Das Suchergebnis hat sich seit Ihrer Suchanfrage verändert. Eventuell werden Dokumente in anderer Reihenfolge angezeigt.
  • Treffer 30 von 779
Zurück zur Trefferliste

Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy

  • ZIF-8 is a prominent member of the zeolitic imidazolate frameworks (ZIFs) subfamily of MOFs which possesses high thermal, chemical, and mechanical stabilities. Different routes have been explored to achieve the large-scale production of ZIF-8. However, these synthetic procedures are often inconsistent with the principles of sustainable chemical manufacturing. Aimed at developing scalable and greener production of ZIF-8, we adapted our previously reported in-batch „mix and wait“ synthesis[2] to continuous extrusion. To optimize the process, in-situ Raman spectroscopy was applied. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of MOF syntheses in view of their large-scale production. The synthesis of ZIF-8 was performed using a twin-screw extruder ZE 12 HMI equipped with an automatic volumetric feeder ZD 12B (Three-Tec GmbH, Switzerland) and peristaltic pump BT-L (Lead Fluid, China). The process was monitored inZIF-8 is a prominent member of the zeolitic imidazolate frameworks (ZIFs) subfamily of MOFs which possesses high thermal, chemical, and mechanical stabilities. Different routes have been explored to achieve the large-scale production of ZIF-8. However, these synthetic procedures are often inconsistent with the principles of sustainable chemical manufacturing. Aimed at developing scalable and greener production of ZIF-8, we adapted our previously reported in-batch „mix and wait“ synthesis[2] to continuous extrusion. To optimize the process, in-situ Raman spectroscopy was applied. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of MOF syntheses in view of their large-scale production. The synthesis of ZIF-8 was performed using a twin-screw extruder ZE 12 HMI equipped with an automatic volumetric feeder ZD 12B (Three-Tec GmbH, Switzerland) and peristaltic pump BT-L (Lead Fluid, China). The process was monitored in six different zones using a Raman RXN1TM analyzer (Kaiser Optical Systems, France) with a non-contact probe head. PMMA screw-in parts, which are transparent to Raman laser radiation, were specially manufactured to provide the laser focus within the barrel. PXRD, TGA, N2 adsorption measurements, and SEM were used as complementary techniques to characterize the extrudates. The batch ‘mix and wait’ synthesis of ZIF-8, consisting of bringing solid basic zinc carbonate and 2-methylimidazole in contact in a closed vial, was successfully adapted to reactive extrusion. The crystalline ZIF-8 continuously forms in the extruder under the mixing of solid reagents in the presence of a catalytic amounts of H2O or EtOH. The temperature, type of liquid, feeding rate, and excess of linker were optimized using in situ Raman spectroscopy. Pure and highly crystalline ZIF-8 was isolated at 40 °C by adding a catalytic amount of EtOH and a linker excess of 25%. The resulting material has excellent porosity with the BET surface area slightly exceeding that of the reference Basolite® Z1200 (1816 vs. 1734 m2 g–1). The reaction could yield ~ 3 kg d–1 assuming a continuous operation, with a space-time yield of ca. 67,000 kg m–3 d–1. The present method was compared to the published pathways based on Green Chemistry principles and proved to have the highest potential for large-scale production of ZIF-8.zeige mehrzeige weniger

Volltext Dateien herunterladen

  • EuroMOF.pdf
    eng

Metadaten exportieren

Weitere Dienste

Teilen auf Twitter Suche bei Google Scholar Anzahl der Zugriffe auf dieses Dokument
Metadaten
Autor*innen:Nikita Gugin
Koautor*innen:José Antonio Villajos Collado, Olivier Dautain, Michael Maiwald, Franziska Emmerling
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2023
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
6 Materialchemie
6 Materialchemie / 6.3 Strukturanalytik
DDC-Klassifikation:Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten
Freie Schlagwörter:Green chemistry; In situ Raman; Large-scale synthesis; MOFs; Mechanochemistry; Reactive extrusion
Themenfelder/Aktivitätsfelder der BAM:Material
Material / Materialdesign
Veranstaltung:5th European Conference on Metal Organic Frameworks and Porous Polymers (EuroMOF2023)
Veranstaltungsort:Granada, Spain
Beginndatum der Veranstaltung:24.09.2023
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:30.11.2023
Referierte Publikation:Nein
Einverstanden
Diese Webseite verwendet technisch erforderliche Session-Cookies. Durch die weitere Nutzung der Webseite stimmen Sie diesem zu. Unsere Datenschutzerklärung finden Sie hier.