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(Title of the Thesis)* In-Situ Continuous Monitoring of Catastrophic Phase Inversion and Viscosity of Pickering Emulsions by Upinder Bains A thesis presented to the University of Waterloo in fulfillment of the thesis requirement for the degree of Master of Applied Science in Chemical Engineering Waterloo, Ontario, Canada, 2018 ©Upinder Bains 2018 AUTHOR'S DECLARATION I hereby declare that I am the sole author of this thesis. This is a true copy of the thesis, including any required final revisions, as accepted by my examiners. I understand that my thesis may be made electronically available to the public. ii Abstract Emulsions are used in the various field such as petroleum, pharmaceuticals, foods, cosmetics, paints, etc. Emulsions stabilized with solid nanoparticles are called Pickering emulsions. More recently, a growing awareness of using environment friendly products has led to more and more researchers to develop and modify natural materials. Starch nanoparticle might be a suitable candidate because they are environmentally friendly, safe and non-toxic. Also, from a practical point of view, starch nanoparticles are low cost, and rheological properties of their emulsions can easily be altered with the help of additives. Because of the unstable nature of these emulsions, continuous agitation is needed to keep the emulsion from separating. This makes the viscosity measurements a challenge, however this task was made possible at low shear rates under some controlled parameters. In this study, an in-situ viscosity measurement method is used to investigate the viscous behaviour of O/W and W/O emulsions at a different volume fraction of the dispersed phase. For this purpose, rotational viscometer installed in a tank was used along with a high shear mixer. In this work, two sets of emulsions were formulated with starch nanoparticles to study their rheological behaviour. Also, Surfactant-stabilized O/W type emulsions were formulated with commercially known Triton X-100 non-ionic surfactant and compared with solid nanoparticles emulsions for rheology and stability. The emulsions viscosities and shear rate were measured at different concentrations of the dispersed phase and spindle rotation speeds. Experimental results showed that, at low concentration of dispersed phase, emulsions exhibited Newtonian behaviour and at high concentrations of the dispersed phase, emulsions displayed non-Newtonian shear-thinning behaviour in that viscosity was dependent on the shear rate. This nature of the emulsions was confirmed as the viscosity measurements changed with spindle rotation speeds. Starch nanoparticles increased the viscosity of the emulsions and played a critical role in stabilizing emulsions by adsorbing at the oil-water interface. For water- in-oil emulsions, Pickering emulsions displayed phase inversion which was related to particle concentration. iii Acknowledgements I would like to express my sincerest gratitude to my supervisor, Dr. Rajinder Pal for his constant guidance, patience, support and encouragement throughout the course of this research. I deeply appreciate the opportunity to study and work under his supervision. I would also like to express my gratitude to my labmates Sileola Ogunlaja, Arshdeep Singh and Sima Lashkari for their help and useful discussion. My gratitude is also given to graduated student Yifan Wu who helped during the initial stage of the project. I would like to thank all friends and colleagues who have helped and supported me. Finally, a very special thanks to my parents and brother for their encouragement, support and understanding. iv Table of Contents AUTHOR'S DECLARATION ............................................................................................................... ii Abstract ................................................................................................................................................. iii Acknowledgements ............................................................................................................................... iv Table of Contents ................................................................................................................................... v List of Figures ...................................................................................................................................... vii List of Tables .......................................................................................................................................... x Introduction ............................................................................................................................ 1 1.1 Fundamentals of Emulsions ......................................................................................................... 1 1.2 Emulsion Stabilizers ..................................................................................................................... 1 1.2.1 Surfactants ............................................................................................................................. 1 1.2.2 Solid Nanoparticles ............................................................................................................... 2 1.3 Phase Inversion ............................................................................................................................. 4 1.4 Emulsion Stability ........................................................................................................................ 5 1.5 Importance of the Research .......................................................................................................... 7 1.6 Thesis Objectives ......................................................................................................................... 8 Review of In-line Techniques for Viscosity Measurement ................................................. 10 2.1 Rotational Viscometers .............................................................................................................. 10 2.2 Tube Viscometry ........................................................................................................................ 15 2.3 Vibrational Viscometers ............................................................................................................. 18 2.4 Mixer-type Viscometers ............................................................................................................. 21 Experimental Work .............................................................................................................. 25 3.1 Materials ..................................................................................................................................... 25 3.2 Set-up.......................................................................................................................................... 26 3.2.1 Viscosity Measurements ...................................................................................................... 26 3.2.2 Microscopy .......................................................................................................................... 30 3.3 Preparation of Starch Nanoparticle Dispersions ......................................................................... 30 3.4 Preparations of Emulsions .......................................................................................................... 31 3.5 Accuracy and Reproducibility .................................................................................................... 31 Results and Discussion ........................................................................................................ 33 4.1 Oil-in-Water Emulsions.............................................................................................................. 33 4.1.1 Surfactant-Stabilized Emulsion ........................................................................................... 34 v 4.1.2 Solid Nanoparticles-Stabilized Emulsions .......................................................................... 36 4.1.3 Emulsion Stability ............................................................................................................... 40 4.1.4 Microscopy ......................................................................................................................... 42 4.2 Water-in-Oil Emulsions ............................................................................................................. 45 4.2.1 Emulsion Preparation .......................................................................................................... 45 4.2.2 0.25% nanoparticles dispersion (concentration by wt.) ...................................................... 46 4.2.3 0.5% nanoparticle dispersion (concentration by wt.) .......................................................... 47 4.2.4 1% nanoparticle dispersion (concentration by wt.) ............................................................. 49 4.2.5 2% nanoparticle dispersion (concentration by wt.) ............................................................. 50 4.3 Detection of Phase Inversion Points .......................................................................................... 53 4.4 Stability ...................................................................................................................................... 56 4.5 Microscopic Observation ........................................................................................................... 60
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