• Membrane Journal
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• v.24 no.2
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• pp.158-166
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• 2014

In this research, microporous and bicontinuous poly vinylidene fluoride(PVDF) hollow fiber membranes were prepared via hybrid process of the thermally induced phase separation (TIPS) and stretching method. The mechanism of the membrane preparation is based on liquid-liquid phase separation. The final membranes have characteristic structures which have both bicontinuous and fibrillar morphology by applying the stretching method. They showed quite different structure when compared with the spherulitic or nodular structure from S/L TIPS and bicontinuous structure from L/L TIPS. At first, PVDF hollow fiber precursors were prepared via TIPS method using various kind of diluent mixtures. We used gamma-butyrolacton, dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP) as diluents. We could make hollow fiber membranes which had porous outer surface or dense outer surface by controling the parameters such as cooling conditions, PVDF concentration and the ratio of diluent mixtures. Finally, these hollow fiber were stretched at room temperature and diluents were extracted by ethanol. Effects of the stretching ratio on the membrane morphology were investigated using scanning electron microscope (SEM), and its effects on water flux, porosity, pore size, roughness and tensile strength were examined.

• Membrane Journal
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• v.24 no.3
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• pp.177-184
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• 2014

Silica membranes with high permeability were prepared using colloidal and polymeric silica sols on a porous stainless steel-tube support by a DRFF and SRFF method. Silica sols were derived with tetraethylorthosilicate (TEOS) by sol-gel method and analyzed with DLS, FE-SEM, and $N_2$ adsorption. The coating of the intermediate layer with colloidal silica sol on the stainless steel-tube support led to a denser surface morphology of the membrane along with a considerable reduction in the number of surface defect. As the polymeric silica sol enclosed the colloidal silica sol with spherical particles during the SRFF method, the separation-layer-coated silica membrane showed a denser surface than the intermediate layer. Moreover, the silica membranes showed high hydrogen gas permeability of $(6.63-9.21){\times}10^{-5}mol{\cdot}m^{-2}{\cdot}s^{-1}{\cdot}Pa^{-1}$ with low $H_2/N_2$ perm-selectivity (2.9-3.1) at room temperatures.

• Bulletin of the Korean Chemical Society
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• v.25 no.9
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• pp.1371-1378
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• 2004

A porous stainless steel (SUS) as a substrate of silica composite membranes for hydrogen purification was used to improve mechanical strength of the membranes for industrial application. The SUS support was successfully modified by using submicron Ni powder, $SiO_2$ sols with particle size of 500 nm and 150 nm in turns. Silica top layer was coated on the modified supports under various preparation conditions such as calcination temperature, dipping time and repeating number of dipping-drying process. The calcination temperature for proper sintering was between H ttig temperature and Tamman temperature of the coating materials. Maximum hydrogen selectivity was investigated by changing dipping time. As repeating number of dipping-drying process increased, permeances of nitrogen and hydrogen were decreased and $H_2/N_2$ selectivity was increased due to the reduction of non-selective pinholes and mesopores. For the silica membrane prepared under optimized conditions, permeance of hydrogen was about $3\;{\times}\;10^{-5}\;cm^3{\cdot}cm^{-2}{\cdot}s^{-1}{\cdot}cmHg^{-1}$ combined with $H_2/N_2$ seletivity of about 20.

• Membrane Journal
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• v.11 no.3
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• pp.124-132
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• 2001

Silica membranes were prepared on a porous ${\alpha}$-alumina tube with pore size of 150nm by sol-gel and chemical vapor deposition(CVD) method for hydrogen separation at high temperatures. Silica and ${\gamma}$-lumina membranes formed by the sol-gel method possessed a large amount of mesopores of a Knudsen diffusion regime. In order to improve the $H_2$ selectivity, silica was deposited in the sol-gel derived silica/${\gamma}$-alumina layer by thermal decomposition of tetraethyl orthosilicate(TEOS) at $600^{\circ}C$. The CVD with forced cross flow through the porous wall of the support was very effective in plugging mesopores that were left unplugged in the membranes. The CVD modified silica/alumina composite membrane completely rejected nitrogen permeation and thus showed a high $H_2$ selectivity by molecular sieve effect. the permeation of hydrogen was explained by activated diffusion and the activation energy was 9.52kJ/mol.

• Membrane Journal
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• v.33 no.5
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• pp.257-268
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• 2023

Membrane capacitive deionization (MCDI) is a variation of the conventional CDI process that can improve desalination efficiency by employing an ion-exchange membrane (IEM) together with a porous carbon electrode. The IEM is a key component that greatly affects the performance of MCDI. In this study, we attempted to derive the optimal fabricating factors for IEMs that can significantly improve the desalination efficiency of MCDI. For this purpose, pore-filled IEMs (PFIEMs) were then fabricated by filling the pores of the PE porous support film with monomers and carrying out in-situ photopolymerization. As a result of the experiment, the prepared PFIEMs showed excellent electrochemical properties that can be applied to various desalination and energy conversion processes. In addition, through the correlation analysis between MCDI performance and membrane characteristic parameters, it was found that controlling the degree of crosslinking of the membranes and maximizing permselectivity within a sufficiently low level of membrane electrical resistance are the most desirable membrane fabricating condition for improving MCDI performance.

• Korean Chemical Engineering Research
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• v.43 no.1
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• pp.16-20
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• 2005

Porous polypropylene membranes were prepared by a thermally induced phase separation method in super-critical $CO_2$, where polypropylene and Camphene were used as raw materials. The porosity of polypropylene membranes with 10 wt% polypropylene concentration was 78, 80, 73% by using methanol, ethanol, and n-buthanol as an analytical solvent, respectively. The tensile strength increased with an increasing polypropylene concentration, where it was $0.17kg_f/mm^2$ at 10 wt% polypropylene concentration. The extraction rate for Camphene increased with time and Camphene was removed 94% in 5 min. It increased with an increasing temperature and was 99% at $45^{\circ}C$, however, decreased with an increasing temperature at higher than $45^{\circ}C$. The extraction rate increased with an increasing pressue up to 150 bar, however, decreased slightly with an increasing pressure over 150 bar. The extraction rate had a relation with the solubility of Camphene in supercritical $CO_2$.

• Membrane Journal
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• v.9 no.2
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• pp.97-106
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• 1999

A and 2SM-5 type zeoli tic crystal films were synthesized on porous supports from the reaction mixture of 1.9 ${SiO}_2$1.5 $Na_20-Al_2O_3-40$ $H_20$ and $Si0_2$-0.l3 $Na_2O$-52 $H_20$-O.l2 TPAOH composition, respectively. The zeolite films were characterized by XRD and SEM. The 2SM -5 crystals grown on the porous matrix were very closely bound together. It was so difficult to obtain the perfectly intergrown crystals in the case of A-type zeolite and this crystal was transformed into P-type zeolite membrane with a prolonged reaction time. The densely intergrown A type zeolite crystal membrane could be also synthesized by the hydrothermal treatment at 100$^{\cirt}C$ after pressing the reaction mixture without addition of water. The pervaporation performance of the synthesized porous inorganic membranes was investigated for alcohol and water mixtures. A-type zeolite membrane crystallized as a thin film showed the selective \'Jermeability of water from the mixtures through the molecular sieving activity of micropores.

• Membrane Journal
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• v.20 no.2
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• pp.159-168
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• 2010

In this study, high porous PVdF flat sheet membranes were prepared to obtain reinforced membrane support for polymer electrolyte membrane fuel cell. Nano-size laponite was randomly dispersed in the membranes to improve mechanical property which lowered by the high porosity. The morphology and porosity of prepared PVdF/Laponite composite membranes were examined using the SEM analysis and the weight method and all membranes showed over 60% porosity. The membrane thermal stability depending on the laponite contents in the composite membranes was evaluated by membrane heat shrinkage at $105^{\circ}C$ and $135^{\circ}C$. MD and TD heat shrinkage of the PVdF composite membrane containing 5 wt% laponite was 2~3% and 2~3.5% at $135^{\circ}C$, respectively. The mechanical strength was enhanced after incorporating laponite particles and 30% increase in the modulus compared to pure PVdF membrane was obtained.

• Membrane Journal
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• v.22 no.3
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• pp.191-200
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• 2012

New composite membranes were manufactured by impregnating post-sulfonated poly(arylene ether sulfone)s containing perfluorocyclobutane (PFCB) groups into porous polytetrafluoroethylene (PTFE) films. Two kinds of post-sulfonated poly(arylene ether sulfone)s with two different monomer ratios (sulfonable biphenylene monomer : non-sulfonable sulfonyl monomer = 6 : 4, 4 : 6) were first prepared through three synthetic steps: synthesis of trifluorovinylether-terminated monomers, thermal cycloaddition polymerization and post-sulfonation using chlorosulfonic acid (CSA). The composite membranes were then prepared by adjusting the concentrations (5~20 wt%) of the resulting copolymers impregnated in the PTFE films. The water uptake, ion exchange capacity (IEC) and ion conductivity of the composite membranes were characterized and compared with their unreinforced dense membranes and Nafion. All the synthesized compounds, monomers and polymers were characterized by $^1H$-NMR, $^{19}F$-NMR and FT-IR and the composite membranes were observed with scanning electron micrographs (SEM).

• Membrane and Water Treatment
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• v.6 no.3
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• pp.205-224
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• 2015

A novel hydrophilic poly (vinylidene fluoride)/poly (p-phenylene terephthalamide) (PVDF/PPTA) blend membrane was prepared by in situ polycondensation of p-phenylene diamine (PPD) and terephthaloyl chloride (TPC) in PVDF solution with subsequent nonsolvent induced phase separation (NIPS) process. For comparison, conventional solution blend membrane was prepared directly by adding PVDF powder into PPTA polycondensation solution. Blend membranes were characterized by means of viscometry, X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM). The effects of different blending methods on membrane performance including water contact angle (WCA), mechanical strength, anti-fouling and anti-compression properties were investigated and compared. Stronger interactions between PVDF and PPTA in in situ blend membranes were verified by viscosity and XPS analysis. The incorporation of PPTA accelerated the demixing rate and caused the formation of a more porous structure in blend membranes. In situ blend membranes exhibited better hydrophilicity and higher tensile strength. The optimal values of WCA and tensile strength were $65^{\circ}$ and 34.1 MPa, which were reduced by 26.1% and increased by 26.3% compared with pure PVDF membrane. Additionally, antifouling properties of in situ blend membranes were greatly improved than pure PVDF membrane with an increasing of flux recovery ratio by 25%. Excellent anti-compression properties were obtained in in situ blend membranes with a stable pore morphology. The correlations among membrane formation mechanism, structure and performance were also discussed.