• Title/Summary/Keyword: Room temperature synthesis

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Synthesis and Characterization of Linear and Branched Copolymers of Poly(ethylene glycol) and $Poly({\varepsilon}-caprolactone)$ (선형 및 분지 구조의 폴리(에틸렌 글리콜)/폴리카프로락톤 공중합체의 합성 및 특성 검토)

  • Hyun Hoon;Kim Moon-Suk;Khang Gil-Son;Rhee John-M.;Lee Hai-Bang
    • 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.

Synthesis of Methoxy Poly(ethylene glycol)/Polyesters Diblock Copolymers and Evaluation of Micellar Characterization as Drug Carrier (메톡시 폴리(에틸렌 글리콜)/폴리에스테르 블록공중합체의 합성 및 미셀 특성 비교)

  • Hyun, Hoon;Yang, Jae-Chan;Kim, Moon-Suk;Lee, Hai-Bang;Khang, Gil-Son
    • 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.

Synthesis of Aminated Poly(ether imide) for the Preparation of Bi-polar Membranes and Their Application to Hypochlorite Production through the Surface Direct Fluorination (바이폴라막 제조를 위한 폴리에테르이미드의 아민화 합성 및 표면불소화를 통한 차아염소산 생성)

  • Kim, Cheong Seek;Kang, SuYeon;Rhim, Ji Won;Park, Soo-Gil
    • 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.

Cross-Linked PGMA-co-PMMA/DAAB Membranes for Propylene/Nitrogen Separation (프로필렌/질소 분리를 위한 가교 구조의 PGMA-co-PMMA/DAAB 분리막)

  • Kim, Na Un;Park, Byeong Ju;Kim, Jong Hak
    • 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.

Synthesis and Properties of Arylacetylene Resins with Siloxane Units

  • Gao, Fei;Zhang, Lingling;Tang, Lemin;Zhang, Jian;Zhou, Yan;Huang, Farong;Du, Lei
    • 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.

Synthesis and Characterization of Hybrid Nanocomposites of Pd Nanoparticles Containing POSS(Pd-POSS) and Poly(acrylic acid) via Ionic Interactions (실세스키옥세인을 포함한 팔라듐 나노입자와 폴리아크릴산과의 이온결합에 의한 나노복합체 제조 및 특성평가)

  • Jeon, Jong-Hwan;Lim, Jung-Hyurk;Chujo, Yoshiki;Kim, Kyung-Min
    • 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.

A Convenient Radiolabeling of [$^{11}$C](R)-PK11195 Using Loop Method in Automatic Synthesis Module ($^{11}$C 표지 자동합성장치에서 루프법을 이용한 ($^{11}$C)(R)-PK11195의 간편한 합성법)

  • Lee, Hak-Jeong;Jeong, Jae-Min;Lee, Yun-Sang;Kim, Hyung-Woo;Choi, Jae-Yeon;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul
    • 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.

Study on Synthesis of Pyrochlore in Gd-Ti-O and Gd-Zr-O Systems (Gd-Ti-O계 및 Gd-Zr-O 계에서의 파이로클로어 합성연구)

  • ;;;S.V. Yudintsev
    • 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.

A Study on the Reactions of Diamines with 2,5-Dimethoxytetrahydrofuran and 1,3-Acetonedicarboxylic Acid (1,3-Acetonedicarboxylic acid와 2,5-dimethoxytetrahydrofuran에 의한 diamine들의 반응에 관한 연구)

  • Jung Dai-Il;Song Ju-Hyun;Lee Do-Hun;Lee Yong-Gyun;Choi Soon-Kyu;Park Yu-Mi;Hahn Jung-Tai
    • 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.

Synthesis of $[^{51}Cr]Cr(III)$-EDTA Complex and Measurement of Glomerular Filtration Rate br Radioactivity Counting of Head and Neck Region ($[^{51}Cr]Cr(III)$-EDTA 착물 합성 및 $[^{51}Cr]Cr(III)$-EDTA 주사후 두경부 방사능 계측에 의한 사구체 여과율 측정)

  • Yang, Seung-Dae;Lim, Sang-Moo;Chun, Kwon-Soo;Suh, Yong-Sup;Yoon, Yong-Ki;Park, Hyun;Woo, Kwang-Sun;Chung, Wi-Sup;Oh, Ok-Doo;Lee, Jung-Doo
    • The Korean Journal of Nuclear Medicine
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    • v.28 no.3
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    • pp.364-370
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    • 1994
  • The purpose of this study is to evaluate the clinical application of the no carrier added $[^{51}Cr]Cr(III)$-EDTA complexes, produced at Korea Cancer Center Hospital. The $[^{51}Cr]Cr(III)$-EDTA complexes, usefut for measurement of GFR were prepared at room temperature in the presence of bicarbonate catalysts. The radiochemical purity of $[^{51}Cr]Cr(III)$-EDTA was over 99% by paper electrophoresis. The time activity curves were obtained by counting the blood samples from 5 volunteers and counting the head and neck regions with whole body counter after injection of the $^{51}Cr$-EDTA, respectively. After the nonlinear regression, the area under curve was obtained. The plasma clearance of the $^{51}Cr$-EDTA was calculated with injected dose/AUC. The clearance rate calculated with the head and neck counting data was in good agreement with the result from the plasma sample radioactivity at 1-3 hrs after injection. From this result, the counting of head and neck region and the nonlinear regression by 2-compartment model could be applied for the measurement of the clearance rate. Using MIRD system, the absorbed radiation dose was calculated by residence $time{\times}S$. The absorbed whole body radiation dose was negligibly small.

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