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Field integration of benchtop NMR instruments for online monitoring and process control of a modular industrial reaction step

  • Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectroscopy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. Within the project CONSENS, the continuous production of high-value products in small production scale is advanced by introducing benchtop NMR spectroscopy. CONSENS is a research and innovation project on integratedOnline monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectroscopy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. Within the project CONSENS, the continuous production of high-value products in small production scale is advanced by introducing benchtop NMR spectroscopy. CONSENS is a research and innovation project on integrated control and sensing for sustainable operation of flexible intensified processes. This poster will present the first steps of the process integration of a benchtop NMR instrument for a lithiation process and outlines further fields of activity and potential challenges. Hereby, the following issues are going to be addressed: explosion-proof housing for the spectrometer, automation of signal processing (data pretreatment, evaluation and communication to the control system), flow cells and measuring conditions. Furthermore, first online spectra of the lithiation reaction in batch mode were acquired in lab scale. The reaction was performed in a 25 mL glass reactor with thermal jackets for temperature control of the reaction mixture. The Li-HMDS was dosed stepwise by using a glass syringe. First spectra in the proton and fluorine domain were recorded online using a flowrate of 3.5 mL min–1 and a simple 5 mm polytetrafluoroethylene tube (PTFE) as a flow cell.zeige mehrzeige weniger

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Metadaten
Autoren/innen:Klas Meyer
Koautoren/innen:Patrick Gräßer, Nicolai Zientek, Michael Maiwald, Andrea Paul, Simon Kern
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2016
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
Veröffentlichende Institution:Bundesanstalt für Materialforschung und -prüfung (BAM)
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Online NMR spectroscopy; Reaction monitoring
Themenfelder/Aktivitätsfelder der BAM:Analytical Sciences
Analytical Sciences / Zerstörungsfreie Prüfung und Spektroskopie
Veranstaltung:4th Practical Applications of NMR in Industry Conference (PANIC)
Veranstaltungsort:Houston, Texas, USA
Beginndatum der Veranstaltung:15.02.2016
Enddatum der Veranstaltung:18.02.2016
URN:urn:nbn:de:kobv:b43-354427
Verfügbarkeit des Volltexts:Volltext-PDF für die Öffentlichkeit verfügbar ("Open Access")
Lizenz (Deutsch):License LogoCreative Commons - CC BY-NC-ND - Namensnennung - Nicht kommerziell - Keine Bearbeitungen 4.0 International
Datum der Freischaltung:16.03.2016
Referierte Publikation:Nein
Schriftenreihen ohne Nummerierung:BAM Präsentationen