Membrane emulsification in preparation of single site catalyst

In the theory part the membrane emulsification was studied. Emulsions are used in many industrial areas. Traditionally emulsions are prepared by using high shear in rotor-stator systems or in high pressure homogenizer systems. In membrane emulsification two immiscible liquids are mixed by pressuring one liquid through the membrane into the other liquid. With this technique energy could be saved, more homogeneous droplets could be formed and the amount of surfactant could be decreased. Ziegler-Natta and single-site catalysts are used in olefin polymerization processes. Nowadays, these catalysts are prepared according to traditional mixing emulsification. More homogeneous catalyst particles that have narrower particle size distribution might be prepared with membrane emulsification. The aim of the experimental part was to examine the possibility to prepare single site polypropylene catalyst using membrane emulsification technique. Different membrane materials and solidification techniques of the emulsion were examined. Also the toluene-PFC phase diagram was successfully measured during this thesis work. This phase diagram was used for process optimization. The polytetrafluoroethylene membranes had the largest contact angles with toluene and also the biggest difference between the contact angles measured with PFC and toluene. Despite of the contact angle measurement results no significant difference was noticed between particles prepared using PTFE membrane or metal sinter. The particle size distributions of catalyst prepared in these tests were quite wide. This would probably be fixed by using a membrane with a more homogeneous pore size distribution. It is also possible that the solidification rate has an effect on the particle sizes and particle morphology. When polymeric membranes are compared PTFE is probably still the best material for the process as it had the best chemical durability.

Membrane development for oil contaminated water treatments

The aim of this Master’s thesis study was to develop a membrane for oil contaminated water treatments. Oily wastewaters are a big problem to environment and therefore it is important to find an efficient method for their treatment. There are several treatment methods, but one of the most promising methods is membrane filtration. In the theoretical part of this study the membrane technology and polymeric membrane preparation with phase inversion and membrane modification methods was discussed. It was also told about the most important properties of the membranes. Oily waters, their treatment methods and oily wastewater sources were discussed more specifically. In the experimental part membranes from cellulose acetate were prepared and membranes were modified with two different methods. Modification methods were surface modification and polymer mixing. The modification purpose was to make membranes more hydrophilic and increase surface charge, which can reduce fouling. Membranes were characterized by determining zeta potential, contact angle, oil retention, pure water permeability, pressure-normalized flux and fouling. It were used both synthetic and real spent oil-water emulsion in membrane filtration. Surface modification resulted membranes, which had better properties than unmodified membrane. The amount of substance used in surface modification affected a lot to membrane properties, so it would be necessary to try different amounts of substance to develop the best membrane for oil-water emulsion treatment.

Öljy-vesiemulsioiden erottumisen tehostaminen erilaisten geometrioiden avulla

Työn kirjallisuusosassa selvitettiin neste-nestedispersioiden ja emulsioiden pisarakokojakauman määrittämiseen soveltuvia menetelmiä. Kirjallisuusosa painottuu emulsioiden stabiliteettiin liittyvään teoriaan ja menetelmiin, joilla voidaan tutkia pisarakokojakaumia suoraan prosessista. Erillisnäytteiden analysointiin perustuvista menetelmistä on esitettynä mikroskooppianalyysi sekä lasersäteen sirontaan perustuva mittaus, joita molempia käytettiin tämän työn kokeellisessa osassa. Kokeellisessa osassa pyrittiin selvittämään, vaikuttavatko kaksi erimuotoista ruuvi-kapaletta eri tavalla öljy-vesiemulsion pisarakokojakaumaan, kun emulsio virtasi ruuvin vuorovaikutusalueen läpi. Tätä tutkittiin määrittämällä ennen vuorovaikutusaluetta ja vuorovaikutusalueen jälkeen kerättyjen emulsionäytteiden pisarakokojakaumat lasersäteen sirontamittauksilla. Mitattujen pisarakokojakaumien perusteella ei voitu tehdä varmaa johtopäätöstä, vaikuttivatko ruuvit pisarakokojakaumaan vai eivät. Syynä tähän on pisarakokojakaumien vaihtelu rinnakkaisnäytteissä. Rinnakkaismittauksissa havaittu vaihtelu johtui arvaamattomasti muuttuneista virtausolosuhteista, mikä aiheutti edelleen öljypitoisuuden muutoksia. Muita mahdollisia syitä ovat veden ionivahvuuden, pH:n ja lämpötilan vaihtelu.