• Title/Summary/Keyword: 4-phenylenediamine

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Gas Separation by Polyimide.Silica Composite Membrane (폴리이미드/실리카 복합막에 의한 가스분리)

  • 송병준;김건중;남세종
    • Proceedings of the Membrane Society of Korea Conference
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    • 1997.10a
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    • pp.71-72
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    • 1997
  • 1. 서론 : 공기중의 산소분리용 고분자막은 높은 선택도를 동시에 요구한다. 이 두가지 조건을 만족시키는 소재 개발과 기존의 고분자물질을 수식하는 연구가 진행되고 있다. 고분자막에 대한 수식방법으로는 UV처리, plasma처리등이 있으나, 이들 방법은 선택도는 증가시키나 투과도를 감소시키는 경향이 있다. 기체의 투과저항을 줄이기 위하여 다공성 지지체 위에 박막을 입힌 복합막과 박막의 skin layer와 sub-layer를 갖는 비대칭막은 투과저항을 줄일수 있으나 선택도는 고분자 고유의 80%정도까지 감소되는 것으로 알려졌다. 본 연구의 목적은 고분자 복합막의 투과분리특성을 향상시키기 위한 것으로 지지층의 세공과 표면에 실리카/고분자를 충전, 피복시켜 투과분리특성을 조사하였다. 현재까지의 연구는 낮은 투과계수와 높은 선택도를 갖는 고분자물질이 사용되었으나, 본 연구에서는 폴리이미드로는 폴리이미드 중에서 투과계수가 가장 높다고 알려진 6FDA-p-TeMPD[{(3,3',4,4'-dicarboxyphenyl)hexafluoropropanedianhydride}-{2,3,5,6-Tetra-methyl-1,4-phenylenediamine}] 폴리이미드를 택하였으며 다공성지지체는 aluminum oxide를 사용하였다 . 본 실험에서는 선택도와 투과속도에 주로 영향을 미치는 폴리이미드와 실리카의 양에 대하여 고찰하였다.

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Synthesis of Several New Isoxazole, Imidazo[1, 2-a]pyridine, Imidazo[1, 2-a]pyrimidine, Benzoxadiazine and Benzothiazine Derivatives from Hydroximoyl Halides

  • Abdelhamid, Abdou O.;Abdou, Sadek E.;Mahgoub, Sayed A.
    • Archives of Pharmacal Research
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    • v.15 no.4
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    • pp.317-321
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    • 1992
  • Furoyldroximoyl chloride 3d reacted with 2-aminopyridine, 2-aminopyrimidine. O-aminophenol, O-phenylenediamine and aminothiophenol to afford imidazo [1, 2-a]pyridine 6. imidazo[1, 2-a]pyrimidine 8, benzoxadiazine 10, nitrosobenzopyrizine 13a and nitrosobenzothiazine 13b, respectively. Isoxazoline 18 and pyrrolidino[3, 4-d]isoxazolin-4, 6-dione derivatives 19a and 19b obtained by the reaction of 3 with acrylonitrile and N-arylmaleimide. Hydroximoyl chloride 3 reacted with thiophenol and sodium benzene-sulfinate to yield furylglyoxaloxime 16a and 16b, respectively. Hydroximoyl chloride 3 reacted also with some active methylene compound to give isoxazole derivatives 20-23, respectively.

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Characterization and Preparation of Polyimide Copolymer Membranes by Non-Solvent Induced Phase Separation Method (비용매 유도 상전이법을 이용한 공중합체 폴리이미드 분리막의 제조 및 특성평가)

  • Lee, Jung Moo;Park, Jeong Ho;Kim, Deuk Ju;Lee, Myung Gun;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.4
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    • pp.343-351
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    • 2015
  • In this study, we synthesis polyimide with high gas selectivity using 2,2-bis(3,4-carboxylphenyl) hexafluoropropane, 2,4,6-Trimethyl-1,3-phenylenediamine (DAM) and 4,4-Methylenedianiline (p-MDA), and then the asymmetric membrane was fabricated by non-solvent phase separation method. To confirm the property change of the membrane using different solvent, we measured and compared the viscosity of the polymer solution, cloud point and non-solvent phase separation coefficient. The morphology and gas separation property of membrane prepared by phase separation method was confirmed using Field Emission Scanning Electron Microsope and the single gas permeation measurement apparatus. The single gas ($CH_4$, $N_2$, $O_2$, $CO_2$) permeation property and selectivity value of the membrane prepared with NMP was higher than the membrane prepared with DMAc. We confirmed that the gas selectivity of the membrane increased and the permeation property decreased with increasing of the solvent evaporation time.

Synthesis and Characterization of Molybdenum(Ⅲ) and (Ⅳ) Complexes with N, P, O-Donating Ligands(Ⅲ) (질소, 산소, 인 주개 리간드를 갖는 몰리브덴 (Ⅲ) 및 (Ⅳ) 착물의 합성과 특성 (제 3 보))

  • Kim, Eun Gi;Yu, Eun Yeong;Park, Yu Cheol
    • Journal of the Korean Chemical Society
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    • v.38 no.2
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    • pp.101-107
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    • 1994
  • Some molybdenum(III) and (IV) complexes have been prepared from the reaction of $MoCl_4$·2MeCN with N, P, O-donating ligands and characterized by elemental analysis, infrared and UV-Visible spectroscopy. 3,5-Lutidine, 1,2-phenylenediamine, 8-hydroxyquinoline, 9,10-phenanthrenequinone, triphenylphosphine and 1,2-bis(diphenylphosphino)ethane were chosen as coordinating ligands. Stretching frequencies $\upsilon$ (Mo-Cl) of Mo(IV) appear at higher frequencies than those of Mo(III) complexes due to the increasing oxidation number of metal. $MoCl_4(L)_2$ exhibit one Mo-Cl stretching frequency, whereas Mo$Cl_4$(L^L) exhibit four Mo-Cl stretching frequencies. The number of Mo-Cl stretching frequency suggestes the former complexes have trans($D_{4h}$) and the latter complexes have cis($C_{2v}$) symmetry. Stretching frequency ${\nu}g(C{\equiv}N)$ of acetonitrile in Mo(III) complexes are shifted to about 30 $cm^{-1}$ higher frequency compared with that of a free ligand (2260 $cm^{-1}$). These spectral data indicates that Mo(III) complexes are in the octahedral geometries with the coordinated acetonitrile. Finally each molybdenum(III) and (IV) complexes showed the following formulation; $[MoCl_4(L)_2]$,[Mo$Cl_4$(L^L)], $[MoCl_3(L)_2MeCN]$ and [Mo$Cl_3$(L^L)MeCN].

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Gas Transport Properties of Crosslinked Polyimide Membranes Induced by Aliphatic Diamines with Different Chain Length (사슬 길이가 다른 지방족 디아민으로 가교된 폴리이미드 분리막의 기체 투과 특성)

  • Lee, Hye Rim;Lee, Jung Moo;Nam, Sang Yong
    • Membrane Journal
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    • v.23 no.6
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    • pp.450-459
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    • 2013
  • 2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) based polyimide (PI) were crosslinked with 1,2-Diaminoethane (DAE) and 1,6-Diaminohexane (DAH) to enhance gas transport properties. Fourier transform infrared (FT-IR) studies show that imide groups were converted into amide groups during crosslinking process. Thermogravimetric analysis (TGA) results indicate that the degradation temperature of crosslinked PI membranes decreased after crosslinking. This is due to degradation of alkyl group in crosslinking agent. The d-space of crosslinked PI membranes decreased with increasing crosslinking time. The ideal permeability for $CH_4$, $N_2$, $O_2$, and $CO_2$ decreased after crosslinking and the ideal permeability of crosslinked PI membranes induced by DAH is larger than that by DAE. In contrast, the permselectivity of $CO_2/CH_4$, $CO_2/N_2$ and $O_2/N_2$ increased during crosslinking. For the gas pair of $CO_2/CH_4$, the maximum increment is about 39.5% after 6 minutes of DAE crosslinking. Also, that of $O_2/N_2$ gas pair is about 20.5% after 6 minutes of DAE crosslinking. According to these result, DAE is more suitable for enhanced permselectivity than DAH. On the contrary, DAE is not useful for $CO_2/N_2$ separation due to reduction in $CO_2/N_2$ permselectivity after 3 minutes DAE crosslinking.

Synthesis and Characterization of Tetradentate N2O2 Schiff Base Ligand and its Rare Earth Metal Complexes (사배위 N2O2 Schiff 염기 리간드와 그 희토류 금속착물의 합성 및 특성)

  • Shelke, Vinod A.;Jadhav, Sarika M.;Shankarwar, Sunil G.;Munde, chut S.;Chondhekar, Trimbak K.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.436-443
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    • 2011
  • The solid complexes of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with 4-hydroxy-3-(1-{2-(2,4-dihydroxy-benzylidene)-amino phenylimino}-ethyl)-6-methyl-pyran-2-one ($H_2$L) derived from o-phenylenediamine, 3-acetyl-6-methyl-(2H)pyran,2,4(3H)-dione (dehydroacetic acid or DHA) and 2, 4-dihydroxy benzaldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, FT-IR, $^1H$-NMR, X-ray diffraction, thermal analysis study, and screened for antimicrobial activity. The FT-IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests distorted octahedral geometry for La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) complexes. The X-ray diffraction data suggests monoclinic crystal system for La(III) and Ce(III) and orthorombic crystal system for Pr(III) and Nd(III) complexes. Thermal behavior (TG/DTA) of the complexes was studied and kinetic parameters were determined by Horowitz-Metzger and Coats-Redfern methods. The ligand and its metal complexes were screened for antibacterial activity against Staphylococcus aureus, Escherichia coli, Bacillus Sp. and fungicidal activity against Aspergillus Niger, Trichoderma and Fusarium oxysporum.

Characterization of Gas Permeation Properties of Polyimide Copolymer Membranes (공중합체 폴리이미드를 이용한 기체분리막의 특성평가)

  • Lee, Jung Moo;Lee, Myeong Geon;Kim, Se Jong;Koh, Hyung Chul;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.3
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    • pp.223-230
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    • 2015
  • We synthesized novel polyimides with high gas permeability and selectivity for application of gas separation membrane. 2,2-bis(3,4-carboxylphenyl) hexafluoropropane dianhydride (6FDA) and two kinds of amines with high permeability and solubility were used to prepare the novel polymide. 2,4,6-Trimethyl-1,3-phenylenediamine (DAM) was used to improve gas permeability and 4,4-Methylenedianiline was used to improve the gas selectivity respectively. The polyimide copolymers were synthesized by commercial chemical imidization method using Triethylamine and Acetic anhydride and their average molecular weights were over 100,000 g/mol. The glass temperature (Tg) and the thermal degradation temperature were characterized using differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The synthesized copolymers showed high Tg over $300^{\circ}C$ and high thermal degradation temperature over $500^{\circ}C$. The gas permeation properties were measured by time-lag equipment. Although general polyimides showed very low gas permeability, synthesized polyimide copolymer showed high $O_2$ permeability of 10.1 barrer with high $O_2/N_2$ selectivity around 5.3. From this result, we confirm that these membranes have possibility to apply to gas separation membrane.

Characterization of Gas Permeation Properties of Polyimide Copolymer Membranes for OBIGGS (OBIGGS용 공중합체 폴리이미드를 이용한 기체분리막의 투과 특성평가)

  • Lee, Jung Moo;Lee, Myung Gun;Kim, Deuk Ju;Nam, Sang Yong
    • Membrane Journal
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    • v.24 no.4
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    • pp.325-331
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    • 2014
  • We synthesized novel polyimides with high gas permeability and selectivity for application of on board inert gas generation system (OBIGGS). 2,2-bis(3,4-carboxylphenyl) hexafluoropropane dianhydride (6FDA) and two kinds of amines with high permeability and solubility were used to prepare the novel polymide. 2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) was used to improve gas permeability and various kinds of diamines were used to improve the gas selectivity respectively. The polyimide copolymers were synthesized by commercial chemical imidization method and their average molecular weights were over 100,000g/mol. The glass temperature ($T_g$) and the thermal degradation temperature were characterized using differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The synthesized copolymers showed high $T_g$ over $300^{\circ}C$ and high thermal degradation temperature over $500^{\circ}C$. The gas permeation properties were measured by time-lag equipment. Although general polyimides showed very low gas permeability, synthesized polyimide copolymer showed high $O_2$ permeability of 36.21 barrer with high $O_2/N_2$ selectivity around 4.1. From this result, we confirm that these membranes have possibility to apply to OBIGGS.

Antimutagenic Potential of Phellinus igniarius

  • Shon, Yun-Hee;Lee, Jae-Sung;Lee, Hang-Woo;Nam, Kyung-Soo
    • Journal of Microbiology and Biotechnology
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    • v.9 no.4
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    • pp.525-528
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    • 1999
  • Mutagenic activities of extracts from the filtrate of the cultured broth (PI-I), mycelia (pI-II), and the fruiting bodies (PI-III) of Phellinus igniarius were examined by Ames/Salmonella tests. No mutagenic activity was found in Salmonella typhimurium strains TA98 and TA100, either with or without S9 activation. In contrast, PI-I, PI-II, and PI-III showed inhibitory effects on the mutagenic activities by the directly-acting mutagens, 4-nitro-ο-phenylenediamine(NPD) and sodium azide ($NaN_3$), and also by the indirectly-acting mutagens, 2-aminofluorene (2-AF) and benzo[a]pyrene (B[a]P). These results suggest that P. igniarius possesses some antimutagenic activity and may contain some chemopreventive agents.

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Synthesis and Characterization of Some Transition Metal Complexes of Unsymmetrical Tetradentate Schiff Base Ligand (비대칭 Tetradentate Schiff 염기 리간드의 전이금속 착물에 대한 합성 및 특성)

  • Munde, A. S.;Jagdale, A. N.;Jadhav, S. M.;Chondhekar, T. K.
    • Journal of the Korean Chemical Society
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    • v.53 no.4
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    • pp.407-414
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    • 2009
  • The solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with 4-hydroxy-3-(1-{2-(2-hydroxybenzylidene)- amino phenylimino}-ethyl)-6-methy-pyran-2-one (H2L) derived from o-phenylenediamine, 3-acetyl- 6-methyl-(2H) pyran, 2,4 (3H)-dione (dehydroacetic acid or DHA) and salicylic aldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, IR, $^1H$-NMR spectra, X-ray diffraction, thermal analysis, and screened for antimicrobial activity. The IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests square planar geometry for Cu(II) and Ni(II) complexes and octahedral geometry for Co(II), Mn(II) and Fe(III) complexes. The x-ray differaction data suggests orthorhombic crystal system for Cu(II) complex, monoclinic crystal system for Ni(II), Co(II) and Fe(III) and tetragonal crystal system for Mn(II) complex. Thermal behaviour (TG/DTA) of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus Niger and Trichoderma.