• Title/Summary/Keyword: solvent-nonsolvent method

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Anisotropic Acorn-like Particle Fabrication Via a Dynamic Phase Separation Method (동적 상분리법을 이용한 이방성 도토리형상 입자 제조)

  • Park, Chul Ho;Baek, Il-hyun
    • Membrane Journal
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    • v.29 no.1
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    • pp.61-65
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    • 2019
  • Anisotropic particles have been issued in various fields due to their unique physical properties. Herein, a novel dynamic phase separation method (DPS) is introduced to fabricate anisotropic acorn-like nanoparticles. DPS consists of two dynamic conditions; solvent evaporation and nonsolvent induced precipitation. The bottom layer is controlled by feeding the water as a non-solvent diluent, and the phase separation of the upper layer relies on the diffusion and evaporation of a volatile good solvent. At this condition, the acorn-like particles were fabricated. Under a closed box filled with water (spontaneous phase separation), monodisperse polystyrene (PS) particles were synthesized. At the coexistence between DPS and spontaneous phase separation, the sizes of cap and particle were changed. Also, the volume of PS solutions influences on the particle shape. Since the unique structures could be utilized into various applications, if advanced techniques such as membrane-based controlled water feeding is developed, monodisperse acorn-like particles could be tuned.

Preparation and characterization of PVDF Flat sheet membrane for VMD: Effect of different non-solvent additives and solvents in dope solution

  • Meenakshi Yadav;Sushant Upadhyaya;Kailash Singh
    • Membrane and Water Treatment
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    • v.15 no.4
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    • pp.163-176
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    • 2024
  • Asymmetric flat sheet poly(vinylidene fluoride) (PVDF) membranes were fabricated using the phase inversion technique, employing four distinct solvents with varying solubility power: N, N-dimethylacetamide (DMAc), N, N-dimethylformamide (DMF), Dimethyl sulfoxide (DMSO), and N-Methyl-2-pyrrolidone (NMP). The influence of these solvents on the crystalline properties of the polymers was investigated using X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) to elucidate their role in PVDF polymorphism during membrane formation. Our findings revealed significant variations in membrane crystalline phase due to the dissolution of PVDF in different solvents, with α-polymerization predominant in membranes cast with NMP and DMSO, while DMF and DMAc solvents favored β-type polymerization. Further, various additives including PEG-400, TiO2, LiCl, LiBr, acetone, ethanol, propanol, and water were employed to evaluate their impact on membrane morphology and properties. Scanning electron microscopy (SEM) and Ultimate testing machine (UTM) were utilized to analyze membrane morphology, while the tensile strength, contact angle, pore size, and porosity were estimated using the sessile drop method, imageJ, and gravimetric method, respectively. Our results demonstrated that all additives exerted influence on membrane morphology and properties depending on their characteristics and interactions with solvents and polymers. Notably, acetone, being volatile, facilitated the formation of a thin PVDF layer on the membrane surface, resulting in a reduced average pore size (0.18㎛). Conversely, LiCl and LiBr acted as pore-forming additives, yielding membranes with distinct pore characteristics and porosity. Moreover, water as a non-solvent additive induced pregelation during the nonsolvent-induced phase separation (NIPS) process, thereby promoting pore formation (53% porosity) and enhancing membrane hydrophobicity (104° contact angle). To evaluate the quality of synthesized membranes, permeate flux ranging from 16.2 L/m2.hr to 27.9 L/m2.hr with a salt rejection rate of 98 %, was evaluated using Vacuum Membrane Distillation (VMD).

Characterization and Preparation of PEG-Polyimide Copolymer Asymmetric Flat Sheet Membranes for Carbon Dioxide Separation (이산화탄소 분리를 위한 폴리에틸렌글리콜계 폴리이미드 공중합체 비대칭 평판형 분리막의 제조 및 기체 투과 특성평가)

  • Park, Jeong Ho;Kim, Deuk Ju;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.6
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    • pp.547-557
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    • 2015
  • In this study, we synthesized polyimide with high carbon dioxide gas transport property using 2,2-bis(3,4-carboxylphenyl) hexafluoropropane, 2,3,5,6-tetramethyl-1,4-phenylenediamine and poly(ethylene glycol) bis(3-aminopropyl) terminated and then we calculated solubility parameter of synthesized polymer and non-solvent phase separation coefficient to determine proper solvent for preparation of asymmetric membrane, also we measured the viscosity of the polymer solution to check polymer contents in membrane solution and prepare asymmetric membrane with $LiNO_3$ additives. The morphology and gas separation property of membrane prepared by phase separation method was confirmed using Field Emission Scanning Electron Microsope and the single gas permeation measurement apparatus. We confirmed that the carbon dioxide permeance of the membrane increased and the selectivity showed little change with decreasing of the volatile solvent contents.

Characterization and Preparation of Polyimide Copolymer Membranes by Non-Solvent Induced Phase Separation Method (비용매 유도 상전이법을 이용한 공중합체 폴리이미드 분리막의 제조 및 특성평가)

  • Lee, Jung Moo;Park, Jeong Ho;Kim, Deuk Ju;Lee, Myung Gun;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.4
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    • pp.343-351
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    • 2015
  • In this study, we synthesis polyimide with high gas selectivity using 2,2-bis(3,4-carboxylphenyl) hexafluoropropane, 2,4,6-Trimethyl-1,3-phenylenediamine (DAM) and 4,4-Methylenedianiline (p-MDA), and then the asymmetric membrane was fabricated by non-solvent phase separation method. To confirm the property change of the membrane using different solvent, we measured and compared the viscosity of the polymer solution, cloud point and non-solvent phase separation coefficient. The morphology and gas separation property of membrane prepared by phase separation method was confirmed using Field Emission Scanning Electron Microsope and the single gas permeation measurement apparatus. The single gas ($CH_4$, $N_2$, $O_2$, $CO_2$) permeation property and selectivity value of the membrane prepared with NMP was higher than the membrane prepared with DMAc. We confirmed that the gas selectivity of the membrane increased and the permeation property decreased with increasing of the solvent evaporation time.

Morphology of Membrane of Acrylic Polymers by Wet Phase Inversion Method (습식 상 역전 방법으로 제조한 아크릴계 고분자 막의 모폴로지)

  • Choi Seung-Eun;Park Han-Soo;Lee Kwang-Hee
    • Polymer(Korea)
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    • v.30 no.2
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    • pp.108-111
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    • 2006
  • In this work, the effect of the hydrophobicity of acrylic polymers on the membrane morphology was investigated. The membranes were prepared with poly(methyl methacrylate) (PMMA), poly(ethyl methacrylate) (PEMA), poly (butyl methacrylate) (PBMA), poly(isobutyl methacrylate), and their blends using the wet phase inversion method. PMMA and PEMA having a relatively less hydrophobicity formed the channel-like structure, whereas PBMA and PIBMA having more hydrophobic units formed the finger-like structure. These morphological changes were attributed to differences in the solidification process of the polymer-rich phase determine d by the polymer/solvent/nonsolvent ternary phase diagram. The membrane structures of the blends were controlled by the main component of their blends.

A Separation of manganese (II) and cobalt (II) ions by D2EHPA/TBP-immobilized PolyHIPE membrane

  • Chen, Jyh-Herng;Mai, Le Thi Tuyet
    • Membrane and Water Treatment
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    • v.10 no.2
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    • pp.127-137
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    • 2019
  • The D2EHPA/TBP co-extractants immobilized PolyHIPE membrane can be used for the selective separation of Mn (II) from Co (II). By solvent-nonsolvent method, D2EHPA/TBP co-extractants can be effectively immobilized into PolyHIPE membrane. The pore structure of PolyHIPE membrane and the presence of TBP enhance the stability of immobilized co-extractants. The optimal operating conditions for the separation of Mn (II) and Co (II) are feeding phase at pH 5.5, sulfuric acid concentration in the stripping phase of about 50 g/L and stirring speed at 400 rpm. The D2EHPA/TBP co-extractants ratio of 5:1 shows synergetic effect on Mn/Co separation factor about 22.74. The removal rate and recovery rate of Mn (II) is about 98.4 and 97.1%, respectively, while for Co (II) the transport efficiency is insignificant. The kinetic study of Mn (II) transport shows that high initial flux, $J_f^o=80.1({\mu}mol/m^2s)$, and maxima stripping flux, $J_s^{max}=20.8({\mu}mol/m^2s)$, can be achieved with D2EHPA/TBP co-extractants immobilized PolyHIPE membrane. The stability and reusability study shows that the membrane can maintain a long term performance with high efficiency. High purity of Co (II) and Mn (II) can be recovered from the feeding phase and stripping phase, respectively.

Controlling the Morphology of Polyvinylidene-co-hexafluoropropylene (PVDF-co-HFP) Membranes Via Phase Inversion Method (상전이법을 이용한 P(VDF-co-HFP) 분리막 구조제어)

  • Song, Ye Jin;Kim, Jong Hoo;Kim, Ye Som;Kim, Sang Deuk;Cho, Young Hoon;Park, Ho Sik;Nam, Seung Eun;Park, You In;Son, Eun Ho;Kim, Jeong F.
    • 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.

Preparation of an Inorganic Scintillator Loaded Film for the Measurement of Surface Contamination and its Performance Test (표면오염 측정용 무기섬광 함침 필름의 제조 및 성능 평가)

  • 서범경;이근우;임난주;박진호;한명진
    • Journal of Energy Engineering
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    • v.13 no.2
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    • pp.93-100
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    • 2004
  • The smear media possible to sampling and radiation detection was prepared and evaluated for the surface contamination using indirect method. The films were made by impregnating Cerium Activated Yttrium Silicate (CAYS) in a polysulfone membrane. The membranes used solution as a dimethylformamide (DMF) and methylene chloride (MC), polysulfone as a polymer matrix and CAYS as a inorganic scintillator. The proximity membranes were prepared with single- and double-layered structure. The solidified methods were immersion to the nonsolvent bath such at water and ethanol and solvent evaporation. The measurement of the photon produced by interaction with radiation and inorganic scintillator used a photomultiflier tube (PMT), amplifier, and counter. In the comparison with the low background alpha/beta counter, the counter rate using inorganic scintillator proximity membrane for the $\^$14/C surface contamination was about 50%. Also. the $^3$H counting results revealed that the prepared membranes were efficient to monitor the surface contaminated with the low energy be-ray emitter nuclides.

Characterizations of Modified Silica Nanoparticles(II) ; Preparation and Application of Silica Nanoparticles as a Environmentally Filler

  • Min, Seong-Kee;Bae, Deok-Kwun;Park, Sang-Bo;Yoo, Seong-Il;Lee, Won-Ki;Park, Chan-Young;Seul, Soo-Duk
    • Korean Journal of Materials Research
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    • v.22 no.8
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    • pp.433-438
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    • 2012
  • A chemical process involves polymerization within microspheres, whereas a physical process involves the dispersion of polymer in a nonsolvent. Nano-sized monodisperse microspheres are usually prepared by chemical processes such as water-based emulsions, seed suspension polymerization, nonaqueous dispersion polymerization, and precipitation polymerizations. Polymerization was performed in a four-necked, separate-type flask equipped with a stirrer, a condenser, a nitrogen inlet, and a rubber stopper for adding the initiator with a syringe. Nitrogen was bubbled through the mixture of reagents for 1 hr. before elevating the temperature. Functional silane (3-mercaptopropyl)trimethoxysilane (MPTMS) was used for the modification of silica nanoparticles and the self-assembled monolayers obtained were characterized by X-ray photoelectron spectroscopy (XPS), laser scattering system (LSS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), elemental analysis (EA), and thermogravimetric analysis (TGA). In addition, polymer microspheres were polymerized by radical polymerization of ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) and acrylamide monomer via precipitation polymerization; then, their characteristics were investigated. From the elemental analysis results, it can be concluded that the conversion rate of acrylamide monomer was 93% and that polyacrylamide grafted to MPSN nanospheres via the radical precipitation polymerization with AAm in ethanol solvent. The microspheres were successfully polymerized by the 'graft from' method.

Effect of Polymer Structure on Membrane Morphology by Addition of 2-butoxyethanol (2-butoxyethanol 첨가에 따른 고분자 구조가 분리막 구조에 미치는 영향)

  • Son, Ye-Ji;Kim, No-Won
    • Membrane Journal
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    • v.21 no.4
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    • pp.377-388
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    • 2011
  • Flat sheet microfiltration membranes were prepared with polysulfone (PSF), polyethersulfone (PES), and polyphenylsulfone (PPS) by an immersion precipitation phase inversion method. In this method, dimethyl formamide (DMF) and polyvinylpyrrolidone (PVP) were used as a solvent and a wetting polymer additive, respectively. 2-butoxyethanol (BE) was used as a nonsolvent additive catalyst to form pore. The morphology of membranes was investigated by scanning electron microscopy and micropermporometer. The permeability of the membranes was evaluated with the flux of pure water. When the BE was added, the pore size of membranes became larger than blank membranes. The changes in the morphology of membrane due to the BE addition depend on polymer structure. All membranes have similar mean pore size and porosity. The mean pore sizes of PSF, PES, and PPS membranes were 0.282, 0.330 $0.308{\mu}m$, respectively. The porosities of PSF, PES and PPS membranes were 68.5, 66.1, 66.4%, respectively. However, the PPS membrane showed higher pore density on surface and narrower pore size distribution than PSF or PES membrane does. As a result, the pure water flux of PPS membrane ($357L/m^2\;hr$) was higher than that of PSF ($196L/m^2\;hr$) or PES membrane ($214L/m^2\;hr$).