• Macromolecular Research
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• 제17권6호
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• pp.365-377
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• 2009

In this feature article, we briefly review the new methods we have utilized recently in the investigation of morphology and phase behavior of block copolymers. We first describe the chromatographic fractionation method to purify block copolymers from their side products of mainly homopolymers or block copolymer precursors inadvertently terminated upon addition of the next monomer in the sequential anionic polymerization. The chromatographic method is extended to the fractionation of the individual block of diblock copolymers which can yield the diblock copolymer fractions of different composition and molecular weight, which also have narrower distributions in both molecular weight and composition. A more detailed phase diagram could be constructed from the set of block copolymer fractions without the need of acquiring many block copolymers each prepared by anionic polymerization. The fractions with narrow distribution in both molecular weight and composition exhibit better long-range ordering and sharper phase transition. Next, epitaxial relationships between two ordered structures in block copolymer thin film is discussed. We employed the direct visualization method, transmission electron microtomography(TEMT) to scrutinize the grain boundary structure.

• 대한화학회지
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• 제21권6호
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• pp.440-444
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• 1977

$CS_2$/KOH catalysis를 이용해서 ${\varepsilon}$-caprolactam의 음이온중합을 시키고 percent conversion과 점도를 측정하였다. $80^{\circ}C,\;105^{\circ}C$의 비교적 낮은 온도에서는 $CS_2$/KOH mole ratio가 0.5일때 percent conversion이 가장 높았으며 또 KOH의 당량에 비례하여 percent conversion도 증가하였다. 그러나 $130^{\circ}C,\;155^{\circ}C$로 중합온도를 상승함에 따라 $CS_2$/KOH mole ratio와 KOH양에는 크게 관계없이 높은 percent conversion을 얻을 수 있었다. 그리고 30分 정도의 짧은 중합시간으로도 $80{\%}$ 이상의 높은 percent conversion을 얻을 수 있었다.

• 공업화학
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• 제9권5호
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• pp.726-728
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• 1998

${\varepsilon}$-caprolactam의 음이온 중합반응을 미네랄 오일의 존재하에서 수행하여 오일함침 나일론 6을 합성하였다. 8 phr 미만의 오일이 첨가되었을 때에는 중합반응속도 및 생성물의 분자량에 큰 변화가 없었다. 오일의 첨가에 의해서 생성물의 신율 및 충격강도는 향상되었으며, 표면경도와 인장강도는 저하되었다. 오일함량이 6 phr인 나일론에서 마찰계수는 최소값을 나타내었으며, 이때의 마찰계수값은 오일이 첨가되지 않은 나일론의 32%에 지나지 않았다.

• Elastomers and Composites
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• 제56권3호
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• pp.152-163
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• 2021

Liquid butadiene rubber (LqBR) is used as a processing aid and plays a vital role in the manufacture of high-performance tire tread compounds. In this study, center-functionalized LqBR (C-LqBR) was polymerized with different vinyl content via anionic polymerization. The effects of the vinyl content on the properties of the compounds were investigated by partially replacing the treated distillate aromatic extract (TDAE) oil with C-LqBR in silica-filled rubber compounds. C-LqBR compounds showed a low Payne effect and Mooney viscosity regardless of the vinyl content, because of improved silica dispersion due to the ethoxysilyl group. As the vinyl content of C-LqBR increased, the optimum cure time (t₉₀) increased owing to a decrease in the number of allylic hydrogen. Moreover, the glass transition temperature (T_g) of the compound increased, and snow traction and abrasion resistance performance decreased, whereas wet grip improved. The energy loss characteristics revealed that the hysteresis attributed to the free chain ends of C-LqBR was dominant.

• 한국응용과학기술학회지
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• 제26권2호
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• pp.199-204
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• 2009

Silicone dioxide absorbed polyoxyethylene alkylether sulfate (EU-S133D) surfactant was prepared. Core-shell polymers of inorganic/organic pair, which have both core and shell component, were synthesized by sequential emulsion polymerization using Acrylate as a shell monomer and potassium persulfate (KPS) as an initiator. We found that when Acrylate core prepared by adding 2.0 wt% EU-S133D, silicone dioxide/Acrylate core-shell polymerization was carried out on the surface of silicone dioxide particle without forming the new silicone dioxide particle during acrylate shell polymerization in the inorganic/organic core-shell polymer preparation. The structure of core-shell polymer were investigated by measuring to the thermal decomposition of polymer composite using thermogravimetric analyzer and morphology of latex by scanning electron microscope(SEM).

• 한국복합재료학회:학술대회논문집
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• 한국복합재료학회 2003년도 추계학술발표대회 논문집
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• pp.16-20
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• 2003

As the preliminary works for the preparation of exfoliated nanocomposites by reactive extrusion (REX) the modified anionic polymerization proceeded in a flask using an $\varepsilon$-caprolactam, catalyst, initiator, and clay. Polymerization methods were classified with a variation of the clay adding time. Intercalations mechanism of clay layers was investigated by measuring the WAXD peaks of clay with polymerization. In the preparation of nanocomposites, the molecular weight of nylon 6 was affected by the clay content. From the mechanical property measurement, improved properties were obtained in comparison to the neat nylon 6, and these properties were also affected by the molecular weight.

• 폴리머
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• 제34권4호
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• pp.306-312
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• 2010

Triphenylvinylsilane (TPVS) containing vinyl acetate (VAc), butyl acrylate (BA), and Nmethylolacrylamide (NMA) copolymers were prepared by emulsion polymerization. The polymerization was performed at $80^{\circ}C$ in the presence of auxiliary agents and ammonium peroxodisulfate (APS) as the initiator. Sodium dodecyl sulphate (SDS) and Arkupal N-300 were used as anionic and nonionic emulsifiers, respectively. The resulting copolymers were characterized by using Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC), and dynamic light scattering (DLS). Thermal properties of the copolymers were studied by using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The morphology of copolymers was also investigated by scanning electron microscopy (SEM) and then the effects of silicone concentrations on the properties of the TPVS-containing VAc-acrylic emulsion copolymers were discussed. The obtained copolymers have high solid content (50%) and can be used in weather resistant emulsion paints as a binder.

• 폴리머
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• 제34권2호
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• pp.159-165
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• 2010

리빙 음이온 중합에 의해 sec-BuLi으로 개시된 polystyryllithium (PSLi)과 polybutadienyllithium (PBDLi)의 연쇄 말단에 di(2-pyridyl)ketone(DPK)을 반응시켜 dipyridine이 말단 관능화된 폴리스티렌과 폴리부타디엔을 각각 합성하였다. 분자량이 1000~2000 g/mol인 PSLi과 PBDLi을 사용하여 TMEDA 존재하에서 말단 DPK-관능화 반응 후 GPC에 의한 분자량 특성분석과 $^1H$-NMR, $^{13}C$-NMR 분석에 의한 고분자 말단 구조 분석을 통하여 말단 관능화 수율과 함께 유기리튬의 피리딘 링 친핵성 부가 반응으로 인한 커플링 현상을 확인하였다. PBDLi에 DPK를 부가하는 일반적인 말단 관능화 방법에 비하여 역으로 부가하는 방법에서 최대 9% 정도의 커플링 정도와 86% 이상의 관능화 수율을 보였다. 이 반응에서 LiCl 첨가효과는 없었으며, 반응온도가 낮을수록 높은 관능화 수율을 나타내었다.

• Macromolecular Research
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• 제14권3호
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• pp.287-299
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• 2006

To successively synthesize star-branched polymers, we developed a new iterative methodology which involves only two sets of the reactions in each iterative process: (a) an addition reaction of DPE or DPE-functionalized polymer to a living anionic polymer, and (b) an in-situ reaction of 1-(4-(4-bromobutyl)phenyl)-1-phenylethylene with the generated 1,1-diphenylalkyl anion to introduce one DPE functionality. With this methodology, 3-, 4-, and 5-arm, regular star-branched polystyrenes, as well as 3-arm ABC, 4-arm ABCD, and a new 5-arm ABCDE, asymmetric star-branched polymers, were successively synthesized. The A, B, C, D, and E arm segments were poly(4-trimethylsilylstyrene), poly(4-methoxystyrene), poly(4-methylstyrene), polystyrene, and poly(4-tert-butyldimethylsilyloxystyrene), respectively. All of the resulting star-branched polymers were well-defined in architecture and precisely controlled in chain length, as confirmed by SEC, $^1H$ NMR, VPO, and SLS analyses. Furthermore, we extended the iterative methodology by the use of a new functionalized DPE derivative, 1-(3-chloromethylphenyl)-1-((3-(1-phonyletheny1)phenyl) ethylene, capable of introducing two DPE functionalities via one DPE anion reaction site in the reaction (b). The number of arm segments of the star-branched polymer synthesized by the methodology could be dramatically increased to 2, 6, and up to 14 by repeating the iterative process.

• 폴리머
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• 제38권6호
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• pp.714-719
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• 2014

라이신과 글루코오스에서부터 제조된 카프로락탐과 모폴리논을 음이온 개환중합법을 이용하여 나일론 6-모폴리논 랜덤 공중합체를 합성함으로써 바이오매스 기반의 새로운 나일론을 제조할 수 있었으며 또한 친수성이 향상된 나일론 6을 제조할 수 있었다. 중합 조건을 적절하게 조절함으로써, 점도평균분자량 30000 g/mol과 수율 80%의 공중합체를 제조할 수 있었다. 모폴리논을 공중합 단량체로 사용함으로써 나일론 6의 친수성을 높게 향상시킬 수 있었다. 제조된 나일론 6-모폴리논 랜덤공중합체를 시차주사 열량계(DSC), 열중량 분석기(TGA), X-선 회절분석기(XRD), 점도계, 접촉각 측정기와 같은 분석방법으로 그 특성을 분석하였다.