Characterization of surface-modified porous PVDF hollow fibers for refinery wastewater treatment using microscopic observation

E. Yuliwati,  A.F. Ismail ,, T. Matsuura , M.A. Kassim , M.S. Abdullah


Microscopic observation was made to investigate the surface structure of porous polyvinylidene fluoride hollow fiber membranes. Field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and the Guerout–Elford–Ferry equation applied for pure water permeation rate were used to determine the average pore sizes. As well, surface roughness parameters and nodule sizes were determined by AFM. The observed unmodified and modified PVDF hollow fiber membranes were prepared by dry-jet wet spinning method from spinning dope mixtures containing 19 wt.% PVDF, 0.98 wt.% lithium chloride (LiCl.H2O) and 0, 1.95, and 3.85 wt.% titanium dioxide (TiO2). Significant difference of spun fibers surface morphology was observed between inner and outer surface by AFM and FESEM. Higher TiO2 concentration formed rougher surfaces, increased average nodule sizes, and decreased the pore size, resulting in lower permeation flux. Pore size obtained from AFM was intermediate  between FESEM and the method based on the Guerout–Elford– Ferry equation.

Keywords: Hollow fiber membranes, Field emission scanning electron microscopy, Atomic force microscopy, Surface roughness, Membrane pore size

download here

Morphological and separation performance study of polysulfone/titanium dioxide (PSF/TiO2) ultrafiltration membranes for humic acid removal

N.A.A. Hamid , A.F. Ismail , T. Matsuura, A.W. Zularisam , W.J. Lau , E. Yuliwati  M.S. Abdullah


In this study, polysulfone (PSF) hollow fiber membranes with enhanced performance for humic acid removal
were prepared from a dope solution containing PSF/DMAc/PVP/TiO2. The main reason for adding titanium
oxide during dope solution preparation was to enhance the antifouling properties of membranes prepared. In the spinning process, air gap distance was varied in order to produce different properties of the hollow fiber membranes. Characterizations were conducted to determine membrane properties such as pure water flux, molecular weight cut off (MWCO), humic acid (HA) rejection and resistance to fouling tendency. The results indicated that the pure water flux and MWCO of membranes increased with an increase in air gap distance while HA retention decreased significantly with increasing air gap. Due to this, it is found that the PSF/TiO2 membrane spun at zero air gap was the best amongst the membranes produced and demonstrated N90% HA rejection. Analytical results from FESEM and AFM also provided supporting evidence to the experimental results obtained. Based on the anti-fouling performance investigation, it was found that membranes with the addition of TiO2 were excellent in mitigating fouling particularly in reducing the fouling resistances due to concentration polarization, cake layer formation and absorption.

key word : Polysulfone, Hollow fiber, Titanium dioxide, Humic acid, Effect of air gap

doenload here

Effect of additives concentration on the surface properties and performance of PVDF ultrafiltration membranes for refinery produced wastewater treatment


The aim of this study was to investigate the effect of pore-forming  hydrophilic additives on the porous asymmetric polyvinylideneflouride (PVDF) ultrafiltration (UF) membrane morphology and transport properties for refinery produced wastewater treatment. PVDF ultrafiltration membranes were prepared via a phase inversion method by dispersing lithium chloride monohydrate (LiCl·H2O) and titanium dioxide (TiO2) nanoparticles in the spinning dope. The morphological and performance tests were conducted on PVDF ultrafiltration membranes prepared from a different additive content. The top surface and cross-sectional area of the membranes were observed using a field emission scanning electron scope (FESEM) and energy dispersive X-ray (EDX) analysis. The surface wettability of porous membranes was determined by the measurement of a contact angle. The mean pore size and surface porosity were calculated based on the permeate flux. The results indicated that the PVDF/LiCl/TiO2 membranes with lower TiO2 nanoparticles loading possessed smaller mean pore size, more apertures inside the membrane with enhanced membrane hydrophilicity. LiCl·H2O has been employed particularly to reduce the thermodynamic miscibility of dope which resulted in increasing the rate of liquid–liquid demixing process. The maximum flux and rejection of refinery wastewater using PVDF ultrafiltration membrane achieved were 82.50 L/m2 h and 98.83% respectively at 1.95 wt.% TiO2 concentration.

Keywords: PVDF membrane, Ultrafiltration, Nanoparticle, Refinery wastewater, Pore forming additives download here