This work investigates the structural formation and analyses of titania membranes (TM) prepared using different vacuum exposure times for molecular weight (MW) cut-off performance and oil/water separation. Titania membranes were synthesized via a sol-gel method and coated on macroporous alumina tubes followed by exposure to a vacuum between 30 and 1200 s and then calcined at 400 °C. X-ray diffraction and nitrogen adsorption analyses showed that the crystallite size and particle size of titania increased as a function of vacuum time. All the TM membranes were mesoporous with an average pore diameter of ~3.6 nm with an anatase crystal morphology. Water, glucose, sucrose, and polyvinylpyrrolidone with 40 and 360 kDa (PVP-40 kDa and PVP-360 kDa) were used as feed solutions for MW cut-off and hexadecane solution for oil filtration investigation. The TM membranes were not able to separate glucose and sucrose, thus indicating the membrane pore sizes are larger than the kinetic diameter of sucrose of 0.9 nm, irrespective of vacuum exposure time. They also showed only moderate rejection (20%) of the smaller PVP-40 kDa, however, all the membranes were able to obtain an excellent rejection of near 100% for the larger PVP-360 kDa molecule. Furthermore, the TM membranes were tested for the separation of oil emulsions with a high concentration of oil (3000 ppm), reaching high oil rejections of more than 90% of oil. In general, the water fluxes increased with the vacuum exposure time indicating a pore structural tailoring effect. It is therefore proposed that a mechanism of pore size tailoring was formed by an interconnected network of Ti-O-Ti nanoparticles with inter-particle voids, which increased as TiO₂ nanoparticle size increased as a function of vacuum exposure time, and thus reduced the water transport resistance through the TM membranes.
This research involved carrying out a unique micro-mesoporous carbon particle incorporation into P84 co-polyimide membrane for improved gas separation performance. The carbon filler was prepared using a hard template method from zeolite and known as zeolite-templated carbon (ZTC). This research aims to study the loading amount of ZTC into P84 co-polyimide toward the gas separation performance. The ZTC was prepared using simple impregnation method of sucrose into hard template of zeolite Y. The SEM result showing a dispersed ZTC particle on the membrane surface and cross-section. The pore size distribution (PSD) of ZTC revealed that the particle consists of two characteristics of micro and mesoporous region. It was noted that with only 0.5 wt% of ZTC addition, the permeability was boosted up from 4.68 to 7.06 and from 8.95 to 13.15 barrer, for CO2 and H2 respectively when compared with the neat membrane. On the other hand, the optimum loading was at 1 wt%, where the membrane received thermal stability boost of 10% along with the 62.4 and 35% of selectivity boost of CO2/CH4 and H2/CH4, respectively. It was noted that the position of the filler on the membrane surface was significantly affecting the gas transport mechanism of the membrane. Overall, the results demonstrated that the addition of ZTC with proper filler position is a potential candidate to be applicable in the gas separation involving CO2 and H2.