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Title: Interafacial tension and surfactant stabilisation during membrane emulsification
Author: Silva, Pedro T. Santos
ISNI:       0000 0004 7651 4315
Awarding Body: Loughborough University
Current Institution: Loughborough University
Date of Award: 2018
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A new insight on the interaction between complex fluids and solid surfaces is given in this study. It is demonstrated how these liquid-solid interactions can greatly influence the droplet generation during membrane emulsification and, therefore, resultant emulsion size and uniformity. These aspects of the process are often underestimated and poorly comprehended by, specially, industrial colleagues. Thus, that unawareness can lead to poor results and to a disbelief in this upcoming technology. A novel membrane emulsification system is reported consisting of a tubular metal membrane, periodically azimuthally (tangentially) oscillated with frequencies up to 50 Hz and 7 mm displacement in a gently cross flowing continuous phase. Using an azimuthally oscillating membrane, oil-in-water (o/w) emulsions were experimentally produced with a diameter of 20 120 µm, and a coefficient of variation (CV) of droplet size of 8%. The drop size was correlated with shear stress at the membrane surface using a force balance. In a single pass of continuous phase, it was possible to achieve high dispersed phase concentrations up to 38% v/v. A vertical oscillation membrane emulsification was used to study the influence of dynamic interfacial tension in membrane emulsification: drop size can be tuned between 35 and 85 µm by changing the surfactant concentration in the continuous phase. In addition, a method to determine the percentage of active pores during membrane emulsification is demonstrated. This method links knowledge acquired in the surfactant adsorption dynamics and drop expansion rate. This study reinforces the importance of dynamic interfacial tension which must be considered in process design, and modelling purposes, particularly in two liquid phase systems using membranes such as membrane emulsification at high injection rates. Hydrophobization of metal surfaces is reported based on silanization reactions to broaden the use of metal porous membranes to water-in-oil (w/o) emulsion production. The developed procedure is shown to be a straightforward hydrophobization method, with minimal cost to apply, reproducible, stable and the possibility of reuse of the membrane after losing hydrophobicity by simply reapplying the hydrophobization method. On the other hand, formation of water-based droplets can be achieved using a hydrophilic porous metal membrane. To investigate this, water-based droplets were produced using a hydrophilic membrane and wetting experiments were also carried out: sessile droplets were used to determine static contact angles and a rotating drum system was used to determine contact angles under dynamic conditions. In the latter case the three-phase contact line was observed between the rotating drum and two immiscible liquids. It was observed that the oil phase can preferably wet a hydrophilic surface in case when a surfactant is present in the oil phase, and above a certain concentration, even in the presence of the water phase. Apart from membrane emulsification, spontaneous formation of water droplets in kerosene was observed, facilitated by the presence of an oil soluble surfactant: Span® 80. This process was characterized and the influence of chemical potential between both phases was evaluated. Nano-sizing analyses were performed for a set of experiments, where the influence of the surfactant concentration in the organic phase, as well as the influence of NaCl concentration in the aqueous phase, was studied. Water droplets between 100 and 400 nm were measured in kerosene. Interfacial tension between both phases, was not lower than 4 mN/m. Therefore, ultra-low interfacial tension was not required for this process to occur spontaneously. Continuous production of spherical polymeric particles, via membrane emulsification, was demonstrated. An o/w emulsion was used as precursor and, by solvent removal, solid particles were obtained. In addition, production of polycaprolactone (PCL) particles containing encapsulated (entrapped) protein model was also demonstrated via a double emulsion method.
Supervisor: Not available Sponsor: Marie Curie Initial Training Network
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available