• Title/Summary/Keyword: polymer synthesis and characterization

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Anion-Dependent Exocyclic Mercury(II) Coordination Polymers of Bis-dithiamacrocycle

  • Siewe, Arlette Deukam;Kim, Seulgi;Choi, Kyu Seong;Lee, Shim Sung
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3459-3464
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    • 2014
  • Synthesis and structural characterization of mercury(II) halides and perchlorate complexes (1-4) of bis-$OS_2$-macrocycle (L) are reported. L reacts with mercury(II) chloride and bromide to yield an isostructural 2D coordination polymers with type $[Hg(L)X_2]_n$ (1: X = Cl and 2: X = Br). In 1, each Hg atom which lies outside the cavity is six-coordinate with a distorted octahedral geometry, being bound to four adjacent ligands via monodentate Hg-S bonds and two remaining sites are occupied by two terminal chlorido ligands to form a fishnet-like 2D structure. When reacting with mercury(II) iodide, L afforded a 1D coordination polymer $\{[Hg_2(L)I_4]{\cdot}CHCl_3\}_n$ (3) in which each exocyclic Hg atom is four-coordinate, being bound to two sulfur donors from different ligands doubly bridging the ligand molecules in a head-to-tail mode. The coordination sphere in 3 is completed by two iodo terminal ligands, adopting a distorted tetrahedral geometry. On reacting with mercury(II) perchlorate, L forms solvent-coordinated 1D coordination polymer $\{[Hg_2(L)(DMF)_6](ClO_4)_4{\cdot}2DMF\}_n$ (4) instead of the anion-coordination. In 4, the Hg atom is five-coordinate, being bound to two sulfur donors from two different ligands doubly bridging the ligand molecules in a side-by-side mode to form a ribbon-like 1D structure. The three remaining coordination sites in 4 are completed by three DMF molecules in a monodentate manner. Consequently, the different structures and connectivity patterns for the observed exocyclic coordination polymers depending on the anions used are influenced not only by the coordination ability of the anions but also by anion sizes.

Synthesis and Characterization of Catechol-Containing Biomimetic Mucoadhesive Polymers (카테콜 함유 생체모방 점막접착형 고분자의 합성 및 특성 연구)

  • Park, Dong Jin;Lee, Sang Jin;Lee, Sang Cheon
    • Polymer(Korea)
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    • v.37 no.5
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    • pp.625-631
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    • 2013
  • Mucoadhesive property is the major function as an adhesive for medical devices, and therefore, these days many researches have conducted to develop polymers having this property. Recently, biomimetic technology has been used for developing mucoadhesive polymers. Among many technologies, mussel-inspired approaches have received noticeable attention because of its thread's strong adhesive characteristics. In this study, we synthesized mucoadhesive biomimetic polymers employing catechol structures which are abundant in mussel adhesive proteins, and their structures and molecular weights were characterized by using nuclear magnetic resonance spectroscopy and gel permeation chromatography. To evaluate in vitro mucoadhesive strength, the sheet type of the small intestinal porcine submucosa was prepared. Compared to commercial fibrin glue adhesives, catechol-containing mucoadhesive polymers showed enhanced adhesive strength. The study of adhesive strength with considering diverse factors, such as temperature, pressure, and oxidant amount indicated that mussel-inspired mucoadhesive polymer could be a promising candidate for an adhesive in various biomedical applications.

Synthesis and Characterization of Allyl Ester Resin-Layered Silicate Nanocomposite (알릴 에스터 수지-층상 실리케이트 나노복합재료의 합성과 특성)

  • 팽세웅;김장엽;허완수;조길원;이상원
    • Polymer(Korea)
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    • v.28 no.2
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    • pp.177-184
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    • 2004
  • Polymer-clay nanocomposite containing the low amounts of clay shows improved physical, mechanical properties. In this study, allyl ester prepolymer was synthesised by reactions of the diallyl terephthalate monomers and the 1,3-butanediol monomers. Nanocomposites of allyl ester prepolymer and the two kinds of the organically layered silicate were prepared by using the intercalation method as well as the in-situ polymerization method using. By varying the amount of clay content, curing conditions, and feeding conditions. the nanocomposite was studied using X-ray diffraction. From XRD results, allyl ester-Cloisite 30 B nanocomposite made by the in-situ polymerization method shows better exfoliation behavior compared with the intercalation method. It can be said that the transesterification reaction between functional groups (-OH) of intercalant and monomers results in the increased gallery distance. Also mechanical and thermal properties indicate that the dispersity of clay is an important factor for improving physical properties of the nanocomposite.

Synthesis and Properties of PEGMA/Na-MMT with Acrylic Monomer by Free-Radical Polymerization (Free Radical 중합에 의한 PEGMA/Na-MMT와 아크릴단량체의 합성 및 물성)

  • Joo, Hong Hee;Park, Chan Young;Kim, Tae Kyoon;Chun, Jae Hwan;Lee, Won Kee;Oh, Sang Taek
    • Journal of Adhesion and Interface
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    • v.11 no.3
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    • pp.106-111
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    • 2010
  • Na-MMT intercalated with PEGMA macromer was prepared using an EtAc/acetone mixture (1/1 by volume) as a solvent. PEGMA/(Na-MMT)-co-MMA/MA nanocomposites was synthesized by copolymerizing intercalated compound with MMA and MA, and then characterization was performed. The results of X-ray diffraction (XRD) showed that in the case of Na-MMT intercalated with PEGMA macromer the d-spacings of silicate of Na-MMT increased with increasing of Na-MMT loading. As the Na-MMT loading increases Tg showed increasing trend through the DSC measurement. TGA result showed that thermal stability of PEGMA/(Na-MMT)-co-MMA/MA nanocomposites improved a little more than the pure PEGMA-co-MMA/MA.

Synthesis and Characterization of Comb-Type Grafted Polymer Hydrogels with Low Temperature Sensitivity (저온 감열 특성을 가지는 Comb-Type Grafted Polymer Hydrogels의 합성 및 특성평가)

  • Taek Kyu Jung;Sung Soo Kim;Byung Cheol Shin
    • Journal of the Korean Chemical Society
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    • v.47 no.1
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    • pp.59-66
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    • 2003
  • The comb-type grafted polymer hydrogels, which composed of N-isopropylacrylamide monomer and oligo(N-isopropylacrylamide-co-tert-butylacrylamide) [oligo(NIPAAm-co-t-BAM)], were synthesized by redox polymerization in 5~10% methanol aqueous solution using ammonium peroxodisulfate (APS) at 4 oC for 24h. The lower critical solution temperatures (LCSTs) of the comb-type grafted hydrogels were decreased with increase of t-BAM content in the grafted copolymer. We observed the effect of crosslinker and concentration of oligo(NIPAAm-co-t-BAM) on the shrinking/swelling ratio of hydrogels. Changes of shrinking/swelling ratio were decreased with increase of concentration of crosslinker. The increase of grafted oligo(NIPAAm-co-t-BAM) in the hydrogel shows an fast changes of shrinking/ swelling rate. The comb-type grafted hydrogels are expected to be valuable for the sensing materials of time-temperature labels(TTLs).

Synthesis and Characterization of Photosensitive Polyimides Containing Alicyclic Structure (지방족고리 구조를 함유하는 감광성 폴리이미드 수지의 합성 및 특성 평가)

  • 심종천;최성묵;심현보;권수한;이미혜
    • Polymer(Korea)
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    • v.28 no.6
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    • pp.494-501
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    • 2004
  • A new alkali developable photosensitive poly(amic acid) (PAA-0) with transmittance at 400 nm was synthesized from cyclobutane-1,2,3,4-tetracarboxylic dianhydride, 2-(methacryloyloxy)ethyl-3,5-diamino-benzoate and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyl disiloxane in N-methyl-2-pyrrolidinone. Photosensitivity of the PAA-0 was investigated at 365-400 nm in the presence of a photoinitiator using a high pressure mercury lamp. The photo-cured poly(amic acid) was insoluble toward aqueous 2.38 wt% tetramethylammonium hydroxide solution. Negative pattern of the PAA-0 with 25 ${\mu}{\textrm}{m}$ resolution was obtained by developing with 2.38 wt% tetramethylammonium hydroxide solution after exposure of 600 mJ/$\textrm{cm}^2$ in the presence of 2,2-dimethoxy-2-phenyl-acetophenone as a photoinitiator. The patterned poly(amic acid) was converted to polyimide by thermal curing at 25$0^{\circ}C$ for 50 min, which showed chemical resistance against photoresist stripper as well as good transmittance at 400 nm.

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.

Preparation and Characterization of Random Copolymer Electrolyte Membranes Containing PFCB (Perfluorocyclobutane) Group (PFCB (Perfluorocyclobutane) Group을 포함한 랜덤 공중합체 고분자 전해질 막 제조 및 특성연구)

  • Kim Jeong-Hoon;Kim Dong-Jin;Chang Bong-Jun;Lee Soo-Bok;Joo Hyeok-Jong
    • Membrane Journal
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    • v.16 no.3
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    • pp.221-229
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    • 2006
  • This study is about the preparation and characterization of sulfonated random copolymer membranes containing perfluorocyclobutane (PFCB), fluorenyl, and sulfonyl units. The polymers were prepared through three synthetic steps, that is, the synthesis of a trofluorovinylether-terminated monomer, its thermal polymerization, and post-sulfonation using chlorosulfonic acid. A series of sulfonated random copolymers with different ion exchange capacity (IEC) were prepared by changing contents of fluorenyl uints in polymers with fixed molar ratio of chlorosulfonic acid during the post-sulfonation reaction. All the synthesized compounds were characterized by FT-lR, $^1H-NMR$, $^{19}F-NMR$, and Mass spectroscopy. As the content of sulfonated fluorenyl units increased, the IEC, water uptake, and ion conductivity of the sulfonated random copolymer membranes increased. The sulfonated random copolymer S-1 and S-2 showed higher values of ion conductivity than the Nafion-115 in a wide range of temperatures ($25{\sim}80^{\circ}C$).

Synthesis of Crosslinkable m-Aramid Ionomer Containing Sulfonated Ether Sulfone and Their Characterization for PEMFC Membrane (Sulfonated Ether Sulfone을 포함한 Crosslinkable m-Aramid계 Ionomer의 합성과 연료전지 막으로의 이용)

  • Jung, Hyun-Jin;Kim, Jung-Min;Cho, Chang-Gi
    • Polymer(Korea)
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    • v.34 no.3
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    • pp.202-209
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    • 2010
  • Aromatic copolyamides were prepared and their applicability to proton exchange membrane wasstudied. The copolymer contains thermally stable and mechanically strong poly(m-phenylene isophthalamide) segments, and easily processable and good film forming polysulfone segments. For the copolymer, amineterminated sulfonated ether sulfone monomer, m-phenylene diamine, and isophthaloyl chloride were reacted, and the obtained copolymer was transformed into crosslinkable prepolymer by the reaction with acryloyl chloride. The prepolymer was thermally cured and converted into proton exchange membranes for fuel cell application. Each reaction step and the molecular characteristics of precursor copolymers were monitored and confirmed by $^1H$ NMR, FTIR, and titration. The performance of the membranes was measured in terms of water uptake, proton conductivity, and thermal stability. The water uptake, ion exchange capacity (IEC), and proton conductivity of the membranes increased with the increase of sulfonated ether sulfone segment content. Membrane containing 30 mol% sulfonic acid sulfone segment showed 1.57 meq/g IEC value. Water uptake was limited less than 44 wt% and the highest proton conductivity up to $3.93{\times}10^{-2}S/cm$ ($25^{\circ}C$, RH= 100%) was observed.

Preparation of Dual-functionalized Polymeric Membrane Electrolyte and Ni, Co-based Nanowire/MOF Array on Carbon Cloth for High-performance Supercapacitor (이중 기능 고분자 전해질 막의 제조 및 탄소 섬유에 니켈, 코발트 기반의 나노와이어/MOF 배열을 통한 고성능 슈퍼커패시터 연구)

  • Hye Jeong Son;Bong Seok Kim;Ji Min Kwon;Yu Bin Kang;Chang Soo Lee
    • Membrane Journal
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    • v.33 no.4
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    • pp.211-221
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    • 2023
  • This study presents a comprehensive study on the synthesis and characterization of PVI-PGMA/LiTFSI polymeric membrane electrolytes and CxNy-C flexible electrodes for energy storage applications. The dual-functional PVI-PGMA copolymer exhibited excellent ionic conductivity, with the PVI-PGMA73/LiTFSI200 membrane electrolyte achieving the highest conductivity of 1.0 × 10-3 S cm-1. The electrochemical performance of the CxNy-C electrodes was systematically investigated, with C3N2-C demonstrating superior performance, achieving the highest specific capacitance of 958 F g-1 and lowest charge transfer resistance (Rct) due to its highly interconnected hybrid structure comprising nanowires and polyhedrons, along with binary Co/Ni oxides, which provided abundant redox-active sites and facilitated ion diffusion. The presence of a graphitic carbon shell further contributed to the enhanced electrochemical stability during charge-discharge cycles. These results highlight the potential of PVI-PGMA/LiTFSI polymeric membrane electrolytes and CxNy-C electrodes for advanced energy storage devices, such as supercapacitors and lithium-ion batteries, paving the way for further advancements in sustainable and high-performance energy storage technologies.