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A Dissertation Entitled Bio Based Active Barrier Materials And A Dissertation entitled Bio Based Active Barrier Materials and Package Development by Michael Angelo Miranda Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Doctor of Philosophy Degree in Engineering _________________________________________ Dr. Maria. R. Coleman, Committee Chair _________________________________________ Dr. Saleh A. Jabarin, Committee Member _________________________________________ Dr. Sridhar Vimajala, Committee Member _________________________________________ Dr. Yakov Lapitsky, Committee Member _________________________________________ Dr. Young- Wah Kim, Committee Member _________________________________________ Dr. Amanda Bryant-Friedrich, Dean College of Graduate Studies The University of Toledo December 2016 Copyright 2016, Michael Angelo Miranda This document is copyrighted material. Under copyright law, no parts of this document may be reproduced without the expressed permission of the author. An Abstract of Bio Based Active Barrier Materials and Package Development by Michael Angelo Miranda Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Doctor of Philosophy Degree in Engineering The University of Toledo December 2016 The food and packaging industries are interested in approaches to reduce the permeability of oxygen in polyethylene terephthalate (PET) to extend the shelf-life of product. This has led to considerable research in barrier improvement including the use of active scavenger that permanently bind oxygen. The purpose of this work is to investigate the use of renewably sourced unsaturated fatty acids as scavengers to reduce the O2 permeability in PET. Specifically fatty acids were characterized and incorporated within PET using both blended and reactive extrusion to analyze the impact on thermal- mechanical and oxygen transport properties. Oleic, linoleic and linolenic acid are renewably resourced unsaturated fatty acids that are being investigated as active scavenger. Utilization of scavenger capacity and kinetics of oxidation are two key parameters that must be considered while selecting a scavenger. The O2 uptake capacities and the utilization of scavenger sites analysis were used to determine the most appropriate scavenger used to make a copolymer with PET. Linoleic acid was chosen due to its higher utilization capacity and relatively fast kinetics iii the cost was also taken into account. Thus linoleic acid was used in preparation of PET/Scavenger system. The effect of addition of unsaturated fatty acid on the thermal, mechanical properties and morphology of PET, were analyzed by preparing blends of PET/linoleic acid of loading of (0.25-2 weight %). The presence of the scavenger were analyzed using end group analysis where an increase in carboxyl end group was determined and NMR to obtain the peaks for the fatty acid. The appropriate method to determine molecular weight was also established. Effects of permeation through amorphous and biaxial oriented films with and without linoleic acid were investigated. The bottles were produced in two different ways (i) reactive extruded bottle and (ii) blended bottles (0.5% weight loading of Linoleic acid). The mechanical properties and density of the bottles were similar. The oxygen permeability of these bottles side wall was lower than that of PET. NMR on sample that has been exposed to oxygen was conducted to confirm the reactivity of linoleic acid with oxygen. iv To my parents, brother and family Acknowledgements My heart felt gratitude to my advisors Dr. Saleh. A Jabarin and Dr. Maria Coleman for having given me the opportunity to work in the Polymer Institute. Their constant guidance through the entire work helped me understand the polymeric systems and I appreciate their willingness to listen to my thoughts and complaints. Thanks are also due to the members of the PET and Active barrier consortium for their financial support and inputs throughout this project, also to the Department of Chemical Engineering of the University of Toledo for all the support that I received. At this point, I also would like to thank Ms. E.A Lofgren for training me on the finer aspects of various instrumentations and her constant inputs at the early stage of my work. Many thanks are due to Mr. Mike Mumford for his support, in teaching and helping me prepare various forms of PET products along with helping me understand how the different devices worked. I also extend my thanks to Dr. Lawrence, Dr. Avalos and Dr. Rodrigues for their support with instrumentation at CMSC, to Dr. Kim at the NMR center for helping me with NMR and for being on my Ph.D. committee. I am grateful to Dr. Lapitsky and Dr. Vimajal for having agreed to be members in my Ph.D. committee sparing valuable time in reviewing my Ph.D. work. Thanks to all my colleagues at the Polymer Institute and the Chemical Engineering Department for making work in the lab an enjoyable and an intellectual experience. Living in Toledo has been so memorable and enjoyable due to my friends without whom it would not have been the same. Last but not least I would like to thank my family for being my strong pillar of support throughout my Ph.D. program. v Table of Contents Abstract .............................................................................................................................. iii Acknowledgements ..............................................................................................................v Table of Contents ............................................................................................................... vi List of Tables ................................................................................................................... ix List of Figures .................................................................................................................. xiv List of Abbreviations ....................................................................................................... xxi 1. Introduction ................................................................................................................. 1 1.1 Hypothesis ............................................................................................................ 7 1.2 Research Objectives ............................................................................................. 7 2 Literature Review ...................................................................................................... 10 2.1 Permeation .......................................................................................................... 11 2.2 Passive Oxygen Barrier ...................................................................................... 14 2.2.1 Coating ........................................................................................................ 14 2.2.2 Nanocomposites .......................................................................................... 15 2.2.3 Polymer Blends: .......................................................................................... 18 2.2.4 Multilayer Films.......................................................................................... 19 2.2.5 Additives that affect free volume ................................................................ 20 2.2.6 Crystallization and branching ..................................................................... 21 2.2.7 Copolymers ................................................................................................. 21 2.3 Active Oxygen Barrier ....................................................................................... 22 2.3.1 Sachets ........................................................................................................ 24 2.3.2 Amosorb ...................................................................................................... 26 vi 2.3.3 Oxbar systems ............................................................................................. 30 2.3.4 Other oxygen scavenger systems. ............................................................... 33 2.4 Rate of scavenging in polymers ......................................................................... 35 2.4.1 Thiele modulus............................................................................................ 35 2.4.2 Selection of renewably sourced scavenger ................................................. 37 2.5 Reactive Extrusion ............................................................................................. 39 2.6 Barrier Improvement Factor (BIF) ..................................................................... 40 3. Material and Methods ................................................................................................ 43 3.1 Materials ............................................................................................................. 43 3.2 Methods .............................................................................................................. 46 3.2.1 Oxygen scavenging ..................................................................................... 46 3.2.2 Preparation of PET/LA systems.................................................................. 49 3.2.3 Preparation of Bottle ................................................................................... 52 3.2.3.1 Injection molding ........................................................................................ 52 3.2.3.2 Stretch Blow Molding
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