• Macromolecular Research
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• v.15 no.4
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• pp.379-384
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• 2007

Sulfonation of polyetheretherketones (PEEK) was carried out in order to fabricate commercial perfluorosulfonic acid membrane alternatives, which were characterized in terms of their ion exchange capacity, ionic conductivity, water swelling, methanol crossover and electrochemical performance in their direct application as a methanol fuel cell. A high ion exchange capacity, 1.88, was achieved with a sulfonation reaction time of 8 h, with a significantly low methanol crossover low compared to that of Nafion. However, the morphological stability was found to deteriorate for membranes with sulfonation reaction times exceeding 8 h. Electrochemical cell tests suggested that the fabrication parameters of the membrane electrode assembly based on the sulfonated PEEK membranes should be optimized with respect to the physicochemical properties of the newly prepared membranes.

• Membrane Journal
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• v.25 no.5
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• pp.406-414
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• 2015

In this study, partially fluorinated cation exchange membranes were prepared by direct sulfonation of Poly(VDF-co-hexafluoropropylene) copolymers (PVDF-co-HFP) followed by a casting method for application in the Membrane capacitive deionization (MCDI). The structure of sulfonated PVDF-co-HFP (SPVDF) was confirmed by Fourier-transform infrared (FT-IR) and $^1H$ Nuclear magnetic resonance ($^1H$ NMR) analysis. For quantitative analysis of the chemical composition, the X-ray Photoelectron Spectroscopy (XPS) was used. The membrane properties such as water uptake, ion exchange capacity and electrical resistance were measured. It was suggested that the optimum direct sulfonation condition of PVDF-co-HFP ion exchange membranes was $60^{\circ}C$ and 7 hours for temperature and duration of sulfonation, respectively. The water uptake of the SPVDF ion exchange membrane was 21.5%. The ion exchange capacity and electrical resistance were 0.89 meq/g and $3.70{\Omega}{\cdot}cm^2$, respectively. It was investigated that if it is feasible to apply these membranes in MCDI at various cell potentials (0.9~1.5 V) and initial flow rates (10~40 mL/min). In the MCDI process, the maximum salt removal rate was 62.5% in repeated absorption-desorption cycles.

• Macromolecular Research
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• v.13 no.6
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• pp.514-520
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• 2005

Composite membranes of Nafion and sulfonated poly(arylene ether sulfone) were prepared. Sulfonated poly(arylene ether sulfone)s with different degrees of sulfonation were blended with Nafion to reduce the methanol crossover. The morphology, proton conductivity and methanol permeability of the resulting composite membranes were investigated by SEM, EDAX, AC impedance spectroscopy and permeability measuring instrument. The cross­sections of the composite membranes showed a phase separated morphology. The morphology and phase separation mechanism could be controlled by varying the blend ratio and the degree of sulfonation of poly(arylene ether sulfone). These complex morphologies can be applied for reducing methanol crossover. The methanol permeability and proton conductivity of the composite membranes were lower than those of Nafion 117 membrane since the development of an ionic pathway in the blend membrane was more difficult than that in Nafion itself.

• Journal of Microbiology and Biotechnology
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• v.25 no.10
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• pp.1742-1750
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• 2015

Human insulin is composed of 21 amino acids of an A-chain and 30 amino acids of a B-chain. This is the protein hormone that has the role of blood sugar control. When the recombinant human proinsulin is expressed in Escherichia coli, a serious problem is the formation of an inclusion body. Therefore, the inclusion body must be denatured and refolded under chaotropic agents and suitable reductants. In this study, H27R-proinsulin was refolded from the denatured form with β-mercaptoethanol and urea. The refolding reaction was completed after 15 h at $15^{\circ}C$, whereas the reaction at $25^{\circ}C$ was faster than that at $15^{\circ}C$. The refolding yield at $15^{\circ}C$ was 17% higher than that at $25^{\circ}C$. The refolding reaction could be carried out at a high protein concentration (2 g/l) using direct refolding without sulfonation. The most economical and optimal refolding condition for human preproinsulin was 1.5 g/l protein, 10 mM glycine buffer containing 0.6 M urea, pH 10.6, and 0.3 mM β-mercaptoethanol at $15^{\circ}C$ for 16 h. The maximum refolding yield was 74.8% at $15^{\circ}C$ with 1.5 g/l protein. Moreover, the refolded preproinsulin could be converted into normal mature insulin with two enzymes. The average amount of human insulin was 138.2 g from 200 L of fermentation broth after enzyme reaction with H27R-proinsulin. The direct refolding process for H27R-proinsulin was successfully set up without sulfonation. The step yields for refolding and enzyme reaction were comparatively high. Therefore, our refolding process for production of recombinant insulin may be beneficial to the large-scale production of other biologically active proteins.

• Journal of the Korean Electrochemical Society
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• v.12 no.2
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• pp.173-180
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• 2009

In order to develop a novel polymer electrolyte membrane for direct methanol fuel cell (DMFC), styrene monomer was graft-polymerized into poly(tetrafluoroethylene perfluoropropyl vinyl ether) (PFA) film followed by a sulfonation reaction. The graft polymerization was prepared by the $\Upsilon$-ray radiation-grafting method. Subsequently, sulfonation of the radiation-grafted film was carried out in a chlorosulfonic acid/1,2-dichloroethane (2 v/v%) solution. The chemical, physical, electrochemical and morphological properties of the radiation-grafted membranes (PFA-g-PSSA) were characterized by fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The water uptake, ionic conductivity, and methanol permeability of the PFA-g-PSSA membrane were also measured. The cell performances of MEA prepared with the PFA-g-PSSA membranes were evaluated and the cell resistances were measured by an impedance analyzer. The MEA using PFA-g-PSSA membranes showed superior performance for DMFCs in comparison with the commercial Nafion 112 membrane.

• Macromolecular Research
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• v.16 no.5
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• pp.457-466
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• 2008

The relation between the phase separated morphologies and their transport properties in the polymer blend membrane for direct methanol fuel cell application was studied. In order to enhance the proton conductivity and reduce the methanol crossover, sulfonated poly(arylene ether sulfone) copolymer, with a sulfonation of 60 mol% (sPAES-60), was blended with nonsulfonated poly(ether sulfone) copolymer (RH-2000, Solvay). Various morphologies were obtained by varying the drying condition and the concentration of the casting solution (10, 15, 20 wt%). The transport properties of proton and methanol molecule through the polymer blend membranes were studied according to the absorbed water. AC impedance spectroscopy was used to measure the proton conductivity and a liquid permeability measuring instrument was designed to measure the methanol permeability. The state of water in the blend membranes was confirmed by differential scanning calorimetry and was used to correlate the morphology of the membrane with the membrane transport properties.

• Journal of the Korean Applied Science and Technology
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• v.6 no.2
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• pp.45-51
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• 1989

Allyl aliphatic carboxylates were synthesized by azotropic reaction with benzene between allyl alcohol and capric acid, lauric acid, myristic acid, palmitic acid or stearic acid respectively. allyl aliphatic carboxylates oligomers were prepared from polymerization giving allyl aliphatic carvboxylates in the presence of potassium persulfate in methanol, and the ${\alpha}-sulfonation$ of these five allyl aliphatic carboxylates oligomers were carried by direct addition of dry sulfur trioxide. Especially, molecular weights of fatty acid alylester oligomers and their sodium salts of ${\alpha}-sulfo$ fatty acid allylester oligomers were measured by boiling point method.

• Journal of the Korean Applied Science and Technology
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• v.6 no.1
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• pp.21-26
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• 1989

Four fatty acid vinyl esters were synthesized by transesterification between vinyl acetate and lauric acid, myristic acid, palmitic acid, stearic acid, respectively. Fatty acid vinyl ester oligomers were prepared from polymerization of four fatty acid vinyl esters in the presence of potassium persulfate in methanol. The ${\alpha}-sulfonation$ of these four fatty acid vinyl ester oligomer were carried by direct addition of sulfur trioxide. Especially, molecular weights of sodium ${\alpha}-sulfo$ fatty acid vinyl ester oligomers were measured by boiling point method.

• Membrane Journal
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• v.12 no.4
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• pp.247-254
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• 2002

In order to develop the ion exchange membranes which would be used in direct methanol fuel cell (DMFC), the polysulfone polymer was sulfonated using chlorosulfonic acid (CSA) and trimethylchlorosilane(TMCS). It has been characterized in terms of ion conductivities, methanol crossover, swelling degree and ion exchange capacities for the heat untreated and treated membranes at $150^{\circ}C.$ Typically, the methanol permeability and ion conductivity at the mole ratio of 1.4 between polysulfone repeating unit and sulfonating agents showed $2.87{\times}10^{-7}\; cm^2/s$(without heat treatment), $1.52{\times}10^{-7}\; cm^2/s$(with heat treatment) and $1.10{\times}10^{-2}\; S/cm$(without heat treatment), $0.87{\times}10^{-2}\;$ S/cm(with heat treatment), respectively. After the mole ration of 1.4 both values indicated mild increase.

• Korean Membrane Journal
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• v.9 no.1
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• pp.52-56
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• 2007

A proton exchange membrane was prepared by ${\gamma}-irradiation-induced$ grafting of styrene into poly(tetrafluoro-ethylene-co-perfluoropropyl vinyl ether) (PFA) and subsequent sulfonation reaction. The degree of grafting (DOG) increased with an increase in the absorbed dose. The prepared membranes showed high ion exchange capacity reaching 3.0 meq/g, which exceeded the performance of commercially available perfluorosulfonic acid membranes such as Nafion. The proton conductivity of PFA-g-PSSA membrane increased with the DOG and reached 0.17 S/cm for the highest sample at room temperature. The DMFC performance of the prepared membranes with 50% DOG was comparable to that of Nafion membrane.