• 한국수소및신에너지학회논문집
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• 제21권4호
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• pp.307-312
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• 2010

Poly (ether sulfone)s with Bisphenol-TP and Bisphenol-AF were prepared with Bisphenol-TP <4,4-dihydroxy tetraphenyl methane>, 4-Fluorophenyl sulfone, and Bisphenol-AF <4,4-(hexafluoroisopropylidene) diphenol> using Potassium carbonate in Sulfolane at $210^{\circ}C$. Sulfonated PBTP-AF were obtained by reaction of Chlorosulfuric acid with copolymers. A series of copolymers were studied by $^1H$-NMR spectroscopy, Differential Scanning Calorimeter (DSC), and Thermo Gravimetric Analysis (TGA). Sorption experiments were conducted to observe the interaction of polymers with water and methanol.

• 한국수소및신에너지학회논문집
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• 제28권1호
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• pp.17-23
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• 2017

Polyether ether ketone (PEEK) composite including tungstophosphoric acid(TPA) membranes have been intensively investigated for polymer electrolyte membrane water electrolysis (PEMWE) and thus covalently linked sulfonated polyether ether ketone (CL-SPEEK) with captured TPA composite membranes were prepared and characterized. Sulfonated polyether ether ketone (SPEEK) was prepared in sulfonation of PEEK and was cross-linked with 1,4 diiodobutane. The carbonyl group of SPEEK was reduced with $NaBH_4$ and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The TPA captured composite was prepared in reaction of TPA with 3-mercaptopropyltrime thoxysilane (MPTMS). The polymer composite membranes showed better thermostability and electrochemical properties than SPEEK. The membranes were prepared by sol-gel casting method. The polymer composite membrane featured 0.1285 S/cm of proton conductivity at $80^{\circ}C$ and outstanding durability.

• 한국수소및신에너지학회논문집
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• 제28권4호
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• pp.338-344
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• 2017

Polyoxometal molybdophosphoric acid (MoPA) bonded polyether ether ketone (PEEK) composite membrane for water electrolysis has been investigated. The composited membrane, covalently cross linked (CL) sulfonated polyether ether ketone (SPEEK) with a bonded MoPA, was prepared in sulfonation of PEEK, cross linkage reaction with 1,4-diiodobutane, and addition with MoPA. PEEK was covalently cross-linked with 1,4-diiodobutane to improve mechanical strength and was added with MoPA to increase proton conductivity. MoPA should be fixed to back bone of SPEEK to prevent bleeding out. Therefore, the carbonyl group of SPEEK was reduced with NaBH4 and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The MoPA bonded composite was produced in the reaction of MoPA with 3-mercaptopropyltrimethoxvsilane (MPTMS). In conclusion, MoPA bonded CL-SPEEK composite membrane featured 0.129 S/cm of proton conductivity at $80^{\circ}C$, and 2,156 hours of chemical stability in Fenton test. These properties are better than those of membranes of other SPEEK system.

• 한국고분자학회:학술대회논문집
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• 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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• pp.58-59
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• 2006

Less than a decade ago, most alternate membrane materials for fuel cells relied upon a post-sulfonation process to generate ionic groups capable of transporting protons from the anode to the cathode. These random post sulfonations showed some promise, but in general they produced materials that were not sufficiently stable or protonically conductive at ion exchange capacities where aqueous swelling could be restricted. Our group began to synthesize disulfonated monomers that could be used to incorporate into random copolymer proton exchange membranes. The expected limitation was that the aromatic polymers might not be stable enough to withstand fuel cell conditions. However, this was mostly based upon an accelerated test known was the Fenton's Reagent Test, which did not seem to this author as being a reliable predictor of performance. A much better approach has been to evaluate the open circuit voltage (OCV) for alternate membranes, as well as the benchmark perfluorosulfonic acid systems. When this is done, the aromatic ionomers of this study, primarily based upon disulfonated polyarylene ether sulfones, show up quite well. Real time 3000 hours DMFC results have also been generated. Obtaining conductive materials at low humidities is another major issue where alternate membranes have not been particularly successful. In order to address this problem, multiblock copolymers with relatively high water diffusion coefficients have been designed, which show promise for conductivity at lowered humidity.

• 멤브레인
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• 제9권3호
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• pp.170-177
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• 1999

Polysulfone을 술폰화하여 물-부탄올 용액의 분리를 위한 투과증발용 비대칭막을 제조하였다. 술론화제로는 chlorosulfoneic acid-trimethyulchlorosilane을 반응시킨 후 이용하였다. FT-IR과 $^1H$-NMR을 이용하여 치환여부를 살펴보았고 술폰화정도는 역적정법과 $^1H$H-NMR을 이용하여 구하였다. DSC와 TGA를 이용하여 열적특성변화를 알아보았다. 비대칭막을 제조하기 위하여 N-methyl-2-pyrrolidone(NMP)rhkdiethyleneglycol dimethyl ether (DGDE)의 혼합용매를 사용하였다. SEM을 이용하여 단면과 skinlayer 의 구조변화를 살펴보았다. 한 연구에서 제조한 비대칭막은 dense film에 비하여 물에 대한 선택도는 거의 변화가 없고 투과유량은 약 80배 정도 증가하였다.

• 폴리머
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• 제24권6호
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• pp.763-769
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• 2000

E-beam 전조사법을 이용하여 아크릴산과 스틸렌 단량체를 폴리프로필렌 섬유에 그라프트 반응시켜 PP-g-(AAc/Sty) 공중합체를 합성하고 술폰화 반응시켜 다관능성 섬유상 양이온 교환체를 합성하였다. 합성체의 그라프트율은 물과 메탄올 혼합비가 30 : 70 vol%인 혼합용매에서 아크릴산과 스틸렌, 단량체비가 30 : 70 vol%일 때 190%로 최대이었으며 혼합용매의 조성비가 일정할 때 아크릴산 단량체의 양이 증가할수록 그라프트율은 감소하였다. 또한 이온교환체의 이온교환용량은 4.6 meq/g이었으며, 술폰화 이온교환체와 아크릴산 이온교환체의 리튬이온에 대한 흡착량을 비교한 결과 본 연구에서 합성한 이온교환체의 흡착성이 우수한 것으로 나타났다.

• Macromolecular Research
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• 제14권4호
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• pp.438-442
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• 2006

Novel sulfonated poly(aryl ether ketones) containing benzoxazole were directly synthesized by aromatic nucleophilic polycondensation using various ratios of 2,2'-bi[2-( 4-flurophenyl)benzoxazol-6-yl]hexafluoropropane to sodium 5,5'-carbonylbis(2-fluorobenzenesulfonate). The copolymers were soluble in polar aprotic solvents such as N-methyl-2-pyrrolidone, N,N-dimethylacetamide, and N,N-dimethylformamide at a relatively high solid composition (>15 wt%) and formed tough, flexible and transparent membranes. The membranes exhibited a degradation temperature of above $290^{\circ}C$. The exact dissolution times of these membranes at $80^{\circ}C$ in Fenton's reagent (3 wt% $H_2O_2$ containing 2 ppm $FeSO_4$) were undetectable, confirming their excellent chemical stability in fuel cell application. The membranes showed a moderate increase in water uptake with respect to increasing temperature. The proton conductivities of the membranes were dependent on the composition and ranged from $1.10{\times}10^{-2}$ to $5.50{\times}10^{-2}Scm^{-1}$ at $80^{\circ}C$ and 95% relative humidity (RH). At $120^{\circ}C$ without externally humidified conditions, the conductivities increased above $10^{-2}Scm^{-1}$ with respect to increasing benzoxazole content, which suggested that the benzoxazole moieties contributed to the proton conduction.

• 대한의용생체공학회:학술대회논문집
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• 대한의용생체공학회 1989년도 춘계학술대회
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• pp.5-6
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• 1989

Polyurethane surface was chemically modified to have different hydrophilic polyethyleneoxide(PEO)/hydrophobic dodecanediol(DDO) groups and negatively charged sulfonate group to investigate the effect to the antithrombogenicity. The hydrophilicity of the surface was significantly increased after PEO grafting or sulfonation. Lowering in-vitro platelet adhesion led to a prologation in the ex-vivo occlusion time. Especially, the sulfonated PU-PEO surface showed most enhanced blood compatibility due to the synergistic effects of PEO and $SO_3$ groups.

• 공업화학
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• 제19권2호
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• pp.205-208
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• 2008

저가인 aromatic elastomer polymer인 polySEBS와 PS의 방향족 작용기에 술폰기를 도입시킴으로써 sulfonated polySEBS과 sulfonated PS를 얻었다. 이 술폰화된 고분자를 활용하여 고분자 전해질 연료전지의 이온 교환막으로 사용될 수 있는 새로운 sulfonated polySEBS/sulfonated PS blending films를 제조하였다. 이 필름들의 수소이온 전도도는 sulfonated polySEBS와 sulfonated PS의 혼합비에 따라 $10^{-2}{\sim}10^{-3}S/cm$로 다양하게 나타났다. 특히, sulfonated polySEBS 10.0 g에 sulfonated PS를 0.5 g 첨가하여 제조한 film이 0.75 meq/g의 이온교환용량 및 25%의 함수율과 함께 가장 우수한 0.07 S/cm의 이온전도도를 나타냈다.

• Macromolecular Research
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• 제16권5호
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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.