• Title/Summary/Keyword: 1H-NMR spectroscopy

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Synthesis and Characterization of Proton Conducting Graft Copolymer Membranes (수소이온 전도성 가지형 공중합체 전해질막 제조 및 분석)

  • Roh, Dong Kyu;Koh, Jong Kwan;Seo, Jin Ah;Kim, Jong Hak
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.126.2-126.2
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    • 2010
  • The "grafting from" technology to prepare the well-defined microphase-separated structure of polymer using atom transfer radical polymerization (ATRP) will be introduced in this presentation. Various amphiphilic comb copolymers were synthesized through this approach using poly (vinylidene fluoride) (PVDF), poly (vinylidene fluoride-co-chlorotrifluoroethylene) (P(VDF-co-CTFE) and poly(vinyl chloride) (PVC) as a macroinitiator. Hydrophilic side chains such as poly (styrene sulfonic acid) (PSSA) or poly (sulfopropyl methacrylate) (PSPMA) were grafted from the mains chains using direct initiation of the chlorine atoms. The structure of mass transport channels has been controlled and fixed by crosslinking the hydrophobic domains, which also provides the greater mechanical properties of membranes. Successful synthesis and microphase-separated structure of the polymer were confirmed by $^1H$ NMR, FT-IR spectroscopy and TEM. The grafted/crosslinked membranes exhibited good mechanical properties (400 MPa of Young's modulus) and high thermal stability (up to $300^{\circ}C$), as determined by a universal testing machine (UTM) and TGA, respectively.

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Novel Electroluminescent Polymer Derived from Pyrene-Functionalized Polyaniline

  • Amarnath, Chellachamy Anbalagan;Kim, Hyoung-Kun;Yi, Dong-Kee;Lee, Sang-Hyup;Do, Young-Rag;Paik, Un-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1495-1499
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    • 2011
  • A solution processable polymer was synthesized, by incorporating pyrene groups into the backbone of the polyaniline chain, and used as an emissive layer in an organic light emitting diode. The polyaniline base was reacted with acid chloride of pyrene butyric acid to form pyrene-functionalized polyaniline chains. The source of pyrene moiety was acid chloride of pyrene butyric acid. The formation of polymer from acid chloride of pyrene butyric acid and polyaniline was confirmed by the FTIR and $^1H$-NMR spectroscopy. Differential scanning calorimetry revealed high glass transition temperature of 210 $^{\circ}C$. Due to the presence of pyrene moieties in the backbone, the polyaniline synthesized in the present study is solution processable with light emitting property. The photoluminescence spectrum of the polymer revealed that emission lies in the blue region, with a peak at 475 nm. The light emitting device of this polymer exhibits the turn-on voltage of 15 V.

Novel Pyridinium Iodide Containing Siloxane High Performance Electrolyte for Dye-Sensitized Solar Cell

  • Lee, Soonho;Jeon, Youngtae;Lim, Youngdon;Cho, Younggil;Lee, Sangyoung;Kim, Whangi
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2583-2588
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    • 2013
  • A new type of solid and gel-state ionics based on siloxane pyridinium iodides was synthesized and used as electrolytes in dye-sensitized solar cells. The resulting electrolytes were characterized by $^1H$ NMR spectroscopy, TGA and diffusion coefficient. The synthesized siloxane pyridinium iodide electrolytes have characteristics of different chain length of siloxane moieties. The ion conductivities were given 2.7-3.2 S/cm. Among the three SiDPIs based electrolytes, DSSC employing the SiDPI2 gives an open circuit voltage of 0.704 V, a short-circuit current of 15.85 $mA/cm^2$ and conversion efficiency of 6.8% under light intensity of 100 $mW/cm^2$. In addition, the performance of the DSSCs showed relatively reasonable compared with the propylpyridinium iodide (PPI) electrolyte.

Synthesis and Characterization of Poly(ether Sulfone)s Containing Bisphenol-TP for PEMFC (고분자 전해질 막 연료전지를 위한 Bisphenol-TP를 포함한 Poly(ether sulfone)s 고분자 막의 합성과 특성)

  • Lim, Young-Don;Seo, Dong-Wan;Lee, Soon-Ho;Islam, Monirul;Kang, Da-Lib;Kim, Whan-Gi
    • Transactions of the Korean hydrogen and new energy society
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    • v.21 no.4
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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.

Synthesis and Characterization of Phenanthrene-substituted Fullerene Derivatives as Electron Acceptors for P3HT-based Polymer Solar Cells

  • Mi, Dongbo;Park, Jong Baek;Xu, Fei;Kim, Hee Un;Kim, Ji-Hoon;Hwang, Do-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1647-1653
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    • 2014
  • 9,10-Bis(bromomethyl)phenanthrene reacted with fullerenes via a Diels-Alder reaction to give phenanthrene-substituted fullerene mono-adducts (PCMA) and bis-adducts (PCBA) as electron acceptors for organic photovoltaic cells (OPVs). The syntheses of the fullerene derivatives were confirmed by $^1H$ $^{13}C$ NMR spectroscopy and MALDI-TOF mass spectrometry. PCMA and PCBA showed better light absorption in the UV-visible region than $PC_{61}BM$. Their electrochemical properties were measured using cyclic voltammetry. Accordingly, the lowest unoccupied molecular orbital (LUMO) energy levels of PCMA and PCBA were -3.66 and -3.57 eV, respectively. Photovoltaic cells were fabricated with a ITO/PEDOT:PSS/poly(3-hexylthiophene)(P3HT):acceptor/LiF/Al configuration, where P3HT and PCBA are the electron donors and acceptors, respectively. The polymer solar cell fabricated using the P3HT:PCBA active layer showed a maximum power conversion efficiency of 0.71%.

Novel Imidazolium Ionic Liquids Containing Quaternary Ammonium Iodide or Secondary Amine for Dye-sensitized Solar Cell

  • Seo, Dong-Wan;Lim, Young-Don;Lee, Soon-Ho;Ur, Soon-Chul;Kim, Whan-Gi
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2633-2636
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    • 2011
  • A new type of ionic liquid based on N-(3-aminepropyl)imidazolium iodide, called IIQAI, which consists of imidazolium and quaternary ammonium salt, and APII-(hydroxyethyl, propyl, hexyl) were synthesized and used as ionic liquid in dye-sensitized solar cells. APII-hexyl is solid, whereas IIQAI, APII-(hydroxyethyl, propyl) are viscous liquids. The synthesized ionic liquid showed relative thermal stability compared to the commercial ionic liquid of DMII. Among them, IIQAI was more stable than the other ionic liquid because of the two salt groups. APII-hydroxyethyl, which contains two hydroxyl groups, showed low viscosity with good flow. New types of ionic liquids were examined by $^1H$-NMR spectroscopy, thermo gravimetric analysis (TGA). IIQAI enabled a solar energy conversion efficiency of 6.3%, which is slightly higher than that of the referenced (DMII, 6.2%).

Synthesis, Structure, and Thermal Property of Poly(trimethylene terephthalate- co-trimethylene 2,6-naphthalate) Copolymers

  • Jeong, Young-Gyu;Jo, Won-Ho;Lee, Sang-Cheol
    • Fibers and Polymers
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    • v.5 no.3
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    • pp.245-251
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    • 2004
  • Poly(trimethylene terephthalate-co-trimethylene 2,6-naphthalate)s (P(TT-co-TN)s) with various copolymer composition were synthesized, and their chain structure, thermal property and crystalline structure were investigated by using $^1$H-NMR spectroscopy, differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD), respectively. It was found from sequence analysis that all the P(TT-co-TN) copolymers synthesized have a statistical random distribution of TT and TN units. It was also observed from DSC thermograms that the glass transition temperature increases linearly with increasing the TN comonomer content, whereas the melting temperature of copolymer decreases with increasing the corresponding comonomer content in respective PTT- and PTN-based copolymer, showing pseudo-eutectic melting behavior. All the samples melt-crystallized isothermally except for P(TT-co-66 mol % TN) exhibit multiple melting endotherms and clear X-ray diffraction patterns. The multiple melting behavior originates from the dual lamellar population and/or the melting-recrystallization-remelting. The X-ray diffraction patterns are largely divided into two classes depending on the copolymer composition, i.e., PTT and PTN $\beta$-form diffraction patterns, without exhibiting cocrystallization.

Characteristic as a Gene Delivery System of Water Soluble Chitosan Conjugated with Cationic Peptide (양이온 펩타이드가 컨쥬게이트된 수용성 키토산의 유전자 전달체로서의 특성)

  • Kim, Young-Min;Kim, Ji-Ho;Park, Seong-Cheol;Park, Yung-Hoon;Jang, Mi-Kyeong
    • KSBB Journal
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    • v.31 no.4
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    • pp.300-311
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    • 2016
  • Recently gene delivery has been designed newly using bioactive biomaterial and applied in the various field by many researchers. In this study, we proposed a new gene delivery system which has the capability of targeting effect in the specific tissue and remarkably enhanced transfection efficiency. We investigated $^1H-NMR$ spectroscopy, particle size analyzer and gel retardation to confirm the correct preparation of gene delivery. Also, we identified the hemo-compatibility of gene delivery by hemolysis assay, non-cytotoxicity by MTT test and transfection efficiency. The uptake mechanism of the gene carrier was confirmed using inhibitor agent such as sodium azide, indomethacin, quercetin, colchicine, and chloropromazine. As a results, it was identified that gene carrier prepared by in this study entered in the cell by the microtubule-dependent, energy-dependent and clathrin-mediated endocytosis pathway.

Sonochemical Synthesis of Closed [5,6]-bridged Aziridino[70]fullerene Derivative and Self-assembled Multilayer Films

  • Yoon, Shin-Sook;Hwang, Sung-Ho;Hong, Sung-Kyu;Lee, Jeong-Ho;Ko, Weon-Bae
    • Carbon letters
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    • v.10 no.4
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    • pp.325-328
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    • 2009
  • This cycloaddition of [70]fullerene with methyl azidoacetate in benzene under ultrasonic irradiated condition afforded the closed [5,6]-bridged aziridino[70]fullerene derivative, which was unusual product of cycloaddition to the 5,6-junction of fullerene. Its structure was determined by FAB-MS, UV-vis, $^1H-$ and $^{13}C$-NMR spectral data. The closed [5,6]-bridged aziridino[70]fullerene-functionalized gold nanoparticle films were self-assembled using the layer-by-layer method on the reactive of glass slides functionalized with 3-mercaptopropyl trimethoxysilane. The functionalized glass slides were alternately soaked in the solution containing closed the [5,6]-bridged aziridino[70]fullerene and 4-aminothiophenoxide/hexanethiolate-protected gold nanoparticles. The closed [5,6]-bridged aziridino[70]fullerene-functionalized gold nanoparticle films have grown up to 5 layers depending on the immersion time. The self-assembled nanoparticle multilayer films were characterized using UV-vis spectroscopy showed that the surface plasmon band of gold at 527 nm gradually became more evident as successive layers were added to the films.

Inclusion Complex of Analgesic and antiinflammatory Agents with Cyclodextrins (II) : Effect of $2-Hydroxypropyl-{\beta}-cyclodextrin$ on the Release of Ibuprofen Suppository (시클로덱스트린과 소염진통제간의 포접복합체에 관한 연구 (II) : 2-히드록시프로필-${\beta}$-시클로덱스트린이 이부프로펜 좌제의 방출에 미치는 영향)

  • Oh, In-Joon;Lee, Mi-Young;Lee, Yong-Bok;Shin, Sang-Chul
    • Journal of Pharmaceutical Investigation
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    • v.27 no.3
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    • pp.165-171
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    • 1997
  • Ibuprofen, a nonsteroidal antiinflammatory, analgesic and antipyretic drug, has several limitations in clinical application because of low solubility in water and gastrointestinal irritation. Effect of ibuprofen/$2-Hydroxypropyl-{\beta}-cyclodextrin\;(HP{\beta}CD)$ inclusion compound on release of suppository was investigated. Complex formation was confirmed by $^{1}H-\;and\;^{13}C-NMR$ spectroscopy. The release of ibuprofen from suppository base in vitro was significantly increased by the complexation with $HP{\beta}CD$. The release of ibuprofen from hydrophilic base was faster than that from hydrophobic base. In vivo studies, the release rate of ibuprofen from suppository was accelerated after rectal administration in complex form. This results suggested that ibuprofen/$HP{\beta}CD$ complex can be practically used for suppository to have faster effect of ibuprofen with reduced side effect.

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