• 제목/요약/키워드: Atom Transfer Radical Polymerization

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곁가지에 다양한 길이의 알코올 그룹을 지닌 고분자들의 저임계 용액온도 민감성 제어 (Precise Control of Thermoresponsive Properties of Polymers with Hydroxy Groups in the Side Chains)

  • 이형일
    • 폴리머
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    • 제39권1호
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    • pp.165-168
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    • 2015
  • 하이드록시 그룹을 지닌 온도민감형 고분자들이 원자전이라디칼중합법(ATRP)과 클릭반응(click reaction)에 의해 합성되어졌다. 고분자들의 분자량과 분자량 분포도는 gel permeation chromatography(GPC)에 의하여 얻어졌고, 고분자들의 분자량은 잘 제어되었으며 분자량 분포도도 낮게 유지되었다. 클릭반응의 효율은 $^1H$ NMR spectroscopy에 의해 얻어졌으며, 높은 효율을 나타내었다. 고분자 사슬 곁가지의 아민 그룹의 종류와, 치환된 알코올 그룹의 종류에 따라 저임계 용액 온도(LCST)의 제어가 가능했다.

수소이온 전도성 가지형 공중합체 전해질막 제조 및 분석 (Synthesis and Characterization of Proton Conducting Graft Copolymer Membranes)

  • 노동규;고종관;서진아;김종학
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2010년도 춘계학술대회 초록집
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    • pp.126.2-126.2
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    • 2010
  • The "grafting from" technology to prepare the well-defined microphase-separated structure of polymer using atom transfer radical polymerization (ATRP) will be introduced in this presentation. Various amphiphilic comb copolymers were synthesized through this approach using poly (vinylidene fluoride) (PVDF), poly (vinylidene fluoride-co-chlorotrifluoroethylene) (P(VDF-co-CTFE) and poly(vinyl chloride) (PVC) as a macroinitiator. Hydrophilic side chains such as poly (styrene sulfonic acid) (PSSA) or poly (sulfopropyl methacrylate) (PSPMA) were grafted from the mains chains using direct initiation of the chlorine atoms. The structure of mass transport channels has been controlled and fixed by crosslinking the hydrophobic domains, which also provides the greater mechanical properties of membranes. Successful synthesis and microphase-separated structure of the polymer were confirmed by $^1H$ NMR, FT-IR spectroscopy and TEM. The grafted/crosslinked membranes exhibited good mechanical properties (400 MPa of Young's modulus) and high thermal stability (up to $300^{\circ}C$), as determined by a universal testing machine (UTM) and TGA, respectively.

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무가습 가교 가지형 공중합체 전해질 막의 제조 (Preparation of Anhydrous Crosslinked Graft Copolymer Electrolyte Membrane)

  • 노동규;고주환;박정태;서진아;김종학
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2009년도 춘계학술대회 논문집
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    • pp.270-273
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    • 2009
  • A comb-like copolymer consisting of a poly(vinylidene fluoride-co-chlorotrifluoro-ethylene) backbone and poly(hydroxy ethyl acrylate) side chains, i.e. P(VDF-co-CTFE)-g-PHEA, was synthesized through atom transfer radical polymerization (ATRP) using CTFE units as a macroinitiator. Successful synthesis and a microphase-separated structure of the copolymer were confirmed by proton nuclear magnetic resonance (1H-NMR), FT-IR spectroscopy, and transmission electron microscopy (TEM). This comb-like polymer was crosslinked with 4,5-imidazole dicarboxylic acid (IDA) via the esterification of the -OH groups of PHEA and the -COOH groups of IDA. Upon doping with phosphoric acid ($H_3PO_4$) to form imidazole-$H_3PO_4$ complexes, the proton conductivity of the membranes continuously increased with increasing $H_3PO_4$ content. A maximum proton conductivity of 0.015 S/cm was achieved at $120^{\circ}C$ under anhydrous conditions. In addition, these P(VDF-co-CTFE)-g-PHEA/IDA/$H_3PO_4$ membranes exhibited good mechanical properties (765 MPa of Young's modulus), and high thermal stability up to $250^{\circ}C$, as determined by a universal testing machine (UTM) and thermal gravimetric analysis (TGA), respectively.

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Preparation of Al@Fe2O3 Core-Shell Composites Using Amphiphilic Graft Copolymer Template

  • Patel, Rajkumar;Kim, Sang Jin;Kim, Jin Kyu;Park, Jung Su;Kim, Jong Hak
    • Korean Chemical Engineering Research
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    • 제52권2호
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    • pp.209-213
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    • 2014
  • A graft copolymer of poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) was synthesized via atom transfer radical polymerization (ATRP) and used as a structure-directing agent to prepare $Al@Fe_2O_3$ core-shell nanocomposites through a sol-gel process. The amphiphilic property of PVC-g-POEM allows for good dispersion of Al particles and leads to specific interaction with iron ethoxide, a precursor of $Fe_2O_3$. Secondary bonding interaction in the sol-gel composites was characterized by Fourier transform-infrared (FT-IR) spectroscopy. The well-organized morphology of $Al@Fe_2O_3$ core-shell nanocomposites was observed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) were used to analyze the elemental composition and crystallization structure of the composites.

PDMS-b-PMMA 공중합체 막의 제조 및 투과특성 (Preparation and Permeation Characteristics of PDMS-b-PMMA Copolymer Membrane)

  • 강태범;조아라;이현경
    • 멤브레인
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    • 제18권3호
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    • pp.219-225
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    • 2008
  • 본 연구에서는 atom transfer radical polymerization (ATRP)에 의해 polydimethylsiloxane (PDMS)와 methyl-methacrylate (MMA)로부터 polydimethylsiloxane-polymethylmethacrylate (PDMS-PMMA) block copolymer를 합성하였다. 합성된 PDMS-b-PMMA copolymer막의 특성은 FT-IR, $^1H$ NMR, GPC, DSC 등을 사용하여 조사하였다. 질소와 수소의 투과도는 각각 $1.2{\sim}l.5$ barrer와 $6.2{\sim}10.5$ barrer를 보였고, 질소에 대한 수소의 선택도는 $5.3{\sim}6.9$ 범위였다. PDMS-b-PMMA copolymer 막의 투과도와 선택도는 PDMS 막보다는 낮은 값을 보였고, PMMA 막보다는 높은 결과를 보였다.

원자 이동 라디칼 중합을 이용한 Polystyrene-b-Poly(acrylic acid) 블록 이오노머의 합성 및 분석 (Synthesis and Characterization of Polystyrene-b-Poly(acrylic acid) Block Ionomer via Atom Transfer Radical Polymerization)

  • 박계리;안성국;조창기
    • 폴리머
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    • 제27권1호
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    • pp.17-25
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    • 2003
  • 원자 이동 라디칼 중합 (ATRP)을 이용하여 CuBr/N,N,N',N",N"-pentamethyldiethylene triamine 촉매 시스템하에서 용액중합으로 polystyrene 거대 개시제와 polystyrene-b-t-poly(butyl acrylate) (PS-b-P(tBA)) 블록 공중합체를 합성한 후, 가수분해를 통해 polystrene-b-poly(acrylic acid) 양친매성 블록 공중합체를 얻었다. 또한, 이를 중화하여 블록 이오노머를 제조하였다. 합청된 PS-b-P(tBA) 블록 공중합체는 분자량이 5000-10000 정도로 조절되었고, 분자량 분포도 1.2 이하로 비교적 좁게 나타났다. 공중합체는 $^1$H-NMR, FT-IR로 분석하였으며, DSC로 열적 성질을 측정한 결과, styrene의 비율이 더 많기 때문에 100 $^{\circ}C$ 근처에서 T$_{g}$가 나타났으며, TEM을 통해 이온 그룹의 상분리를 확인하였다.분리를 확인하였다.

Synthesis of a Triblock Copolymer Containing a Diacetylene Group and Its Use for Preparation of Carbon Nanodots

  • Kim, Beom-Jin;Oh, Dong-Kung;Chang, Ji-Young
    • Macromolecular Research
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    • 제16권2호
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    • pp.103-107
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    • 2008
  • Carbon nanodots were prepared by the pyrolysis of a triblock copolymer. The triblock copolymer, poly(methyl methacrylate)-b-polystyrene-b-poly(methyl methacrylate) was synthesized by atom transfer radical polymerization using an initiator containing a diacetylene group. A polymer thin film on a mica substrate was prepared by spin-casting at 2,000 rpm from a 0.5 wt% toluene solution of the triblock copolymer. After drying, the cast film was vacuum-annealed for 48 h at $160^{\circ}C$. The annealed film formed a spherical morphology of polystyrene domains with a diameter of approximately 30 nm. The film was exposed to UV irradiation to induce a cross-linking reaction between diacetylene groups. In the subsequent pyrolysis at $800^{\circ}C$, the cross-linked polystyrene spheres were carbonized and the poly(methyl methacrylate) matrix was eliminated, resulting in carbon nanodots deposited on a substrate with a diameter of approximately 5 mn.

Synthesis of New pH-Sensitive Amphiphilic Block Copolymers and Study for the Micellization Using a Fluorescence Probe

  • Kim, Kyung-Min;Choi, Song-Yee;Jeon, Hee-Jeong;Lee, Jae-Yeol;Choo, Dong-Joon;Kim, Jung-Ahn;Kang, Yong-Soo;Yoo, Hyun-Oh
    • Macromolecular Research
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    • 제16권2호
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    • pp.169-177
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    • 2008
  • This paper reports a facile synthesis of new water-soluble poly(ethylene oxide) (PEO)-based amphiphilic block copolymers showing pH sensitive phase transition behaviors. The copolymers were prepared by atom transfer radical polymerization (ATRP) of methacrylamide type of monomers carrying a sulfonamide group using a PEO-based macroinitiator and a Cu(I)Br/$Me_6TREN$ catalytic system in aqueous media. The resulting polymers were characterized by a combination of $^1H$-NMR, size exclusion chromatography, and UV/Visible spectrophotometeric analysis. The micellization of the block copolymers as a drug-loading mechanism in aqueous media using fluorescein salt was examined as a function of pH. The stable micelle formation and its loading efficacy suggest that the block copolymers can be used as precursors for drug-nanocontainers.

Study on the molecular weights of atom transfer radical polymerization of MA and MMA.

  • Semsarzadeh Mohammad Ali;Daronkola Mohammad Reza Rostami
    • 한국고분자학회:학술대회논문집
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    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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    • pp.324-324
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    • 2006
  • In copolymerization of methyl acrylate (MA) and methyl methacrylate (MMA) with various ratios of MA to MMA and $[CuCl]/[PMDETA]/[PVAc-CCl_{3}]$ catalyst system in bulk at $80^{\circ}C$ via ATRP, several terpolymer with different copolymer composition, were synthesized. The atom transfer radical copolymerization of MA and MMA with macroinitiator, is very sensitive to molecular weight and its distribution. In this work it was possible to calculate the molecular weight of the terpolymers and show that it is close to the experimentally determined number average molecular weight from GPC.

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Poly(3,4-ethylenedioxythiophene)을 이용한 Core/shell 나노입자와 원자이동 라디칼중합 공정에 의한 다중벽 탄소나노튜브 나노복합체 제조 (Preparation of Core/Shell Nanoparticles Using Poly(3,4-ethylenedioxythiophene) and Multi-Walled Carbon Nanotube Nanocomposites via an Atom Transfer Radical Polymerization)

  • 주영태;진선미;김양수
    • 폴리머
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    • 제33권5호
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    • pp.452-457
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    • 2009
  • 다중벽 탄소나노튜브 및 전도성 고분자인 PEDOT으로 이루어진 하이브리드 나노재료를 제조하였다. 다중벽 탄소나노튜브 표면에 처리반응을 수행함으로써 -Br 특성기를 갖는 다중벽 탄소나노튜브를 제조하였으며, 이를 중합반응의 개시제로 사용하였다. 이와 함께 MMA를 사용하여 촉매와 리간드 존재 하에서 원자이동 라디칼중합 공정을 수행함으로써 다중벽 탄소나노튜브 표면에 PMMA가 공유결합된 나노복합체를 제조하였다. 미니에멀젼 중합공정을 통하여 제조된 PS 수용성 에멀젼에 EDOT과 산화가를 투입하여 산화중합을 수행함으로써 core-shell 구조를 갖는 PEDOT/PS 나노입자를 제조하였다. 실란화합물로 표면 처리한 silica 입자를 PEDOT:poly(styrene sulfonate) (PSS) 수용성 분산액에 투입한 후 표면화학 반응과정을 수행함으로써 silica 외벽에 PEDOT:PSS가 코팅된 나노입자를 제조하였다. 하이브리드 나노재료들은 TEM, FE-SEM, TGA, EDX, UV 그리고 FT-IR 등을 사용하여 분석되었다.