the presented method. The concentration profiles of the different reactants and products could be determined accurately even though the two hydrolysis reactions proceeded simultaneously in the FBCR and the concentration profiles of the different species overlapped strongly. The measured concentration profiles are in good agreement with additional RI measurements which, however, do not facilitate a component specific analysis. The accurate measurement of the concentration profiles enables to study the interaction of reaction and separation in the FBCR. At low concentrations of the reactants the measured concentration profiles agree well with predictions based on a model of the FBCR developed in previous works. At higher concentrations, however, the comparison of the predictions and experimental results reveals deficits in the model. The results demonstrate that the presented inline NMR spectroscopy method is a valuable tool to gain insights into complex dynamic processes and to gather accurate experimental data that is essential for the development of reliable process models.

Original language	English
Pages (from-to)	518-530
Number of pages	13
Journal	Chemical Engineering Journal
Volume	336
Early online date	6 Dec 2017
DOIs	https://doi.org/10.1016/j.cej.2017.12.004
Publication status	Published - 15 Mar 2018

Bibliographical note

Funding Information:
We gratefully acknowledge Flavio Sottile, Nikolas Krüger, Konstantin Sauer and Richard Behrens for their valuable help in establishing and testing the new set-up in various ways. L.M. Kreußer was supported by the UK Engineering and Physical Sciences Research Council (EPSRC) Grant No. EP/L016516/1 for the University of Cambridge Centre for Doctoral Training, the Cambridge Centre for Analysis. E. v. Harbou thanks the German Science Foundation (DFG) for the financial support within the Collaborative Research Center SFB/TRR 173 Spin+X.

Keywords

Dynamic process
Fixed-bed chromatographic reactor
Inline NMR spectroscopy
Modeling and simulation

ASJC Scopus subject areas

General Chemistry
Environmental Chemistry
General Chemical Engineering
Industrial and Manufacturing Engineering

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10.1016/j.cej.2017.12.004

Cite this

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title = "Application of quantitative inline NMR spectroscopy for investigation of a fixed-bed chromatographic reactor process",

abstract = "A Nuclear Magnetic Resonance (NMR) spectroscopy method is presented that facilitates inline analysis of dynamic processes. Compared to other commonly used optical inline analysis methods, NMR spectroscopy has the advantage that it can resolve different species in complex multicomponent mixtures. An inline NMR spectroscopy method was optimized to enable analysis with high temporal resolution. The method was applied to study the dynamic behavior of a fixed-bed chromatographic reactor (FBCR) by monitoring the composition at the reactor outlet. The heterogeneously catalyzed hydrolysis reactions of methyl acetate and methyl formate were chosen as test systems. The influence of different process parameters such as the concentration of reactants, reactor temperature and flow rate of the mobile phase (water) were systematically studied with the presented method. The concentration profiles of the different reactants and products could be determined accurately even though the two hydrolysis reactions proceeded simultaneously in the FBCR and the concentration profiles of the different species overlapped strongly. The measured concentration profiles are in good agreement with additional RI measurements which, however, do not facilitate a component specific analysis. The accurate measurement of the concentration profiles enables to study the interaction of reaction and separation in the FBCR. At low concentrations of the reactants the measured concentration profiles agree well with predictions based on a model of the FBCR developed in previous works. At higher concentrations, however, the comparison of the predictions and experimental results reveals deficits in the model. The results demonstrate that the presented inline NMR spectroscopy method is a valuable tool to gain insights into complex dynamic processes and to gather accurate experimental data that is essential for the development of reliable process models.",

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note = "Funding Information: We gratefully acknowledge Flavio Sottile, Nikolas Kr{\"u}ger, Konstantin Sauer and Richard Behrens for their valuable help in establishing and testing the new set-up in various ways. L.M. Kreu{\ss}er was supported by the UK Engineering and Physical Sciences Research Council (EPSRC) Grant No. EP/L016516/1 for the University of Cambridge Centre for Doctoral Training, the Cambridge Centre for Analysis. E. v. Harbou thanks the German Science Foundation (DFG) for the financial support within the Collaborative Research Center SFB/TRR 173 Spin+X. ",

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N1 - Funding Information: We gratefully acknowledge Flavio Sottile, Nikolas Krüger, Konstantin Sauer and Richard Behrens for their valuable help in establishing and testing the new set-up in various ways. L.M. Kreußer was supported by the UK Engineering and Physical Sciences Research Council (EPSRC) Grant No. EP/L016516/1 for the University of Cambridge Centre for Doctoral Training, the Cambridge Centre for Analysis. E. v. Harbou thanks the German Science Foundation (DFG) for the financial support within the Collaborative Research Center SFB/TRR 173 Spin+X.

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N2 - A Nuclear Magnetic Resonance (NMR) spectroscopy method is presented that facilitates inline analysis of dynamic processes. Compared to other commonly used optical inline analysis methods, NMR spectroscopy has the advantage that it can resolve different species in complex multicomponent mixtures. An inline NMR spectroscopy method was optimized to enable analysis with high temporal resolution. The method was applied to study the dynamic behavior of a fixed-bed chromatographic reactor (FBCR) by monitoring the composition at the reactor outlet. The heterogeneously catalyzed hydrolysis reactions of methyl acetate and methyl formate were chosen as test systems. The influence of different process parameters such as the concentration of reactants, reactor temperature and flow rate of the mobile phase (water) were systematically studied with the presented method. The concentration profiles of the different reactants and products could be determined accurately even though the two hydrolysis reactions proceeded simultaneously in the FBCR and the concentration profiles of the different species overlapped strongly. The measured concentration profiles are in good agreement with additional RI measurements which, however, do not facilitate a component specific analysis. The accurate measurement of the concentration profiles enables to study the interaction of reaction and separation in the FBCR. At low concentrations of the reactants the measured concentration profiles agree well with predictions based on a model of the FBCR developed in previous works. At higher concentrations, however, the comparison of the predictions and experimental results reveals deficits in the model. The results demonstrate that the presented inline NMR spectroscopy method is a valuable tool to gain insights into complex dynamic processes and to gather accurate experimental data that is essential for the development of reliable process models.

AB - A Nuclear Magnetic Resonance (NMR) spectroscopy method is presented that facilitates inline analysis of dynamic processes. Compared to other commonly used optical inline analysis methods, NMR spectroscopy has the advantage that it can resolve different species in complex multicomponent mixtures. An inline NMR spectroscopy method was optimized to enable analysis with high temporal resolution. The method was applied to study the dynamic behavior of a fixed-bed chromatographic reactor (FBCR) by monitoring the composition at the reactor outlet. The heterogeneously catalyzed hydrolysis reactions of methyl acetate and methyl formate were chosen as test systems. The influence of different process parameters such as the concentration of reactants, reactor temperature and flow rate of the mobile phase (water) were systematically studied with the presented method. The concentration profiles of the different reactants and products could be determined accurately even though the two hydrolysis reactions proceeded simultaneously in the FBCR and the concentration profiles of the different species overlapped strongly. The measured concentration profiles are in good agreement with additional RI measurements which, however, do not facilitate a component specific analysis. The accurate measurement of the concentration profiles enables to study the interaction of reaction and separation in the FBCR. At low concentrations of the reactants the measured concentration profiles agree well with predictions based on a model of the FBCR developed in previous works. At higher concentrations, however, the comparison of the predictions and experimental results reveals deficits in the model. The results demonstrate that the presented inline NMR spectroscopy method is a valuable tool to gain insights into complex dynamic processes and to gather accurate experimental data that is essential for the development of reliable process models.

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KW - Fixed-bed chromatographic reactor

KW - Inline NMR spectroscopy

KW - Modeling and simulation

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M3 - Article

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SN - 1385-8947

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JO - Chemical Engineering Journal

JF - Chemical Engineering Journal

ER -

Application of quantitative inline NMR spectroscopy for investigation of a fixed-bed chromatographic reactor process

Abstract

Bibliographical note

Keywords

ASJC Scopus subject areas

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