• Proceedings of the Membrane Society of Korea Conference
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• 1996.04a
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• pp.40-41
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• 1996

기존에 membrane의 소재로 사용되어 왔던 Polyethersulfone은 막 제조 특성이 우수하고 여러 가지 환경에 대한 저항성이 뛰어나서 많이 이용되어 왔지만 소수성을 띠므로 농도분극과 fouling등 많은 문제점을 안고 있다. 이런 문제점을 극복하기 위하여 친수성의 도입, 물리적, 화학적 세척등 여러 가지 방법을 사용하고 있고 본 연구에서는 hydrophobic Polyethersulfone에 hydrophilic Sulfonate group(-SO$_3$H)을 도입하여 이와같은 문제를 극복하고자 했다. 본 연구에서 사용한 sulfonating agent로는 Chlorosulfonic acid (in CCl$_4$)를 사용하였다.

• Proceedings of the Membrane Society of Korea Conference
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• 1996.10a
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• pp.71-72
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• 1996

Polyetherimide(PEI)계의 고분자는 막 성능이 우수하고 내열성과 내유기용매성 등이 우수한 열가소성수지로서 film, sheet, tubular형으로 만들 수 있어 한외여과막이나 역삼투막, 기체분리막 등에 이용되고 있다. 한편 투과속도를 높이고, fouling을 줄이기 위한 친수성 향상은 막 소재의 화학적 개질에 있어서 주된 목표이다. sulfonation은 막 재질의 소수성을 감소시켜 water permeability를 향상시키는데 있어서 매우 유용한 방법으로 이온교환수지, 이온교환막, anion형 하전막의 제조에 이용되어 왔다. 본 실험에서는 polyetherimide계 고분자를 chlorosulfonic acid(CSA)를 이용하여 술폰화시킨 sulfonated polyetherimide(SPEI)를 제조하여 막 성능을 측정하였다.

• Applied Chemistry for Engineering
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• v.9 no.2
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• pp.249-254
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• 1998

To synthesize cation exchange resin which has thermal stability, the sulfonated poly(ether ether sulfone) (SPEES) was obtained by sulfonation after synthesis of poly(ether ether sulfone) (PEES). It was prepared from hydroquinone and dichlorophenyl sulfone. From FT-IR results, the sulfonation was confirmed by the bands of asymmetric O=S=O stretching of $SO_3Na$ Na group at $1140cm^{-1}$ and S-C stretching at $621cm^{-1}$. The optimum condition of the sulfonation of PEES, based on IR absorbance, was 3 hr of reaction time, $30^{\circ}C$ of reaction temperature, and chlorosulfonic acid of 150 mol%. Ion exchange capacities calculated by the IR absorbance of PEES sulfonated in optimum condition was 6.2 meq/g, which was nearly similar to the ion exchange capacity calculated by titration. When the metal ion was adsorved, small brain, lump, hulled millet shape and compact surface, were observed in the morphology of SPEES.

• Polymer(Korea)
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• v.30 no.6
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• pp.486-491
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• 2006

Heterogeneous membranes were prepared by compression molding for the recovery of ammonium ion from waste water. Degree of sulfonation for sulfonated ion exchange resin increased with increasing amount of chlorosulfonic acid. It was 3.32 meq/g at 10 vol%. The tensile strength and elongation of the heterogeneous membrane was decreased with increasing contents of ion exchange resin. The tensile strength for LLDPE matrix membrane was the highest and also the elongation for EVA matrix membranes were the highest. The water content of heterogeneous membrane was increased with increasing contents of ion exchange resin. The maximum value of transport number for PE matrix membrane was 0.973. The electrical resistance of LLDPE matrix membrane was the lowest. It was value of $10.36{\Omega}/cm^2$ at 70 wt% resins.

• 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 Journal
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• v.9 no.1
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• pp.1-9
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• 1999

Sulfonated polyetherimide having anionic charge and better hydrophilicity than polyetherimide was prepared by reacting polyetherimide with chlorosulfonic acid. To prepare casting solution, from which the membrane having good performance can produce. Polyvinylpyrrolidone as a pore forming agent and volatile weak solvent such as dichloromethane to foml the dense skin layer were added to the sulfonated polyetherimide / N -methyl-2-pyrrolidone solution. Membrane fabricated sulfonated PEl showed better fouling resistance to the protein than those fabricated PEL because of its hydrophilicity. Solute having negative charge was removed effectively with membrane fabricated from the sulfonated PEl because of its the same electron charge.

• Membrane Journal
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• v.6 no.1
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• pp.10-21
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• 1996

This study is undertaken to investigate the major factor which causes a fouling phenomenon in membrane separation system and effect of hydrophilic treatment on fouling repression of hydrophobic polymer (polysulfone, PSf). Chlorosulfonic acid (CSA) and sulfuric acid as a sulfonating agents are used to produce sulfonated PSf (SPSf). SPSf membrane is prepared under several conditions to investigate it's separation process. The extent of fouling-repression is measured by membrane filtration index (MFI) value. With increasing the ion exchange capacity (I.E.C), the flux of SPSf membrane is decreased but the rejection is increased and the flux is less reduced. According to the MFI value, the SPSf membrane has a fouling-retardant effect.

• Textile Coloration and Finishing
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• v.18 no.6 s.91
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• pp.31-36
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• 2006

Study has been made for producing anionic surfactant using waste fleshing scraps from the leather making process through refining, esterification, sulfonation and blending processes. As a most optimum lard oil refining method, refining was carried out for 4 hours under temperature of $120^{\circ}C$ and approximately 200 mbar vacuum, which gave a recovery of more than 80% lard oil. Refined lard oil obtained thus was undergone methlyl-esterification, then sulfonated to make a degreasing agent. By methyl-esterification using lard oil, more than 85% of fatty acid and $12{\sim}13%$ of glycerine were extracted from the oil. Sulfonation of the extracted fatty acid ester lard oil has shown most optimum at $15{\sim}20%$ chlorosulfonic acid content, and the content of bonding sulfate at this time was higher than 3.5%. Finally the followed anionic surfactant having degreasing force of 80% and higher could be made by blending process.

• Membrane Journal
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• v.14 no.2
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• pp.173-184
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• 2004

For the application of direct methanol fuel cell (DMFC), sulfonated polystyrene/teflon (PS/PTFE) composite membranes were developed by changing monomer ratio of styrene and DVB. The composite membranes were prepared as follows: first, the monomer mixtures consisting of styrene, divinyl benzene and AIBN were impregnated in porous PTFE film and then, polymerized under 8$0^{\circ}C$ to give PS/PTFE membranes. Finally, the membranes were reacted with chlorosulfonic acid in 1,2-dichloroethane to give the sulfonated composite membranes. The measurements of ATR-FTIR, SEM, solvent uptake test and ion exchange capacity (IEC) were done for the resulting membranes before or after sulfonation, respectively, which showed the composite membranes with proper crosslinking degree and sulfonic acid content were prepared well as a function of styrene/DVB ratio. ion conductivity and methanol permeability were studied for the sulfonated membranes. It was found that with decreasing the ratio of styrene/DVB, methanol permeability decreased from $6.6{\times}10^{-7}∼1.3{\timas}10^{-7}$ $\textrm{cm}^2$/s, which are much lower values than that of Nafion$^{(R)}$117($1.02{\times}10^{-6}$ $\textrm{cm}^2$/s). Under the same monomer condition, ion conductivity decreased from 0.11 S/cm ($25^{\circ}C$) to 0.08 S/cm ($25^{\circ}C$), which are similar or a little higher values compared with $Nafion^{(R)}117 (1.02{\times}10^{-6}$ $\textrm{cm}^2$/s, 0.0824 S/cm). These two results confirmed the composite membranes prepared could be applied successfully to DMFC.C.

• Proceedings of the Membrane Society of Korea Conference
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• 1996.04a
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• pp.42-43
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• 1996

고분자 분미막을 이용한 분리기술은 기존의 분리기술에 비하여 에너지의 절약과 높은 분리효율 등의 장점이 있어 거의 모든 산업에 이용되고 있다. 분리막의 용도가 다양화됨에 따라서 내열성, 내약품성, 내유기용매성을 갖는 막소재의 개발이 필요하게 되었다. polyimide(PI)게의 고분자는 물리, 화학적 성능이 우수하고 내열성과 내유기용매성 등이 우수한 열가소성수지로서 film, sheet, tubular형으로 만들 수 있어 한외여과막이나 역삼투막, 기체분리막 등에 이용되고 있다. 그러나 투과속도를 높디고, fouling을 줄이기 위해서는 화학적 개질을 통해 친수성을 높이는 방법이 필요하다. 본 실험에서는 내열성과 내유기용매성이 우수한 polyetherimide계 고분자를 chlorosulfonic acid(CSA)를 이용하여 술폰화시킴으로써, 극성기의 도입에 의해 친수성이 향상된 sulfonated polyetherimide(SPEI)를 합성하였다.