Grafen Katkılı Ultrafiltrasyon Membranların Hazırlanması ve Karakterizasyonu
Özet
Ultrafiltration, a low-pressure membrane process, has attracted more attention
due to the increasing advances in membrane technology. Ultrafiltration is a widely
used process especially in obtaining potable quality clean water, wastewater
treatment and membrane separation processes. The hydrophilic and porous
structure of the membranes plays an important role in membrane separation
processes. Among all inorganic-organic materials, polyvinylidene fluoride (PVDF)
is an excellent material capable of forming membranes. PVDF based membranes
show superior oxidation, thermal stability as well as good mechanical and filmforming
properties. Therefore, PVDF membranes are widely used in many
ultrafiltration processes through various modifications. Graphene has received
considerable scientific interest in recent years due to its superior mechanical,
thermal and electrical properties as well as its large surface area. In composite
preparation, graphene has been frequently used as a nano filler in recent years
to improve the mechanical, electrical and thermal properties of polymers. In this
thesis, nanofiber mats were prepared by electrospinning from PVDF solutions
prepared using suitable solvents. For comparison, PVDF films were also
iv
prepared by solvent evaporation. Composite PVDF materials were prepared to
change the hydrophilic-hydrophobic properties of the membranes. Graphene was
chosen as reinforcement material. First, the graphene was modified with HNO3
to give hydrophilic character to PVDF, then the miscibility of composite formed
by addition of HNO3 modified graphene was changed. PVDF / HNO3 modified
graphene nanofiber mats were prepared by electrospinning method using PVDF
as matrix with HNO3 modified graphene. Characterization studies were
performed using FT-IR, XRD, SEM, TGA / DTG, DSC. In addition, contact angle
measurements were performed to measure surface hydrophobicity. Then, watergasoline
mixtures were separated using PVDF / HNO3 modified graphene
nanofiber mats and films and their separation performances were compared. In
the electrospinning experiments, process and system parameters affecting fiber
diameter and morphology; solvent, polymer solution concentration, molecular
weight were investigated. It has been found that the most suitable solvent mixture
for electrospinning and subsequent film preparation is acetone / DMF. In SEM
images of nanofibers, it was observed that nanofiber diameter increased due to
both solution concentration and molecular weight of PVDF. The composite
structure obtained with HNO3 modified graphene added to provide hydrophilic
structure to the PVDF was fiberized by electrospinning. The addition of HNO3
modified graphene to the structure has led to a reduction in nanofiber diameters,
thereby reducing bead formation and obtaining more homogeneous fibers. It was
confirmed from the FT-IR and XRD results that the acid modification gave the
hydrophilic character to the graphene and thus PVDF with functional ends (such
as –OH) formed on the edges of the graphene, as well as the observations during
the solution preparation. As a result of TGA / DTG and DSC studies, it was
observed that composite nanofibers and films obtained by adding HNO3 modified
graphene to the PVDF matrix were thermally stable and mechanically more
resistant than pure PVDF.