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Chapter 5, Environmentally-Friendly Fatty Acids with Different Chemical Characteristics Have Be Evaluated As Phase Change Materials

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Chapter 5, Environmentally-Friendly Fatty Acids with Different Chemical Characteristics Have Be Evaluated As Phase Change Materials Universidad de Castilla-La Mancha Facultad de Ciencias y Tecnologías Químicas Departamento de Ingeniería Química DEVELOPMENT OF MICROCAPSULES WITH THERMAL ENERGY STORAGE (TES) CAPABILITY FOR CONCRETE APPLICATIONS A thesis submitted for the degree of Doctor of Philosophy (PhD) by ANNA MARIA SZCZOTOK-PIECHACZEK Supervisors: Prof. Juan Francisco Rodríguez Romero Prof. Anna-Lena Kjøniksen Ciudad Real, April 2018 Prof. Juan Francisco Rodríguez Romero, Professor of Chemical Engineering at the University of Castilla-La Mancha and Prof. Anna-Lena Kjøniksen, Professor of Materials Science at Østfold University College, certify that: The research work: "Development of Microcapsules with Thermal Energy Storage (TES) Capability for Concrete Applications", is part of thesis presented by Mrs. Anna Maria Szczotok-Piechaczek to aspire to the degree of Doctor in Chemical Engineering and that has been carried out in the laboratories of the Department of Chemical Engineering of the University of Castilla-La Mancha and Østfold University College under their direction. And for the record, they sign this certificate in Ciudad Real, at April 16th 2018 Juan Fco. Rodríguez Romero Anna-Lena Kjøniksen Table of content Summary .......................................................................................................................... vi 1. Introduction .............................................................................................................. 1 1.1. Motivation and background ............................................................................... 2 1.2. Objective ............................................................................................................ 3 1.3. Thesis structure .................................................................................................. 5 2. State of art ................................................................................................................. 6 2.1. Global energy demand ....................................................................................... 7 2.2. Methods for thermal energy storage .................................................................. 9 2.3. Phase change materials .................................................................................... 10 Organic PCMs .......................................................................................... 11 Inorganic PCMs ........................................................................................ 11 Eutectics PCMs ........................................................................................ 12 2.4. Microencapsulation of phase change materials ............................................... 12 General overview of microencapsulation ................................................. 12 Microencapsulation by suspension polymerization .................................. 16 2.5. Selection criteria of PCMs for passive buildings ............................................. 23 2.6. Phase change materials in building applications ............................................. 24 Free cooling .............................................................................................. 24 Peak load shifting ..................................................................................... 25 Active building systems ........................................................................... 26 Passive buildings system .......................................................................... 27 2.7. Integration of phase change materials in passive systems ............................... 28 Walls ......................................................................................................... 28 Roofs ......................................................................................................... 31 Floors ........................................................................................................ 32 Windows and shutters ............................................................................... 34 Table of content 2.8. Limitations in the PCMs application ............................................................... 36 Thermal conductivity ................................................................................ 36 Supercooling ............................................................................................. 36 Leakage of PCM ....................................................................................... 37 Flammability ............................................................................................. 37 References ...................................................................................................................... 40 3. Materials and methods ............................................................................................ 54 3.1. Materials .......................................................................................................... 55 3.2. Experimental setups ......................................................................................... 57 Synthesis of the microcapsules ................................................................. 57 Bulk polymerization ................................................................................. 62 Thermal properties .................................................................................... 62 3.3. Experimental procedures ................................................................................. 63 Polymerization of the microcapsules ........................................................ 63 Polymerization in mass ............................................................................. 64 Synthesis of PNC-HEMA ......................................................................... 64 Concrete preparation................................................................................. 65 3.4. Characterization techniques and characteristic parameters ............................. 65 Differential scanning calorimetry ............................................................. 65 Thermogravimetric analysis ..................................................................... 66 Ash determination .................................................................................... 67 Density of microcapsules.......................................................................... 67 Porosity ..................................................................................................... 68 Environmental scanning electron microscopy and energy dispersive x-ray spectrometry ........................................................................................................... 68 Low angle laser light scattering ................................................................ 69 Table of content Sieving ...................................................................................................... 70 Surface tension and contact angle ............................................................ 70 Gel permeation chromatography .......................................................... 72 Gas chromatography – mass spectrum analysis ................................... 72 Fourier transform Infrared spectroscopy .............................................. 73 X-ray micro-tomography ...................................................................... 74 Micro-combustion calorimetry ............................................................. 74 Cone calorimetry ................................................................................... 75 Compressive strength test ..................................................................... 76 Thermal conductivity ............................................................................ 77 Specific heat capacity/latent heat .......................................................... 77 Energy saving aspects ........................................................................... 78 Process parameters ................................................................................ 79 References ...................................................................................................................... 80 4. Optimization of microcapsules recipe and properties ............................................ 81 4.1. Background ...................................................................................................... 85 4.2. Results on optimization ................................................................................... 87 Preliminary experiments ........................................................................... 87 Theoretical framework ............................................................................. 90 Effect of different suspending agents on microcapsules properties ......... 91 Effect of continuous/discontinuous phase mass ratio on microcapsules properties ................................................................................................................ 99 Effect of stirring rate on microcapsules properties ................................. 101 Effect of toluene/PCM mass ratio and the PCM content on microcapsules properties .............................................................................................................. 102 Influence of PVP concentration on microcapsules properties ................ 103 Table of content Influence of PNC-HEMA incorporation on morphology and encapsulation efficiency .............................................................................................................
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