• Korean Chemical Engineering Research
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• v.54 no.1
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• pp.57-63
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• 2016

Thermally induced phase separation (TIPS) and nonsolvent induced phase separation (NIPS) were simultaneously induced for the preparation of flat PVDF membranes. N-methyl-2-pyrrolidone (NMP) was used as a solvent and dibutyl-phthlate (DBP) was used as a diluent for PVDF. When PVDF was melt blended with NMP and DBP, crystallization temperature was lowered for TIPS and unstable region was expanded for NIPS. Ratio of solvent to diluent changed the phase separation mechanism to obtain the various membrane structures. Contact mode of dope solution with nonsolvent determined the dominant phase separation behavior. Since heat transfer rate was greater than mass transfer rate, surface structure was formed by NIPS and inner structure was by TIPS. Quenching temperature of dope solution also affected the phase separation mechanism and phase separation rate to result in the variation of structure.

• Membrane Journal
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• v.25 no.1
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• pp.32-41
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• 2015

High performance polysulfone microfiltration membranes with a high were successfully prepared by vapor induced phase separation (VIPS) coupled with non-solvent induced phase separation (NIPS) process. Asymmetric Membranes were prepared with PSF/DMF/PVP/PEG/DMSO/water mixed solutions and water/IPA coagulant. PSF, DMF, PVP, PEG, DMSO, water was used as a membrane polymer, a solvent, a hydrophilic polymer additive, a polar protic liquid polymer, a polar aprotic nonsolvent, and a polar protic nonsolvent in the casting solution, respectively. The addition of polar aprotic nonsolvents, and polar protic nonsolvents is a convenient and effective method to control membrane structure. In order to control the morphology of polymeric membranes, the spontaneous emulsification induced by drawing water vapor into the exposed casting solution surface has been used. Control of the internal morphology of polymeric membranes by using mixed coagulation solution such as water and IPA is discussed in the present work. The pure water permeability, pore size distribution, surface hydrophilicity and membrane morphology were investigated. Due to the addition of DMSO to casting solution, the mean pore size increased almost $0.2{\mu}m$ and the water flux increased about 1000-1800 LMH.

• Membrane Journal
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• v.28 no.3
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• pp.187-195
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• 2018

In this work, the morphology of polyvinylidene-co-hexafluoropropylene (PVDF-co-HFP) membranes were systemically investigated using phase inversion technique, to target membrane contactor applications. As the presence of macrovoids degrade the mechanical integrity of the membranes and jeopardize the long-term stability of membrane contactor processes (e.g. wetting), a wide range of dope compositions and casting conditions was studied to eliminate the undesired macrovoids. The type of solvent had significant effect on the membrane morphology, and the observed morphology were correlated to the physical properties of the solvent and solvent-polymer interactions. In addition, to fabricate macrovoid-free structure, the effects of different coagulation temperatures, inclusion of additives, and addition of nonsolvents were investigated. Due to the slow crystallization rate of P(VDF-co-HFP) polymer, it was found that obtaining porous membrane without macrovoids is difficult using only nonsolvent-induced phase separation method (NIPS). However, combined other phase inversion methods such as evaporation-induced phase separation (EIPS) and vapor-induced phase separation (VIPS), the desired membrane morphology can be obtained without any macrovoids.

• Membrane Journal
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• v.29 no.6
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• pp.348-354
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• 2019

Recently, the application range of organic solvent nanofiltration (OSN) technology has been expanding, requiring membranes with better performance. In this work, thin film composite (TFC) OSN membrane was fabricated. First, ultrafiltration support membrane was prepared via nonsolvent-induced phase separation (NIPS) technique using polysulfone (PSf) and polyethersulfone (PES). Then, the effect of pore forming additives such as polyvinylpyrrolidone (PVP) and pluronic F-127 were employed to improve the membrane permeance. The well-known interfacial polymerization technique was employed using MPD-TMC chemistry to form a thin film on top of the fabricated support, and its solvent permeance and nanofiltration performance was characterized. It was found that polyethersulfone support exhibited more reliable performance compared to polysulfone, and PVP additive was more effective compared to Pluronic F-127. As for the oSN performance, polar aprotic solvents like acetonitrile show significantly higher flux (986.5 L·m^-2·h^-1·bar^-1) compared to water and EtOH (9.5 L·m^-2·h^-1·bar^-1).

• Applied Chemistry for Engineering
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• v.25 no.3
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• pp.274-280
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• 2014

Polysulfone (PSf) hollow fiber membranes were prepared via the nonsolvent induced phase separation technique. The cosolvent of ${\gamma}$-butyrolactone (GBL) was added to the polymer solution containing a mixture of PSf and N,N-dimethylacetamide (DMAc). Water was utilized as a precipitation nonsolvent. The morphology of prepared membranes was investigated using a field emission scanning electron microscopy. The fabricated membrane showed a typical asymmetric structure such as the dense layer on the porous support layer by the addition of GBL to the polymer solution. As the concentration of GBL increased, the asymmetric porous structure was shown to be more intensified. It was thought that the added GBL played a role of enhancing the liquid-liquid phase separation of the polymer solution, since the cosolvent of GBL might change the thermodynamic solubility parameter of the doping solution. Permeation properties through the prepared hollow fiber membranes were characterized by measuring the pure water flux and the solute rejection using $0.05{\mu}m$ polystyrene latex (PSL) beads. Experimental results revealed that the use of PEG as the internal coagulant enhanced the pure water flux up to 130 times compared to the use of EG while the rejection of the PSL beads decreased only 5%.

• Membrane Journal
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• v.32 no.2
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• pp.109-115
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• 2022

In this work, the effect of nonwoven support during fabrication of flat sheet membranes via nonsolvent-induced phase separation, was investigated in detail. It was found that dope solutions with low viscosity tend to penetrate through the nonwoven support during phase inversion, resulting in nonhomogeneous membranes. A simple soaking treatment of nonwoven support prevented such unwanted dope penetration, and resulted in membranes with higher water and solvent permeance performance. The dope penetration through nonwoven was more prominent in solutions with low viscosity, and the nonwoven soaking treatment not effective in solutions with high viscosity.

• Membrane Journal
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• v.31 no.6
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• pp.456-470
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• 2021

In this study, polyetherimide-based hollow fiber membranes were manufactured using the NIPS (nonsolvent induced phase separation) method. THF, Ethanol, and LiNO₃ were used as additives to control the morphology of the PEI-hollow fiber membranes. Furthermore, for the development of a high hydrogen separation membrane, the spinning conditions were optimized through the characterization of SEM and gas permeance. As a result, as the content of THF increased, the hydrogen/carbon dioxide selectivity increased. However, the permeance decreased due to the trade-off relationship. When ethanol was added, a finger-like structure was shown, and when LiNO₃ was added, a sponge structure was shown. In particular, in the case of a hollow fiber membrane with an optimized PDMS coating layer, the permeance was 40 GPU and the hydrogen/carbon dioxide selectivity was 5.6.

• Applied Chemistry for Engineering
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• v.29 no.6
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• pp.759-764
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• 2018

3D porous carbon electrodes (cNPIM), prepared by solution casting of a polymer of intrinsic microporosity (PIM-1) followed by nonsolvent-induced phase separation (NIPS) and carbonization are presented. In order to effectively control the pore size of 3D porous carbon structures, cNPIM was prepared by varying the THF ratio of mixed solvents. The SEM analysis revealed that cNPIMs have a unique 3D macroporous structure having a gradient pore structure, which is expected to grant a smooth and easy ion transfer capability as an electrode material. In addition, the cNPIMs presented a very large specific surface area ($2,101.1m^2/g$) with a narrow micropore size distribution (0.75 nm). Consequently, the cNPIM exhibits a high specific capacitance (304.8 F/g) and superior rate capability of 77% in an aqueous electrolyte. We believe that our approach can provide a variety of new 3D porous carbon materials for the application to an electrochemical energy storage.

• 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.

• Korean Chemical Engineering Research
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• v.59 no.2
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• pp.174-179
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• 2021

Recently, hybrid coal research is underway to upgrade low-grade coal. The hybrid coal is made by mixing low-grade coal with bioliquids such as molasses, sugar cane, and lignin. In the case of lignin used here, a large amount of lignin is included in the wastewater of the papermaking process, and thus, research on hybrid coal production using the same is attracting attention. However, since a large amount of metal ions are contained in the lignin wastewater from the papermaking process, substances that corrode the generator are generated during combustion, and the amount of fly ash is increased. To solve this problem, it is essential to remove metal ions in the lignin wastewater. In this study, metal ions were removed by ion exchange with a alumina hollow fiber membrane coated with K-Phillipsite (K-PHI) zeolite. The alumina hollow fiber membrane used as the support was prepared by the nonsolvent induced phase separation (NIPS) method, and K-PHI seeds were prepared by hydrothermal synthesis. The prepared K-PHI seed was seeded on the surface of the support and coated by secondary growth hydrothermal synthesis. The characteristic of prepared coating membrane was analyzed by Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), Energy Dispersive Spectroscopy (EDX), and the concentration of metal ions before and after ion exchange was measured by Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES). The extraction amount of K+ is 86 mg/kg, and the extraction amount of Na+ is 54.9 mg/kg. Therefore, K-PHI zeolite membrane has the potential to remove potassium and sodium ions from the solution and can be used in acidic lignin wastewater.