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PEMFC용 설폰화 Poly(ether ether ketone) (SPEEK) 전기방사 나노섬유 이온교환막의 제조 및 특성
곽노석(Noh Seok Kwak),최은정(Eun Jung Choi),황택성(Taek Sung Hwang) 한국고분자학회 2012 폴리머 Vol.36 No.2
전기방사 방법으로 sulfonated poly(ether ether ketone) (SPEEK) 나노섬유를 제조하고, 압축성형법으로 고분 자 전해질막 연료전지(polymer electrolyte membrane fuel cell, PEMFC)용 나노섬유막을 제조하였다. SPEEK의 최 대 설폰화율은 95% 이었고 초기 열분해 온도는 약 280 oC로 PEEK 보다 낮았으며 접촉각은 설폰화도가 증가함에 따라 감소하였다. 전기방사 나노섬유의 최적 인가전압, 유속, 방사거리(tip to collector distance, TCD) 및 농도는 각각 22 kV, 0.3 mL/hr, 5 cm, 23 wt% 이었고 평균 섬유직경은 47.6 nm 이었다. 한편, SPEEK 이온교환 나노섬유막 의 함수율 및 이온교환용량은 설폰화 시간과 설폰화제 함량이 증가함에 따라 증가하였으며 최적값은 각각 20%, 2.03 meq/g으로 Nafion 117 보다 우수하였다. 막의 전기저항은 설폰화 시간이 증가함에 따라 감소하였고 그 값은 0.58~0.06 Ω·cm2로 측정되었다. 또한 막의 수소이온전도도는 설폰화 시간이 증가함에 따라 증가하였으며 최대 0.099 S/cm로 Nafion 117 보다 우수하였다. Sulfonated poly(ether ether ketone) (SPEEK) nanofibers were prepared by electrospinning. The nanofibrous membrane for polymer electrolyte membrane fuel cell (PEMFC) was fabricated by compression molding. The maximum degree of sulfonation was 95% and the initial thermal degradation temperature was 280 oC and it`s value was lower than that of PEEK. The contact angle of SPEEK increased with decreasing the degree of sulfonation. The optimum voltage, flow rate, tip to collector distance (TCD) and concentration of electrospinning conditions were 22 kV, 0.3 mL/hr, 15 cm, and 23 wt%, respectively. The average nanofibrous diameter was 47.6 nm. The water uptake and ion exchange capacity of SPEEK nanofibrous membrane increased with increasing the sulfonation time and the amount of sulfonating agent. The electrical resistance and proton ionic conductivity of SPEEK membrane increased with decreasing and increasing the sulfonation time, respectively. Their values were 0.58~0.06 Ω·cm2 and 0.099 S/cm.
막 축전식 탈염용 비불소계 아민화 Poly(vinylbenzyl chloride-co-ethyl methacrylate-co-styrene) 음이온교환막의 합성 및 특성
구진선(Jin Sun Koo),곽노석(Noh Seok Kwak),황택성(Taek Sung Hwang) 한국고분자학회 2012 폴리머 Vol.36 No.5
본 연구에서는 막축전식 탈염(membrane capacitive deionization, MCDI) 공정용 음이온교환막의 제조를 위하여 vinylbenzyl chloride-co-ethyl methacrylate-co-styrene(VBC-EMA-St) 공중합체를 합성하였으며, 아민화 반응과 열처리를 통하여 음이온교환막을 제조하였다. 구조확인을 위하여 FTIR 분석을 하였고, GPC와 TGA를 통하여 합성한 고분자의 분자량과 분자분포, 열안정성을 분석하였으며, 함수율 및 이온교환용량을 측정하였다. 또한 LCR meter로 전기저항을 측정하고, MCDI 공정에 적용하기 위하여 제조한 음이온교환막을 충방전 시험 측정하였다. 이온교환용량, 함수율, 전기저항, 분자량은 각각 1.69 meq/g, 23.7%, 1.61 Ω·cm, 3.4×10(4) g/mol이었으며, CDI 충방전 시험 결과 상용화막인 AMX보다 우수한 성능을 나타내었다. A terpolymer of vinylbenzyl chloride-co-ethyl methacrylate-co-styrene (VBC-EMA-St) was prepared for membrane capacitive deionization (MCDI) by radical polymerization and amination reaction of various amination times. Nonfluoro aminated VBC-EMA-St anion-exchange membranes were characterized by Fourier transform infrared (FTIR) spectrometry. Molecular weight, polydispersity and thermal stability were obtained by gel permeation chromatography (GPC) and thermogravimetric analysis (TGA). The basic properties such as water uptake, ion exchange capacity, electrical resistance and CDI charge-discharge current were measured. The optimal values of ion exchange capacity, water uptake, electrical resistance and molecular weight of synthesized anion-exchange membrane were 1.69 meq/g, 23.7%, 1.61 Ω·cm and 3.4×10(4) g/mol, respectively. As compared with conventional membrane, the pattern of cyclic charge-discharge current of synthesized anion-exchange membrane indicated efficient electrosorption and desorption.
술폰화 반응에 의한 High impact polystyrene(HIPS) 양이온교환막의 제조 및 특성
김용태 ( Yong Tae Kim ),곽노석 ( Noh Seok Kwak ),이철호 ( Choul Ho Lee ),진창수 ( Chang Soo Jin ),황택성 ( Taek Sung Hwang ) 한국화학공학회 2011 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.49 No.2
In this study, ion exchange membranes were prepared using high impact polystyrene(HIPS) with various crosslinking and sulfonation time. Degree of sulfonation(DS) of sulfonated HIPS(SHIPS) membrane was increased with sulfonation time and decreased with crosslinking time. The highest value of DS was 66%. Also, water uptake and ion exchange capacity(IEC) of SHIPS membrane were decreased with degree of crosslinking and increased with sulfonation time. Then their values were 35.2% and 1.55meq/g, respectively. Electrical resistance and ion conductivity of the membranes were showed more excellent value with sulfonation time. The maximum value of electrical resistance and ion conductivity were 0.4Ω·cm2 and 0.1 S/cm, respectively. It is indicated that the SHIPS membrane has the higher performance compare with Nation 117. Durability of SHIPS membranes in a organic solvent was increased with increasing crosslinking time. The surface roughness of HIPS membranes were confirmed with SEM that was become uneven surface with progressing sulfonation.
전바나듐계 레독스-흐름 전지용 IPA-co-HDO-co-(TPA/MA) 음이온교환막의 합성 및 특성
황택성(Taek Sung Hwang),정재철(Jae Chul Jung),곽노석(Noh Seok Kwak) 한국고분자학회 2011 폴리머 Vol.35 No.6
본 연구에서는 전바나듐 레독스-흐름 전지용 음이온교환막의 제조를 위하여 isophthalic acid (IPA), 1,6- hexanediol(HDO), terephthalic acid(TPA), maleic anhydride(MA)의 용융 축합중합 방법에 의해 IPA-co- HDO-co-(TPA/MA)(IHTM) 공중합체를 합성하였다. 합성된 IHTM 공중합체 아민화 반응을 trimethylamine으로 하였으며, UV 가교 반응을 통하여 음이온교환막을 제조하였다. IHTM 공중합체의 구조 및 열안정성을 FTIR, 1H NMR, TGA 분석을 통하여 확인하였다. 또한 IHTM 음이온교환막의 함수율, 이온교환용량, 전기저항, 전기전도도를 중량법, 적정법 및 LCR 미터로 측정하였으며, 전바나듐 레독스-흐름 전지의 효율 실험을 하였다. 막의 이온교환용량, 전기저항, 전기전도도는 각각 1.10 meq/g, 1.98 Ω·cm2, 0.009 S/cm로 우수하게 나타났으며, 전바나듐 레독스-흐 름 전지의 충·방전효율, 전압효율 및 에너지효율은 각각 96.5, 74.6, 70.0%이었다. The IPA-co-HDO-co-(TPA/MA) copolymers for all-vanadium redox flow battery were synthesized by melt condensation polymerization using isophthalic acid(IPA), 1,6-hexandiol (HDO), terephthalic acid(TPA) and maleic anhydride(MA). The amination of chloromethylated IPA-co- HDOco-( TPA/MA)(CIHTM) copolymer was carried out using trimethylamine, and the anion exchange membrane was also prepared by UV crosslinking reaction. The structure and thermal stability of IHTM copolymers were confirmed by FTIR, 1H NMR, and TGA analysis. The anion membrane properties such as water uptake, ion exchange capacity, electric resistance and electrical conductivity, were measured by gravimetry, titration and LCR meter. The efficiency of the all-vanadium redox flow battery was analyzed. The ion exchange capacity, electric resistance and electrical conductivity were 1.10 meq/g, 1.98 Ω· cm2, and 0.009 S/cm, respectively. The efficiency of charge-discharge, voltage, and energy for the allvanadium redox flow battery were 96.5, 74.6, 70.0%, respectively.