• Macromolecular Research
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• v.17 no.6
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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.

• Journal of the Korean Chemical Society
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• v.21 no.6
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• pp.440-444
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• 1977

The anionic polymerization of ${\varepsilon}$-caprolactam via $CS_2$/KOH catalysis was carried out under various conditions. The inherent viscosity of the polymers and percent conversion of the polymers were determined. It was observed that the percent conversion was increased as an increasing concentration of catalyst and initiator. The percent conversion was relatively low at low temperature and the highest percent conversion was obtained at temperature between $130^{\circ}C,\;to\;155^{\circ}C$ with any $CS_2$/KOH mole ratio.

• Applied Chemistry for Engineering
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• v.9 no.5
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• pp.726-728
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• 1998

Oil-impregnated nylons were synthesized by anionic polymerization of ${\varepsilon}$-caprolactam in the presence of mineral oils. Reaction rate and molecular weight of the product were not significantly affected by the addition of oils less than 8 phr. Physical properties such as elongation and notched impact strength were improved by the addition of oil, on the other hand hardness and tensile stress at break were slightly decreased. Oil-impregnated nylon with an oil content of 6 phr showed a minimum friction coefficient, which is only 32% compared to a friction coefficient of nylon 6 without oil.

• Elastomers and Composites
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• v.56 no.3
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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.

• Journal of the Korean Applied Science and Technology
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• v.26 no.2
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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).

• Proceedings of the Korean Society For Composite Materials Conference
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• 2003.10a
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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.

• Polymer(Korea)
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• v.34 no.4
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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.

• Polymer(Korea)
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• v.34 no.2
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• pp.159-165
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• 2010

Dipyridine-terminated polystyrenes and polybutadienes were synthesized by the chain endfunctionalization reaction of polystyryllithium (PSLi) and polybutadienyllithium (PBDLi) with di(2-pyridyl) ketone(DPK) using a living anionic polymerization method in the Ar-glove box. Living polymeric lithiums with low molecular weights (Mw=1000~2000 g/mol) were used to investigate the chain end-functionalization yield with DPK and the degree of coupling reaction by the attack of organolithium to the pyridine ring in the presence of TMEDA using GPC, $^1H$-NMR, $^{13}C$ analysis. DPK-terminated PBD exhibited much higher functionalization yield and less amount of coupling reaction compared with DPK-terminated PS. 86% functionalization yield with 9% degree of coupling was obtained when the PBDLi was added dropwise to DPK solution at room temperature. The functionalization yield was increased as the reaction temperature decreased, however, no LiCl effect was observed in this chain end-functionalization reaction with DPK.

• Macromolecular Research
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• v.14 no.3
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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.

• Polymer(Korea)
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• v.38 no.6
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• pp.714-719
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• 2014

Bio-based nylon 6-morpholinone random copolymers were prepared by the anionic ring opening polymerization of ${\varepsilon}$-caprolactam and morpholinone, both of which were prepared from lysine and glucose, respectively. From this work, a new biomass based nylon 6 with improved hydrophilicity was prepared. Optimizing the polymerization condition, copolymer with a viscosity-average molecular weight of 30000 g/mol was prepared, with a yield of 80%. It was possible to improve the hydrophilicity of nylon 6 by its copolymerization with morpholinone. The prepared nylon 6-morpholinone random copolymers were then characterized using several analytical methods such as DSC, TGA, XRD, viscosity measurement with U-shaped glass capillary viscometer and contact angle measurement.