• Membrane Journal
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• v.25 no.3
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• pp.231-238
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• 2015

Co-polyimide membranes were prepared by two-step polymerization using semi-alicyclic 5-(2,5-dioxotetrahydrofuryl)-3-methyl-cyclohexene-1,2-dicarboxylic anhydride (DOCDA) with five diamines such as 2,5-dimethyl-1,4-phenylene diamine (2M), 2,4,6-trimethyl-1,3-phenylene diamine (3M), 1,5-naphthalene diamine (NDA), 4,4-diaminodiphenyl methane (MDA), 4,4'-diaminodiphenyl ether (ODA). Synthesized co-polyimides were characterized by FT-IR, viscosity, solubility, DSC, TGA and gas permeation properties, compared with 6FDA-based co-polyimides. All co-polyimides had the intrinsic viscosity of 0.32~0.58 and excellent solubility in various solvents. DOCDA-based co-polyimides had thermal stability over $400^{\circ}C$ although those were lower than 6FDA-based co-polyimides. Gas permeabilities of the copolyimide membranes were measured for $CO_2$ and $CH_4$ at room temperature and presented the trade-off relationship.

• Polymer(Korea)
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• v.30 no.2
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• pp.146-151
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• 2006

Linear and branched copolymers consisting of poly(ethylene glycol) (PEG) and $Poly({\varepsilon}-caprolactone)$ (PCL) were prepared to compare the characterization of star-shaped copolymers with various molecular architecture. Linear and branched PEG-PCL (1-arm, 2-arm, 4-arm, and 8-arm) copolymers were synthesized by the ring-opening polymerization of ${\varepsilon}-caprolactone$ in the presence of HCl $Et_2O$ as a monomer activator at room temperature. The synthesized copolymers were characterized with $^1H-NMR$, GPC, DSC, and XRD. As a result of the DSC and XRD, each copolymers showed different thermal properties and crystallinity according to the number of ms. The micellar characterization of linear and branched copolymers in an aqueous phase was carried out by using NMR, dynamic light scattering, AM, and fluorescence techniques. The critical micelle concentration (CMC) and diameters of micelles depended on the number of arms. Most micelles exhibited a spherical shape in AFM. In this study, we characterized star-shaped PEG-PCL copolymers and investigated their molecular architecture effect on the various properties. Furthermore, we confirmed that the micelles termed with linear and branched PEG-PCL copolymers have possibility as a potential hydrophobic drug delivery vehicle.

• Polymer(Korea)
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• v.30 no.6
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• pp.464-470
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• 2006

Diblock copolymers consisting of methoxy Poly (ethylene glycol) (MPEG) and poly (${\epsilon}-ca$ prolactone) (PCL), poly(${\delta}-valerolactone$) (PVL), poly(L-lactide) (PLLA), or poly(L-lactide-co-glycolide) (PLGA) were prepared to compare the characterization of diblock copolymers as a drug carrier. MPEG-PCL, MPEG-PVL, MPEG-PLLA, and MPEG-PLGA diblock copolymers were synthesized by the ring-opening polymerization of ${\epsilon}$-caprolactone or ${\delta}$-valerolactone in the presence of $HCl{\cdot}Et_2O$ as a monomer activator at room temperature and by the ring-opening polymerization of L-lactide or a mixture of L-lactide and glycolide in the presence of stannous octoate at $130^{\circ}C$, respectively. The synthesized diblock copolymers were characterized with $^1H-NMR$, GPC, DSC, and XRD. The micellar characterization of MPEG-polyester diblock copolymers in an aqueous phase was carried out by using NMR, dynamic light scattering, AFM, and fluorescence techniques. Most micelles exhibited a spherical shape in AFM. Thus, ore confirmed that the micelles formed with MPEG-polyester diblock copolymers have possibility as a potential hydrophobic drug delivery vehicle because a hydrophobic drug could be preferentially distributed in the micelle core.

• Polymer(Korea)
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• v.39 no.2
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• pp.338-345
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• 2015

Poly(phenylene oxide) (PPO) and polyether imide (PEI) were sulfonated and aminated to create sulfonated poly(phenylene oxide) (SPPO) and aminated polyether imide (APEI), respectively. Characterization of the SPPO and APEI were performed via measurements of FTIR, thermogravimetry (TGA), swelling degree, ion exchange capacity (IEC), and ion conductivity. Next, the surfaces of these membranes were modified by surface fluorination at room temperature. The surface fluorinated SPPO and APEI membranes underwent characterization again for the mentioned measurements to determine any differences. The 3 types of bi-polar membranes were prepared by varying the IEC of the APEI at a fixed SPPO IEC value, which were applied to the low and high NaCl concentration of feed solution at the different current density, respectively. The hypochlorite concentration derived from the surface fluorinated membranes was dependent on the IEC of the APEI and ranged from 491 to 692 ppm at $80mA/m^2$. At low current density of $5mA/m^2$, the hypochlorite concentrations ranged from 18 to 28 ppm for the 4 hrs surface fluorinated membranes and their durability increased greatly.

• Membrane Journal
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• v.30 no.4
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• pp.252-259
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• 2020

Olefins are industrially important materials used for the synthesis of various petrochemicals. During the polymerization process, unreacted olefin monomers are discharged together with a large amount of nitrogen. For economic benefits, these olefin gases should be efficiently separated from nitrogen. In this study, a poly(glycidyl methacrylate-co-methyl methacrylate) (PGM) comb-like copolymer was synthesized and 4,4'-diaminoazobenzene (DAAB) was introduced to the copolymer to prepare a cross-linked membrane for C₃H₆/N₂ separation. PGM and DAAB were readily reacted at room temperature through an epoxide-amine reaction without additional thermal treatment. PGM-based membrane, which is a glassy polymer, showed a faster permeation of N₂ compared to C₃H₆. The pristine PGM membrane exhibited the N₂ permeability of 0.12 barrer and the high N₂/C₃H₆ selectivity of 32.4. As DAAB was introduced as a cross-linker, the thermal stability of the membrane was significantly improved, which was confirmed by TGA result. The N₂/C₃H₆ selectivity was decreased at 1 wt% of DAAB content, but the N₂ permeability increased by approximately 4.7 times. We analyzed N₂/C₃H₆ gas separation properties through a glassy polymer-based membrane, which has not been widely studied. Also, we proposed that thermal stability of the membrane can be greatly improved by the cross-linking method.

• Bulletin of the Korean Chemical Society
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• v.31 no.4
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• pp.976-980
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• 2010

A series of arylacetylene resins with siloxane units were synthesized by the condensation reactions of m-diethynylbenzene magnesium reagents with various $\alpha,\omega$-bis(chloro)dimethylsiloxanes. These resins are liquids and are miscible with common organic solvents at room temperature. The structures of the resins were characterized by FT-IR, $^1H$ NMR, $^{13}C$ NMR, $^{29}Si$ NMR, and gel permeation chromatography (GPC). The thermal behaviors of the resins were examined with differential scanning calorimetry (DSC). These resins have good processability. They can be thermally cross-linked through the ethynyl groups to produce cured resins. The thermal and thermooxidative stabilities of the cured resins were studied by thermogravimetric analysis (TGA). The cured resins possess high thermal and thermooxidative stability. Their decomposition occurs at above $500^{\circ}C$ in both $N_2$ and air. With increasing the length of siloxane units in the resins, the thermal stability of the cured resins decreases in $N_2$. When the cured resins were sintered above $1450^{\circ}C$ under argon, hard and glassy SiOC ceramics were obtained. These SiOC ceramics have the decomposition temperatures at 5% weight loss above $800^{\circ}C$ in air.

• Polymer(Korea)
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• v.33 no.6
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• pp.615-619
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• 2009

Pd-POSS nanoparticles were produced from the reaction of palladium (II) acetate and octa(3-aminopropyl)octasilsesquioxane octahydrochloride (POSS-${NH_3}^+$) in methanol at room temperature. Pd-POSS nanoparticles with a mean diameter of 60-80 nm were the highly ordered spherical aggregates. In contrast, Pd nanoparticles with a size of 4.0 nm were obtained when POSS-${NH_3}^+$ was not introduced. Pd-POSS/PAA nanocomposites of Pd-POSS nanoparticles and poly(acrylic acid) (PAA) were fabricated by utilizing ionic interactions between positively charged Pd-POSS nanoparticles and negatively charged carboxylate groups of PAA. PAA was used as a cross-linker for the preparation of hybrid nanocomposites with the controlled organized structures of Pd-POSS nanoparticles. That is, the self-organization of Pd-POSS nanoparticles was formed into the shape of continuous lines by using PAA as a cross-linker. The composition, structure, surface morphology, and thermal stability of the Pd-POSS/PAA nanocomposites were studied by FE-SEM, AFM, TEM, FT-IR, and TGA.

• Nuclear Medicine and Molecular Imaging
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• v.43 no.4
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• pp.337-343
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• 2009

Purpose: ((R)-1-(2-chlorophenyl)-N-1-[$^{11}$C]methyl-N(1-propyl)-3-isoquinoline carboxamide ((R)-PK11195) is a specific ligand for the peripheral type benzodiazepine receptor and a marker of activated microglia, used to measure inflammation in neurologic disorders. We report here that a direct and simple radiosynthesis of [$^{11}$C](R)-PK11195 in mild condition using NaH suspension in DMF and one-step loop method. Materials and Methods: (R)-N-Desmethyl-PK11195 (1 mg) in DMSO (0.1 mL) and NaH suspension in DMF (0.1 mL) were injected into a semi-prep HPLC loop. [$^{11}$C]methyl iodide was passed through HPLC loop at room temperature. Purification was performed using semi-preparative HPLC. Aliquots eluted at 11.3 min were collected and analyzed by analytical HPLC and mass spectrometer. Results: The labeling efficiency of [$^{11}$C](R)-PK11195 was 71.8$\pm$8.5%. The specific activity was 11.8:$\pm$6.4 GBq/$\mu$mol and radiochemical purity was higher than 99.2%. The mass spectrum of the product eluted at 11.3 min showed m/z peaks at 353.1 (M+1), indicating the mass and structure of (R)-PK11195. Conclusion: By the one-step loop method with the [$^{11}$C]CH3l automated synthesis module, [$^{11}C$](R)-PK11195 could be easily prepared in high radiochemical yield using NaH suspension in DMF.

• Economic and Environmental Geology
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• v.37 no.3
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• pp.303-309
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• 2004

Pyrochlores were known as promising materials for the immobilization of radioactive actinide. Accordingly, we synthesized pyrochlores with Gd$_2$Ti$_2$$O_7$ and Gd$_2$Zr$_2$$O_7$compositions by sintering method, and studied its properties and phase relations in Gd-Ti-O and Gd-Zr-O system. The mixed powders were pressed into pellets under 200-400 kgf/cm$^2$ at room temperature. and then sintered at 1000-1$600^{\circ}C$ for 0.5-40 hours. The synthesized samples were analyzed and were identified with XRD and SEM/EDS analyses. The optimal synthetic conditions of pyrochlores with Gd$_2$Ti$_2$$O_7$composition were at 140$0^{\circ}C$/0.5hrs, 130$0^{\circ}C$/3hrs and 120$0^{\circ}C$/20hrs. Its chemical composition was $Gd_{2.0-2.1}$$Ti_{1.9-2.0}$$O_7$ and similar to the stoichiometric composition without any relationship in temperature and atmosphere. The optimal synthetic conditions of pyrochlores with $Gd_{2}$$Zr_{2}$$O_7$composition were at 155$0^{\circ}C$/40hrs and 1$600^{\circ}C$/30hrs. The compositions of pyrochlore synthesized from these optimal conditions were irregular with $Gd_{1.5-2.4}$$Zr_{1.7-2.4}$$O_7$. Such heterogeneity indicates that the reaction rate of pyrochlore with Gd$_2$Zr$_2$$O_7$composition is very low, and then its equilibrium state could not be attained even for 40 hours which was the longest sintering time in this research.

• Journal of Life Science
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• v.16 no.2 s.75
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• pp.206-212
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• 2006

In order to synthesize novel anticonvulsants, we researched that the reactions of diamines with 2,5-dimethoxytetrahydrofuran and 1,3-acetonedicarboxylic acid. The reaction of ethylenediamine with 2,5-dimethoxytetrahydrofuran and 1,3-acetonedicarboxylic acid afforded 8-(2-pyrrol-1-yl-ethyl)-8-aza-bicyclo[3,2,1]octan-3-one (yield; 5.0%) and 1,2-di-(8-aza-bicyclo[3,2,1]octan3-onyl)ethane (yield; 17.0%). In case of 1,3-diaminopropane, 8-(3-pyrrol-1-yl-propyl)-8-aza-bicyclo[3,2,1]octan-3-one(yield; 6.0%) and 1,3-di-(8-aza-bicyclo[3,2,1]octan-3-onyl)propane (yield; 21.0%) were obtained. In case of 1,8-diaminooctane, 8-(8-pyrrol-1-yl-octyl)-8-aza-bicyclo-[3,2,1]octan-3-one (yield; 2.6 %) and 1,8-di-(8-aza-bicyclo[3,2,1]octan-3-onyl)octane (yield; 24.9%) were obtained. In diaminobenzene reactions, synthetic yields of 8-aza-bicyclo-[3,2,1]octan-3-one derivatives were higher than those of pyrrole derivatives because re actions were done under room temperature. The longer the carbon chain of diaminoalkane is, the more reactive N atom is due to more electron donating effect, and the less steric hindrance around the carbon gave the higher chemical yields. The reaction of p-phenylenediamine as a diaminobenzene with 2,5-dimethoxyte-trahydrofuran and 1,3-acetonedicarboxylic acid produced p-dipyrrolylbenzene (yield; 4.0%), 8-(4-pyrrol-1-yl-phenyl)-8-aza-bicyclo[3,2,1]octan-3-one (yield; 12.0%), and 1,4-di-(8-aza-bicyclo[3,2,1]octan-3-onyl)benzene (yield; 59.0%). In case of m-phenylenediamine, 8-(3-pyrrol-1-yl-phenyl)-8-aza-bicyclo[3,2,1]octan-3-one(yield; 2.0%) and 1,3-di-(8-aza-bicyclo[3,2,1]octan-3-onyl)benzene (yield ; 28.0%) were obtained. But, synthesis of 1,2-di-(8-aza-bicyclo[3,2,l]octan-3-onyl)benzene by treatment of o-phenylenediamine was not successful, presumably due to the steric hindrance of 8-aza-bicyclo-[3,2,1]octan-3-one rings.