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Pyrene Based Metal Organic Frameworks

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Pyrene Based Metal Organic Frameworks Pyrene based Metal Organic Frameworks. Thesis submitted in accordance with the requirements of the University of Liverpool for the degree of Doctor in Philosophy by Thomas Ian Mangnall. November 2015. 1 Contents Abstract .......................................................................................................... 7 Extended Abstract ........................................................................................ 7 Acknowledgements. ..................................................................................... 11 Abbreviations. .............................................................................................. 13 1. Introduction .............................................................................................. 15 1.1. General Introduction ........................................................................... 15 1.2. Porous Materials ................................................................................. 15 1.2.1. Inorganic Porous Materials .......................................................... 16 1.2.2. Organic Porous Materials ............................................................. 20 1.2.3. Hybrid Porous Materials/Metal Organic Frameworks (MOFs) ... 21 1.2. History of Metal Organic Frameworks and Common Examples ........ 26 1.3. Applications of Metal Organic Frameworks ....................................... 31 1.3.1. Separation ..................................................................................... 31 1.3.2. Gas Storage .................................................................................. 34 1.3.3. Drug Delivery............................................................................... 40 1.3.4. Sensing ......................................................................................... 42 1.3.5. Catalysis ....................................................................................... 46 1.4. Photocatalysis ...................................................................................... 48 1.4.1. Semi-conductor Photocatalysis. ................................................... 48 1.4.2. Molecular photocatalysts. ............................................................ 54 2 1.4.3. Pyrene photocatalysis. .................................................................. 55 1.5. Conclusions ......................................................................................... 59 2. Synthetic and Experimental Techniques. ................................................. 64 2.1. Introduction. ........................................................................................ 64 2.2. Synthesis Techniques .......................................................................... 65 2.2.1. Solvothermal Synthesis of MOFs. ............................................... 65 2.3. X-Ray Diffraction. .............................................................................. 70 2.3.1. Principles of X-Ray Diffraction. .................................................. 70 2.3.2. Single Crystal X-Ray Diffraction. ............................................... 74 2.3.3. Powder X-Ray Diffraction. .......................................................... 75 2.4. Thermogravimetric Analysis. .............................................................. 76 2.5. CHN Combustion Elemental Analysis ............................................... 76 2.6. Inductively Coupled Plasma Optical Emission Spectroscopy. ........... 77 2.7. Gas Sorption. ....................................................................................... 77 2.8. Electron Microscopy. .......................................................................... 82 2.9. Optical Spectroscopy. ......................................................................... 83 2.9.1. Ultra Violet/Visible Spectroscopy. .............................................. 83 2.9.2. Fluorescence Spectroscopy. ......................................................... 84 2.10. Gas Chromatography and Thermal Conductivity Detector. ............. 86 2.11. Nuclear Magnetic Resonance Spectroscopy. .................................... 88 3. AlTBAPy ................................................................................................. 93 3 3.1. Overview. ............................................................................................ 93 3.2. Experimental ....................................................................................... 96 3.2.1. Synthesis ...................................................................................... 96 3.2.2. Photocatalysis. ............................................................................ 105 3.3. Characterisation................................................................................. 107 3.3.1. PXRD ......................................................................................... 107 3.3.2. SEM ........................................................................................... 109 3.3.3. TGA ........................................................................................... 111 3.3.4. Elemental analysis. ..................................................................... 112 3.3.5. Surface Area Measurements. ..................................................... 113 3.3.6. Optical Spectroscopy. ................................................................ 115 3.4. Water stability ................................................................................... 118 3.5. Photocatalysis. ................................................................................... 120 3.5.1. TEM ........................................................................................... 123 3.6. Pt@AlTBAPy MOF .......................................................................... 127 3.6.1. Characterisation.......................................................................... 128 3.6.2. Photocatalytic hydrogen evolution. ............................................ 138 3.7. Heat of adsorption of gasses. ............................................................ 139 3.7.1. Carbon dioxide ........................................................................... 140 3.7.2. Methane. ..................................................................................... 144 Conclusion. .............................................................................................. 148 4 4. ZrTBAPy ................................................................................................ 152 4.1. Overview. .......................................................................................... 152 4.2. Experimental ..................................................................................... 156 4.2.1. NU-1000 Synthesis. ................................................................... 156 4.2.2. Photocatalysis. ............................................................................ 157 4.3. Characterisation................................................................................. 159 4.3.1. PXRD ......................................................................................... 159 4.3.2. SEM ........................................................................................... 161 4.3.3. TGA ........................................................................................... 163 4.3.4. Elemental analysis. ..................................................................... 164 4.3.5. Surface Area Measurements. ..................................................... 165 4.3.6. Optical Spectroscopy. ................................................................ 167 4.4. Water stability ................................................................................... 170 4.5. Photocatalysis. ................................................................................... 172 4.5.1. TEM ............................................................................................ 175 4.6. Pt@NU-1000 MOF ........................................................................... 177 4.6.1. Characterisation.......................................................................... 178 4.6.2. Photocatalytic hydrogen evolution. ........................................... 190 4.7. Conclusion. ....................................................................................... 192 5. EuTBAPy ............................................................................................... 194 5.1. Overview. .......................................................................................... 194 5 5.2. MOF Synthesis. ................................................................................. 195 5.2.1. High Throughput Synthesis........................................................ 195 5.2.2. Single Crystal Synthesis. ............................................................ 200 5.2.3. Phase Pure Powder Synthesis..................................................... 202 5.3. Characterisation................................................................................. 203 5.3.1.SCXRD ....................................................................................... 203 5.3.2. PXRD ......................................................................................... 205 5.3.3. SEM ........................................................................................... 207 5.3.4. TGA ........................................................................................... 209 5.3.5.
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