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Improving the Sustainability of the Synthesis of Mofs Used for the Production of Catalysts for Dry Reforming of Methane

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Improving the Sustainability of the Synthesis of Mofs Used for the Production of Catalysts for Dry Reforming of Methane POLITECNICO DI TORINO Collegio di Ingegneria Chimica e dei Materiali Corso di Laurea Magistrale in Ingegneria Chimica e dei Processi Sostenibili Tesi di Laurea Magistrale Improving the sustainability of the synthesis of MOFs used for the production of catalysts for dry reforming of methane Relatori prof. Stefania Specchia firma del relatore Candidato Arianna Miglio firma del candidato Ottobre 2019 “Ai miei zii Mimmo e Giuseppina esempio di vita, amore e famiglia.” The project has been carried out at ‘Laboratoire de Réactivité de Surface’ during an Erasmus project at Sorbonne Univerité of Paris. Table of contents 1.Riassunto in italiano............................................................................................................I 1.1 Introduzione.................................................................................................................I 1.1.1 Metal-organic frameworks (MOFs): definizione, proprietà e struttura................II 1.1.2 Metodi di sintesi dei metal-organic frameworks................................................III 1.1.3 Applicazione dei MOFs in catalisi.....................................................................IV 1.1.4 MIL-53(Al) ........................................................................................................V 1.1.5 Dry reforming del metano .................................................................................VI 1.2 Materiali e metodi...................................................................................................VIII 1.2.1 Sintesi in un solo step del MIL-53(Al)............................................................VIII 1.2.2 Sintesi in due step del MIL-53(Al)..................................................................VIII 1.2.3 Preparazione del catalizzatore...........................................................................IX 1.2.4 Diffrazione raggi X.............................................................................................X 1.2.5 Analisi termogravimetrica..................................................................................X 1.2.6 Fisisorbimento dell’azoto...................................................................................X 1.2.7 Microscopia elettronica a trasmissione e a scansione..........................................X 1.2.8 Risonanza magnetica nucleare............................................................................X 1.2.9 Riduzione a temperatura programmata..............................................................XI 1.2.10 Misurazioni catalitiche....................................................................................XI 1.3 Risultati e discussione...............................................................................................XI 1.3.1 Sintesi in un solo step del MIL-53(Al) e preparazione del catalizzatore...........XII 1.3.2 Sintesi in due step del MIL-53(Al) e preparazione del catalizzatore..............XVII 1.4 Conclusioni..............................................................................................................XX 2. Introduction.......................................................................................................................1 2.1 Metal-organic frameworks (MOFs): definition, properties and structures ..................2 2.1.1 Metal Ions and organic ligands as Building Units of MOFs.................................3 2.1.2 Open Metal Sites in MOFs...................................................................................4 2.2 Methods of synthesis of metal-organic frameworks.....................................................5 2.3 Applications of MOFs in catalysis...............................................................................6 2.4 MIL-53 (Al).................................................................................................................7 2.5 Dry reforming of methane............................................................................................9 2.5.1 Thermodynamics..............................................................................................10 2.5.2 Coke formation ................................................................................................11 2.5.3 Catalysts and catalytic property........................................................................12 2.6 Poly (ethylene terephthalate) .....................................................................................13 3. Methods and material........................................................................................................14 3.1 MIL-53(Al) synthesis.................................................................................................14 3.1.1 One step synthesis of MIL-53(Al) ....................................................................15 3.1.2 Two steps synthesis of MIL-53(Al) ..................................................................15 3.2 Catalyst preparation....................................................................................................16 3.3 Physicochemical characterization techniques.............................................................17 3.3.1 X-ray diffraction...............................................................................................17 3.3.2 Thermo Gravimetric Analysis..........................................................................18 3.3.3 N2 physisorption...............................................................................................19 3.3.4 Transmission electron microscopy (TEM) .......................................................21 3.3.5 Nuclear magnetic resonance (NMR) ................................................................22 3.3.6 Temperature-programmed reduction (TPR) ....................................................23 3.3.7 Scanning electron microscopy (SEM) ..............................................................25 3.4 Catalytic measurements..............................................................................................25 3.4.1 Description of the equipment............................................................................25 3.4.2 Catalytic test conditions...................................................................................27 4. Results and discussion.....................................................................................................28 4.1 One step synthesis.....................................................................................................28 4.1.1 As-synthesized MIL-53(Al) .............................................................................28 4.1.2 Activated MIL-53(Al) ......................................................................................30 4.1.3 Impregnated MIL-53(Al) .................................................................................33 4.1.4 Calcined MIL-53(Al) .......................................................................................35 4.1.5 Reduced MIL-53(Al) .......................................................................................38 4.2 Two steps synthesis..................................................................................................41 4.2.1 Alcoholysis of PET...........................................................................................41 4.2.2 Synthesis and activation of MIL-53(Al) ...........................................................41 4.2.3 Nickel impregnation of MIL-53(Al) ................................................................43 4.2.4 Calcination of MIL-53(Al) ...............................................................................46 5. Conclusion.......................................................................................................................48 6. Abbreviations..................................................................................................................50 7. References.......................................................................................................................52 8.Acknowledgements..........................................................................................................55 1.Riassunto in italiano 1.1 Introduzione Il lavoro è parte di un progetto più ampio che coinvolge una ricerca sulla sintesi di nuove strutture porose che possano fungere da supporti nella reazione di dry reforming del metano. Negli ultimi venti anni, c'è stato un aumento del consumo di energia, principalmente a causa di una rapida crescita della popolazione umana.1 Per soddisfare la crescente domanda di energia, vengono utilizzati combustibili fossili come petrolio, gas naturale e carbone. La dipendenza dai combustibili fossili per soddisfare la domanda di energia ha creato problemi ambientali attraverso la produzione di gas a effetto serra (GHG). Il metano e il biossido di carbonio costituiscono una parte importante dei gas a effetto serra, e hanno contribuito in modo determinante al cambiamento climatico, che incide sulla produttività, sugli ecosistemi naturali, sull'agricoltura e sulla società.2 Sebbene la concentrazione di metano nell'atmosfera sia inferiore a quella di CO2, ha causato sorprendentemente circa il 20% del riscaldamento globale.3-4 Tradizionalmente il metano è prodotto da due fonti; in primo luogo proviene da fonti naturali come termiti, praterie, incendi, laghi e zone umide, e in secondo luogo da attività umane come l'estrazione del carbone, le discariche, la lavorazione di petrolio e gas e le attività
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