• Title/Summary/Keyword: high-pressure NMR

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Equimolar Carbon Dioxide Absorption by Ether Functionalized Imidazolium Ionic Liquids

  • Sharma, Pankaj;Park, Sang-Do;Park, Ki-Tae;Jeong, Soon-Kwan;Nam, Sung-Chan;Baek, Il-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2325-2332
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    • 2012
  • A series $[C_3Omim]$[X] of imidazolium cation-based ILs, with ether functional group on the alkyl side-chain have been synthesized and structure of the materials were confirmed by various techniques like $^1H$, $^{13}C$ NMR spectroscopy, MS-ESI, FTIR spectroscopy and EA. More specifically, the influence of changing the anion with same cation is carried out. The absorption capacity of $CO_2$ for ILs were evaluated at 30 and $50^{\circ}C$ at ambient pressure (0-1.6 bar). Ether functionalized ILs shows significantly high absorption capacity for $CO_2$. In general, the $CO_2$ absorption capacity of ILs increased with a rise in pressure and decreased when temperature was raised. The obtained results showed that absorption capacity reached about 0.9 mol $CO_2$ per mol of IL at $30^{\circ}C$. The most probable mechanism of interaction of $CO_2$ with ILs were investigated using FTIR spectroscopy, $^{13}C$ NMR spectroscopy and result shows that the absorption of $CO_2$ in ether functionalized ILs is a chemical process. The $CO_2$ absorption results and detailed study indicates the predominance of 1:1 mechanism, where the $CO_2$ reacts with one IL to form a carbamic acid. The $CO_2$ absorption capacity of ILs for different anions follows the trend: $BF_4$ < DCA < $PF_6$ < TfO < $Tf_2N$. Moreover, the as-synthesized ILs is selective, thermally stable, long life operational and can be recycled at a temperature of $70^{\circ}C$ or under vacuum and can be used repeatedly.

Thermal and Optical Properties of Heat-Resistant Core Materials in Plastic Optical Fiber (내열성 플라스틱 광섬유 코어재료의 열적 및 광학적 성질)

  • Lee Gyu-Ho;Cho Won-Keun;Park Min;Lee Hyun-Jung
    • Polymer(Korea)
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    • v.30 no.2
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    • pp.158-161
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    • 2006
  • Recently the application of plastic optical fiber (POF) in automotives and planes demands the heat-resistant and high refractive index con materials. We synthesized polyglutarimides (PGIs) via imidization of PMMA with primary amines under high pressure and high temperature and investigated thermal and optical properties by varying the molar ratio of amines and the type of amines (ethyl amine vs. isopropyl mine). The degree of imidization was calculated based on the peak intensity in $^1H$ NMR and FTIR. We found that the glass transition temperature $(T_g)$ of PGIs increased over $30^{\circ}C$ compared to the traditional core materials in POF, PMMA, and they are stable up to $300\sim400^{\circ}C$. PGIs anthesized with ethyl mine show the better heat resistance than those with isopropyl amines. Additionally, they show the comparable transparency and higher refractive index than PMMA. It implies that they can be utilized as the excellent photo-efficient and heat-resistant core materials in POF.

Synthesis of Acrylic Nonionic Reactive Emulsifier with Aromatic Ring and the Properties of Water-based Acryl Pressure Sensitive Adhesive (방향족 고리를 가지는 아크릴계 비이온 반응성 유화제 합성 및 이를 이용한 수성 점착제 물성 연구)

  • Yeom, Do-Young;Kim, Dong Hwan;Hwang, Gaeun;Hwang, Do-Hoon;Jung, Yu Jin
    • Journal of Adhesion and Interface
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    • v.22 no.2
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    • pp.31-38
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    • 2021
  • In this study, a nonionic reactive emulsifier with aromatic and acryl group was synthesized by using polyoxyethylene(10) dodecylphenyl ether with 3-butenoic acid. The synthesized nonionic reactive emulsifier was confirmed by 1H-NMR and FT-IR. In addition, the reactive emulsifier synthesized in the preparation of aqueous acrylic adhesives base emulsion was used and the properties of the solid content, conversion, particle size distribution, peel strength and high temperature holding force were compared to those of nonionic emulsifiers without aromatic group. The particle size was distributed from 370 nm to 698 nm, and the peel strength were measured in the range of 1.507~1.802 kgf. The high temperature holding force of prepared adhesives base emulsion were measured in the range of 0.50~2.00 mm. Especially, in the result of synthesized nonionic reactive emulsifier with aromatic group, it was confirmed that high temperature holding force results were the most excellent than the case of using other nonionic reactive emulsifiers, and it can be useful for water-based acryl pressure sensitive adhesive.

Preparation and Permeation Characteristics of PTMSP-PDMS-Silica/PEI Composite Membranes (PTMSP-PDMS-Silica/PEI 복합막의 제조 및 투과특성)

  • Lee, Hyun-Kyung;Hong, Se-Lyung
    • Membrane Journal
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    • v.18 no.2
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    • pp.146-156
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    • 2008
  • In this study, PTMSP of high permeability and high molecular weight was synthesized, and PTMSP-PDMS graft copolymer was synthesized from poly [1-(trimethylsily)propyne] (PTMSP) and hydroxy-terminated poly(dimethylsiloxane) (PDMS). The PTMSP-PDMS-silica composites were prepared by the addition of 15, 30, or 50 wt% tetraethoxysilane (TEOS) to PTMSP-PDMS graft copolymer by sol-gel process. To investigate the physico-chemical characteristics of PTMSP-PDMS-silica/PEI composite membranes, the analytical methods such as $^1H$-NMR, FT-IR, TGA, XPS, GPC, and SEM have been utilized. The gas permeability and selectivity properties of $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4,\;n-C_4H_{10}$, were evaluated. Permeability of the composite membranes increased as TEOS content and pressure increased. Selectivity of $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4,\;and\;n-C_4H_{10}$, showed the maximum value at 30 wt% of TEOS content and decreased thereafter.

Synthesis and Photovoltaic Properties of Conducting Polymers Based on Phenothiazine (Phenothiazine계 전도성고분자의 합성 및 유기박막태양전지로의 적용 연구)

  • Yoo, Han-Sol;Park, Yong-Sung
    • Applied Chemistry for Engineering
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    • v.24 no.1
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    • pp.93-98
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    • 2013
  • In this paper, four conducting polymers (poly[(N-butyl-phenothiazine)-sulfide] (PBPS), poly[(N-hexyl-phenothiazine)-sulfide] (PHPS), poly[(N-decyl-phenothiazine)-sulfide] (PDPS), and poly[(N-(2-ethylhexyl)-phenothiazine)-sulfide] (PEHPS)) were synthesized with a high temperature and high pressure reaction. The structures of synthesized polymers were confirmed by $^1H-NMR$ and characterized by UV-Vis, cyclic voltammetry, and GPC. From the UV-Vis absorption spectra, the ${\lambda}_{max}$ values of PBPS, PHPS, PDPS, and PEHPS were 338, 341, 340, and 334 nm, respectively and their optical band gaps were 3.11, 3.13, 3.16, and 3.05 eV, respectively. To evaluate the feasible applicability as a photovoltaic cell, the devices composed of for example, ITO/PEDOT : PSS/polymer (PBPS, PDPS) : $PC_{71}BM$ (1 : 3, w/w)/$BaF_2$/Ba/Al were fabricated using the blends of the PBPS and PDPS as a donor, and $PC_{71}BM$ as an acceptor. Then, the power conversion efficiencies (PCE) of devices were estimated as 0.076% of PBPS and 0.136% of PDPS by solar simulator.

Phase equilibria and structure identification of tert-butylhydroperoxide + gaseous clathrate hydrates (이성분계(3차 부틸-히드로과산화물 + 기체) 클러스레이트 하이드레이트의 구조적 특성과 열역학적 안정성에 관한 연구)

  • Youn, Yeobeom;Cha, Minjun;Kwon, Minchul;Lee, Huen
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.150.1-150.1
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    • 2011
  • Structure-II hydrate has been highlighted due to its higher gas storage capacity and favorable thermodynamic conditions. In this study, we introduce a new structure-II hydrate former, tert-butyl hydroperoxide (TBHP) and confirm the structural characteristics through High-Resolution Powder Diffraction (HRPD), $^{13}C$ solide-state NMR and Ramanspectroscopy. Here,we also investigated the thermodynamic stability of binary(TBHP+gaseous) clathrate hydrates. The experimental data were generated using an isochoric pressure-search method. The dissociation data for (TBHP +gaseous) clathrate hydrates are compared with the other hydrocarbon hydrate and pure gaseous hydrate.

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Screening of Inhibitory Effect of Edible Mushrooms on Tyrosinase and Isolation of Active Component (한국산 식용버섯류의 Tyrosinase 활성 저해 검색 및 그 유효성분 분리)

  • 박영현;장성근
    • Journal of Food Hygiene and Safety
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    • v.12 no.3
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    • pp.195-199
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    • 1997
  • For the purpose of isolation and screening of tyrosinase inhibitory activity from edible mushrooms, Pleurotus ostreatus, Auricularia auricula-Judae, Umbilicaria esculenta, Agaricus bisporus, Flammuline velutipes, Lentinus edodes, Ganoderma lucidum, and Coriouls versicolor were examined by tracing inhibitory activities against tyrosinase, utilizing L-3,4-dihydroxyphenylalanine (L-DOPA) as a substrate. Among the eight edible mushrooms tested, Umbilicaria esculenta showed potent enzyme inhibitory activities above 7804% against tyrosinase in ethylacetate (EtOAc) extracts. Ganoderma lucidum and Agaricus bisporus showed inhibitory activities of 67.3% and 51.5% in water extracts. EtOAc extracts of Umbilicaria esculenta was fractionated from silicagel column chromatography and one fraction showed the most inhibitory activity of 60.9%. The three bands (Rf=0.38, 0.27, 0.19) were isolated from preparative TLC of the fraction for purification and identified as mixtures of orsellinate, methyl orsellinate, methyl lecanorate, and methyl gyrophorate by high pressure liquid chromatography (HPLC), ultravisible spectrophotometer (UV), mass spectrophotometer (Mass), nuclear magnetic resonance spectrometer (NMR).

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Synthesis and Photoisomerization Properties of Polynorbornenes with Azobenzene Chromophores

  • Kang, Suk-Hoon;Shin, Hee-Deuk;Oh, Cha-Hwan;Choi, Dong-Hoon;Park, Ki-Hong
    • Bulletin of the Korean Chemical Society
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    • v.23 no.7
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    • pp.957-963
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    • 2002
  • We successfully synthesized the addition-type polynorbonenes (PNB) exhibiting photochromic properties and excellent thermal stability. Three norbornene-based monomers with different azobenzene moiety (R=NO2, H,OCH3) were synthesized by transesterification method. The corresponding PNB copolymers were synthesized by transition metal-catalyzed addition polymerization method, and characterized by GPC, UV-Vis spectroscopy, NMR, and thermal analysis. For comparison of the photochromic properties depending on the rigidity of polymer backbone, we prepared the polymethylmethacrylate (PMMA) copolymer with the corresponding azobenzene moiety. We investigated the photoisomerization behavior by means of optical muitichannel analyzer with Xe lamp as well as real-time UV-Vis spectroscopy with high-pressure mercury lamp. Among three PNB copolymers, a polymer with azobenzene (R=H) was the most adaptable for observation of photoisomerization behavior. It was found that the rate of photoisomerization and relaxation depended on the structure of azobenzene chromophore, rather than that of polymer backbone.

Changes in Chemical Compositions of Pumpkin(Cucurbita moschata DUCH.) Seed Sprouts (호박(Cucurbita moschata DUCH.)종실의 발아 성장 과정 중 성분 변화)

  • 이병진;장희순;이규희;오만진
    • Food Science and Preservation
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    • v.10 no.4
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    • pp.527-533
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    • 2003
  • This study was performed for increasing the consumption and developing the function of pumpkin(Cucurbita moschata DUCH.) seed. The changes of the contents of general chemical compositions, fatty acids, amino acids, ascorbic acid and ${\beta}$-carotene during sprouting were analyzed. Also, the bitter taste, which was produced during sprouting, were purified by using thin layer chromatography and preparative high pressure liquid chromatography. The purified bitter compound was identified by mass spectrum and nuclear magnetic resonance($^1$H '||'&'||' $\^$13/C-NMR). Weight of pumpkin seed sprout was increased to 348.4% and the length of stem was dramatically increased at 8 days. In each head and stem parts of the pumpkin seed sprout, the contents of protein and lipid were decreased, however, the contents of fiber, ash and soluble inorganic nitrogen were increased. The fatty acids of the pumpkin seed sprout were mainly represented as linoleic acid, oleic acid, palmitic acid and stearic acid. During sprouting, palmitic acid was gradually increased, reversely, linoleic acid was gradually decreased. The general amino acids of head part in the pumpkin seed sprout grown at 23$^{\circ}C$ during 8 days were orderly more contained glycine, alanine, arginine, cystein and proline. Those of free amino acids were orderly more contained arginine, threonine, alanine and glutamine. The contents of L-ascorbic acid and ${\beta}$-camtene of the pumpkin seed sprout were gradually increased with increasing sprouting days. The bitter taste material of head part of the pumpkin seed sprout was detected at Rf value 0.72 on silicagel TLC plate and separuted as one peak by HPLC. The chemical structure of the puified bitter compound was identified as a cucurbitacin glycoside by MS and NMR. The content of bitter compound at 8 days was contained 42.2 mg per 1kg sprout head.

Study of CO2 Absorption Characteristic and Synthesis of 1-(2-methoxyethyl)-3-methylimidazoLium Methanesulfonate Ionic Liquid (1-(2-methoxyethyl)-3-methylimidazolium Methanesulfonate 이온성 액체 합성 및 CO2 흡수 특성 연구)

  • Jin, Yu Ran;Jung, Yoon Ho;Park, So Jin;Baek, Il Hyun
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.35-40
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    • 2012
  • In this study, 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate ionic liquid has been synthesized, characterized and tested with respect to carbon dioxide absorption with the aim to use it as advanced absorbent materials in fossil fuel processing. The ionic liquid was synthesized by a one step method, low cost. The thermal and chemical stability of selected ionic liquid has been investigated by DSC, TGA and the structure was verified by $^1H$-NMR spectroscopy. The solubility of carbon dioxide in the methanesulfonate-based ionic liquids were measured using a high-pressure equilibrium apparatus equipped with a variable-volume view cell at 30, 50 and $70^{\circ}C$ and pressure up to 195 bar. The results show that carbon dioxide solubilities of 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate increased with pressure increasing and temperature decreasing, and the carbon dioxide absorption capacity showed 27.6 $CO_2/IL$(g/kg) at $30^{\circ}C$, 13 bar.