• Title/Summary/Keyword: solvent-nonsolvent method

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Liquid-Liquid Phase Separation in a Quaternary System of PolysuIfone/Polyethersulfone/N-Methyl-2-pyrrolidone/water (사성분계 시스템의 액액상분리에 관한 연구 (폴리술폰/폴리에테르술폰/NMP/물))

  • 백기전;김제영;이환광;김성철
    • Proceedings of the Membrane Society of Korea Conference
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    • 1998.04a
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    • pp.22-24
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    • 1998
  • 1. INTRODUCTION : The phase inversion method is widely used to prepare a variety of polymeric membranes ranging from micro-filtration to gas separation. The final morphology obtained by immersion precipitation strongly reflects the thermodynamics and kinetics of the system involved. The equilibrium thermodynamics of the ternary system of polymer/solvent/ nonsolvent is still very important to understand and predict membrane structure. Polysulfone (PSf) and polyethersulfone (PES) are important polymers as membrane materials due to the chemical resistance, mechanical strength, thermal stability and transport properies. There are several reports on the experimental phase diagrams in ternary mixtures of PSf/solvent/nonsolvent, and PES/solvent/nonsolvent. It would be interesting to investigate the solution thermodynamics containing these two polymers since PES is slightly less hyclrophobic than PSf.

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Cr (VI) separation by PolyHIPE membrane immobilized with Aliquat 336 by solvent-nonsolvent method

  • Chen, Jyh-Herng;Mai, Le Thi Tuyet;Hsu, Kai-Chung
    • Membrane and Water Treatment
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    • v.8 no.6
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    • pp.575-590
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    • 2017
  • PolyHIPEs membrane prepared with styrene (St), divinylbenzene (DVB), and ethylhexyl acrylate (EHA) can yield a unique pore structure provided by large voids highly interconnected by many small window throats. With the advantageous pore structure, PolyHIPE presents a potential as a support for carrier facilitated transport membrane. Tricaprylmethylammonium chloride (Aliquat 336) can be efficiently incorporated into the PolyHIPE membrane by a two-step solvent-nonsolvent method to obtain an Aliquat 336-immobilized PolyHIPE membrane with good stability. The study of Cr (VI) transport through Aliquat 336-immobilized PolyHIPE membrane indicates that the membrane has high initial flux and maxima stripping flux ($J_f^o=15.01({\mu}mol/m^2s)$, $J_s^{max}=6.15({\mu}mol/m^2s)$). The reusability study shows that the Aliquat 336-immobilized PolyHIPE membrane can maintain high Cr(VI) recovery efficiency even after 15 cycles of operations. The developed membrane was also used in the separation of Cr (VI) from other anions (i.e., $SO_4{^{2-}}$ and $NO_3{^-}$) and other cations (i.e., Ni (II), Mg (II) and Cu (II)) with good selectivity.

Morphology of Membranes Formed from Polysulfone/Polyethersulfone/N-methyl-2-pyrrolidone/Water System by Immersion Precipitation

  • Baik, Ki-Jun;Kim, Je-Young;Lee, Jae-Sung;Kim, Sung-Chul;Lee, Hwan-Kwang
    • Macromolecular Research
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    • v.9 no.5
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    • pp.285-291
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    • 2001
  • The polysulfone(PSf)/polyethersulfone(PES) blend membranes were prepared by an immersion precipitation method. N-methyl-2-pyrrolidone(NMP) was used as a solvent and water as a nonsolvent. The composition of the coagulation bath and the dope polymer concentration as well as the blend ratio of two polymers were varied. The membrane morphologies were interpreted on the basis of the phase diagram of the PSf/PES/NMP/water system. As the solvent content in the coagulation bath increased in the single polymer system, the number of macrovoids decreased and the morphology was changed from finger-like to cellular structure. In the given bath condition phase separation occurs earlier for the solutions of PSf/PES blend than for those of single polymer. A horizontally layered structure and horizontal protuberances inside the macrovoid were observed for the membranes formed from PSf/PES blend solutions. This peculiar structure formation can be interpreted by a PSf-rich/PES-rich phase separation followed by a polymer-rich/polymer-lean phase separation during the exchange of solvent and nonsolvent.

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Fabrication of Polymethylpentene (PMP) Membranes Using Nonsolvent-Thermally-Induced Phase Separation (N-TIPS) Method (비용매-열유도상분리법(N-TIPS)을 활용한 polymethylpentene (PMP) 분리막 제조기술)

  • Guntak Song;Seung Hwan Kim;Bao Tran Duy Nguyen;Jeong F. Kim
    • Membrane Journal
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    • v.34 no.4
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    • pp.216-223
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    • 2024
  • In comparison to commonly employed polypropylene (PP) material, polymethylpentene (PMP) exhibits low surface energy and reduced crystallinity, allowing fabrication of asymmetric membranes with a dense skin layer. However, its higher melting point poses significant challenges with respect to polymer processability. In this work, we utilized the N-TIPS method, which combines the advantages of non-solvent induced phase separation (NIPS) and thermally induced phase separation (TIPS), to fabricate PMP membranes. Cyclohexane was employed as the solvent for preparing the PMP dope solution, while water, ethanol (EtOH), and isopropanol (IPA) were used as nonsolvents. When cyclohexane-immiscible water was used as the nonsolvent, the resulting membrane exhibited TIPS morphology with unifrom pore structure but lacked suface uniformity. In contrast, when cyclohexane-miscible alcohols (EtOH, IPA) were employed, the membranes displayed NIPS morphology with a dense skin layer with higher mechanical strength. Furthermore, the effect of polyethylene glycol (PEG) as a pore forming agent was investigated to better control the surface pore size.

Investigation of Demixing Phenomena of a Polymer Solution During the Phase Inversion Process

  • Han, Myeong-Jin;D. Bhattacharyya
    • Proceedings of the Membrane Society of Korea Conference
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    • 1995.04a
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    • pp.11-15
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    • 1995
  • Polysulfone (PS) membranes were prepared by the phase inversion process using water or isopropanol as nonsolvent. The Flory-Huggins theory for a ternary system nonsolvent/solvent/polymer is applied to describe the thermodynamic equilibria of the components. The calculated ternary phase equilibria show that demixing of a PS binary solution with n-methylpyrrolidone (NMP) will be fast in a water coagulation bath and will be delayed in an isopropanol bath. The prepared membranes were characterized by SEM, gas adsorption-desorption measurement, and permeability test. The membrane, which is precipitated by fast demixing in a water bath, has nodular structures in the skin region and includes finger-like cavities in the sublayer. The membrane coagulated by isopropanol has a very dense and thick skin structure, which is formed by delayed demixing. The membrane coagulated by isopropanol showed considerably lower pore volume and surface area compared to that observed with water coagulation method. With dimethylformamide (DMF) as solvent and 2-3 wt% of water, the solution can show the liquid-liquid phase separation due to agglomation of the polymer-lean phase from the homogeneous solution. The membranes, which were coagulated near an equilibrium state, show the large (micron size) round pores in the whole membranes. The pores do not contribute the permeation characteristics.

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Preparation of Asymmetric Membranes by Addition of Nonsolvent (비용매 첨가제를 이용한 비대칭막의 제조)

  • Kim, Nowon
    • 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.

Simulation of the Coagulation Process of Poly(acrylonitrile) Wet-Spinning (폴리아크릴로니트릴 습식 방사의 응고공정에 대한 모사연구)

  • 오세천;여영구
    • Proceedings of the Korea Society for Simulation Conference
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    • 1999.10a
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    • pp.186-191
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    • 1999
  • The coagulation process of PAN (poly(acrylonitrile)) wet-spinning was modeled and simulated based on the numerical analysis of the coagulation of a viscous polymer solution by diffusional interchange with a bath. Experiments were performed with gelled solutions of PAN in nitric acid to determine the diffusion rate of solvent and nonsolvent (water) during the coagulation. The experimental data were analyzed by using equations of diffusion coefficient which are the function of the solvent concentrations of the coagulation bath and the filament. The concentration profile of solvent in moving filament was predicted by solving the diffusion model equation numerically. A simplex method was used in the computation of the parameters of the diffusion equations to minimize the difference between the numerical results and experimental data.

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Preparation of Organic-inorganic Hybrid PES Membranes using Fe(II) Clathrochelate (Fe(II) clathrochelate을 이용한 유.무기 PES 복합막의 제조)

  • Jung, Bo Ram;Son, Yeji;Lee, Yong Taek;Kim, Nowon
    • Membrane Journal
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    • v.23 no.1
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    • pp.80-91
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    • 2013
  • Metal-templated condensation of cyclohexanedione dioxime and phenylboronic acid in the presence of Fe(II) sulfate heptahydrate proceeds cleanly in methanol to furnish the Fe(II) clathrochelate. An organic/inorganic hybrid membranes composed of Fe(II) clathrochelate and polyethersulfone was prepared by using phase inversion method. For membrane preparation, the Fe(II) clathrochelate was highly soluble (3~5 g/L) in DMF, NMP, and DMAc, which meets the requirements for the solubility of metal complexes in polar aprotic solvent used in membrane preparation. It was stable even in the presence of strong acids, such as trifluorosactic acid (pKa = 0.3). It was characterized by UV-vis spectroscopy, and their stability in solution phase studied in the presence of (i) strong acids or (ii) competing chelates. Organic/inorganic hybrid membranes were prepared with polyethersulfone, polyvinylpyrrolidone, p-toluenesulfonic acid, Fe(II) clathrochelate and DMF by using nonsolvent induced phase inversion method. The addition of Fe(II) clathrochelate leads increase of surface pore density, mean pore size and flux. We can obtain highly asymmetric membranes by addition of Fe(II) clathrochelate.

Effect of Nonwoven Support During Fabrication of Flat Sheet Membranes via Phase Inversion Method (상전이법 기반 평막 제조과정에서 부직포 영향 분석연구)

  • Kim, Minjae;Kim, Subin;Kim, Sumin;Lee, Hoik;Kim, Jeong F.
    • 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.

The Effects of Solvent and Nonsolvent on Asymmetric Membrane Structure of 6FDA-p-TeMPD Polyimide (6FDA-p-TeMPD 폴리이미드 비대칭막 제조에서 용매와 비용매가 막구조에 미치는 영향)

  • 박노춘;김건중;남세종
    • Membrane Journal
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    • v.8 no.3
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    • pp.157-169
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    • 1998
  • The effects of solvents (DMAc, NMP, 1,4-dioxane) and nonsolvents ($H_2O$, Methanol, n-hexane) on the morphology of 6FDA-p-TeMPD polyimide membrane, prepared by the wet phase inversion method, were studied. In the polymer/solvent/nonsolvent ternary system, the binodal curve, the coagulation value and the relative light transmission were measured, and the solubility parameter difference was calculated. The onset state and rate of liquid-liquid alemixing were predicted and the morphology of membrane was analyzed. It is found that the finger-like pores are formed within discontinuous polymer nodules when the binoclal curve is close to the polymer-solvent (P-S) axis, the coagulation value is small, the reduction of light transmission is easy to occur and the order of solubility parameter difference ($\Delta \delta_{i-j}$) is $\Delta \delta_{S-NS} > \Delta \delta_{P-NS} > \Delta \delta_{P-S}$. The dense skin with small nodules and the sponge type sublayer with macrovoid are formed in the case that the binodal curve is distant from the P-S axis, the onset time of liquid-liquid demixing is long and the order of $\Delta \delta_{i-j}$ is $\Delta \delta_{P-NS} >(\Delta \delta_{S-NS} < > \Delta \delta_{P-S})$. The thick layer of fine nodule coagulation and loosely grown sublayer of nodules appear when the binodal curve is distant from the P-S axis, the onset time of liquid-liquid demixing is very long and the order of $\Delta \delta_{i-j}$$\Delta \delta_{S-NS} > (\Delta \delta_{P-NS}$\lessgtr$ > (\Delta \delta_{P-NS} < >)\Delta \delta_{P-S}$ ).

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