• Title/Summary/Keyword: radical polymerization

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Core-Shell Poly(Styrene/Sulfonated N-hydroxy Ethyl Aniline) Latex Particles Prepared by Chemical Oxidative Polymerization in Emulsion Polymerization

  • Shin Jin-Sup;Lee Jung-Min;Suzuki Kiyoshi;Nomura Mamoru;Cheong In-Woo;Kim Jung-Hyun
    • Macromolecular Research
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    • v.14 no.4
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    • pp.466-472
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    • 2006
  • The kinetic behavior of emulsion polymerizations of styrene in the presence of sulfonated N-hydroxy ethyl aniline (SHEA) was investigated with two initiators: 2,2'-azobisisobutyronitrile (AIBN) and potassium persulfate (KPS). SHEA was synthesized using a stepwise polyurethane reaction method from 3-hydroxy-1-propane sulfonic acid sodium salt, isophorone diisocyanate (IPDI), and N-(2-hydroxyethyl) aniline. Stable core-shell poly(styrene/sulfonated N-hydroxy ethyl aniline, St/SHEA) latex particles were successfully prepared by using an appropriate amount of AIBN, in which SHEA plays the role of 'surfmer', i.e., acting as both a surfactant in the emulsion polymerization and a monomer in the chemical oxidative polymerization. The kinetic behavior was dissimilar to that of typical emulsion polymerization systems. A long inhibition period and low rate of polymerization were observed due to radical loss by the oxidative polymerization of SHEA. It was concluded, due to the low water-solubility of AIBN and retardation reaction by SHEA, that the initial loci of polymerization were monomer droplets. However, growing polymer particles as polymerization loci became predominant as polymerization proceeded. It was suggested that AIBN was more effective than KPS in the preparation of the core-shell type poly(St/SHEA) latex particles. With KPS, no substantial polymerization was observed in any of the samples.

Preparation and Characterizations of C60/Polystyrene Composite Particle Containing Pristine C60 Clusters

  • Kim, Jung-Woon;Kim, Kun-Ji;Park, Soo-Yeon;Jeong, Kwang-Un;Lee, Myong-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.9
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    • pp.2966-2970
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    • 2012
  • Fullerene/polystyrene ($C_{60}$/PS) nano particle was prepared by using emulsion polymerization. Styrene and fullerene were emulsified in aqueous media in the presence of poly(N-vinyl pyridine) as an emulsion stabilizer, and polymerization was initiated by water soluble radical initiator, potassium persulfate. The obtained nano particles have an average diameter in the range of 400-500 nm. The fullerene contents in the nano particle can be controlled up to 15 wt % by varying the feed ratio, which was confirmed by themogravimetric analysis (TGA) and elemental analysis (EA). The structure and morphologies of the $C_{60}$/PS nano particles were examined by various analytical techniques such as dynamic light scattering (DLS), scanning electron microscope (SEM), transmission electron microscope (TEM), electron diffraction (ED) pattern, X-ray powder diffraction (XRD), and UV spectroscopy. Unlike conventional $C_{60}$/PS particles initiated by organic free radical initiators, in which the fullerene is copolymerized forming a covalent bond with styrene monomer, the prepared $C_{60}$/PS nano particles contain pristine fullerene as secondary particles homogeneously distributed in the polystyrene matrix.

Bioconjugation of Poly(poly(ethylene glycol) methacrylate)-Coated Iron Oxide Magnetic Nanoparticles for Magnetic Capture of Target Proteins

  • Kang, Sung-Min;Choi, In-Sung S.;Lee, Kyung-Bok;Kim, Yong-Seong
    • Macromolecular Research
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    • v.17 no.4
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    • pp.259-264
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    • 2009
  • Chemical modification of magnetic nanoparticles(MNPs) with functional polymers has recently gained a great deal of attention because of the potential application of MNPs to in vivo and in vitro biotechnology. The potential use of MNPs as capturing agents and sensitive biosensors has been intensively investigated because MNPs exhibit good separation-capability and binding-specificity for biomolecules after suitable surface functionalization processes. In this work, we demonstrate an efficient method for the surface modification of MNPs, by combining surface-initiated polymerization and the subsequent conjugation of the biologically active molecules. The polymeric shells of non-biofouling poly(poly(ethylene glycol) methacrylate)(pPEGMA) were introduced onto the surface of MNPs by surface-initiated, atom transfer radical polymerization(SI-ATRP). With biotin as a model of biologically active compounds, the polymeric shells underwent successful post-functionalization via activation of the polymeric shells and bioconjugation of biotin. The resulting MNP hybrids showed a biospecific binding property for streptavidin and could be separated by magnet capture.

Synthesis of High Molecular Weight 3-Arm Star PMMA by ARGET ATRP

  • Jeon, Hyun-Jeong;Youk, Ji-Ho;Ahn, Sung-Hee;Choi, Jin-Hwan;Cho, Kwang-Soo
    • Macromolecular Research
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    • v.17 no.4
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    • pp.240-244
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    • 2009
  • High molecular weight(MW), 3-arm star poly(methyl methacrylate)(PMMA) with a narrow MW distribution($M_n$=570,000 g/mol, PDI=1.36) was successfully synthesized by activators regenerated by electron transfer(ARGET) atom transfer radical polymerization(ATRP). The polymerization was carried out with a trifunctional initiator/$CuBr_2$/N,N,N',N",N"-pentamethyldiethy lenetriamine(PMDETA) initiator/catalyst system in the presence of a tin(II) 2-ethylhexanoate [$Sn(EH)_2$] reducing agent at $90^{\circ}C$. The concentration of the copper catalyst was as low as 30 ppm, and a high initiation efficiency of the initiating sites was obtained. The chain-end functionality of the high MW, 3-arm star PMMA was confirmed by a chain extension experiment with styrene via ARGET ATRP, using the same catalyst system.

Effect of Solvent on Swelling, Porosity and Morphology of Transparent Poly (HEMA)

  • Pathak Tara Sankar;Kim Lae-Hyun;Chung Kun-Yong
    • Korean Membrane Journal
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    • v.8 no.1
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    • pp.67-73
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    • 2006
  • Transparent materials are well known but preparation of transparent poly 2-hydroxyethyl methacrylate {poly (HEMA)} material by varying solvent is a new one and economically reliable. This material is prepared from hydroxyl based monomer HEMA by radical polymerization using benzoyl peroxide (BPO) as initiator and isobutanol, 2-butanol, 1-butanol, hexane and toluene as a solvent. The reaction temperature, time and stirring speed were set at $70^{\circ}C$, 4 hrs and 150 rpm, respectively. The polymer was characterized for functional group by IR spectroscopy. It was observed that the intensity of band at $1637 cm^{-1}$ a characteristic band of C=C stretching disappeared indicating that it was completely consumed after polymerization. It was observed that swelling percentage increases with increase as time passes but after a certain time a constant swelling percentage is achieved. SEM pictures reveals that poly (HEMA) prepared by different solvent shows pore with a distinguishable void up to several micrometers. The BET surface area, cumulative pore volume and average pore diameter is greater in poly (HEMA) prepared by hexane as a solvent compared to other solvents. Poly (HEMA) prepared by 1-butanol as a solvent shows higher glass transition temperature compared to other solvents. Poly (HEMA) prepared by different solvents shows $90{\sim}94%$ light transmission property from light transmission measurement and looks transparent.

Chain Transfer to Monomer and Polymer in the Radical Polymerization of Vinyl Neo-decanoate

  • Balic, Robert;Fellows, Christopher M.;Van Herk, Alex M.
    • Macromolecular Research
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    • v.12 no.4
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    • pp.325-335
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    • 2004
  • Molecular weight distributions of poly(vinyl neo-decanoate) produced by the bulk polymerization of the monomer to low conversions were investigated to obtain values of the rate constants for the chain transfer to monomer ( $C_{M}$). The value of $C_{M}$ of 7.5($\pm$0.6)${\times}$10$^{-4}$ was obtained from a logarithmic plot of the number distribution at 5,25, and 5$0^{\circ}C$, which suggests that the activation energy for chain transfer is on the order of 20-25 kJ ㏖$^{-1}$ . These plots were linear between the number and weight-average degrees of polymerization, but not over the whole molecular weight range for which a significant signal was observed in the gel permeation chromatography (GPC) trace. Modeling suggests that the deviations observed at high molecular weights can be explained by branching of the chains through chain transfer to the polymer, with a branching density as low as 10$^{-5}$ , without affecting the slope at low values of the number of monomer unit, N. This deviation from the expected distribution of linear chains was used to estimate the branching densities at low conversion.ion.

Ultrasound Energy Effect as Initiator of Polystyrene Latex Polymerization (Polystyrene Latex 제조공정에서 초음파 에너지의 개시효과)

  • Lee, Seung-Bum;Kim, Won-Il;Hong, In-Kwon
    • Elastomers and Composites
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    • v.31 no.3
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    • pp.175-182
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    • 1996
  • Polymer latices, prepared from the emulsion polymerization of vinyl monomer compounds, are widely used for many industrial applications. Included among these are uses in paints, adhesives, flocculants, and heavy-duty plastics as well as their original use in synthetic rubber compounds. The emulsion polymerization process with chemical initiator has chemical disadvantage such as removal of initiator which was left after polymerization. In this study, polystyrene latex was prepared by using ultrasonic irradiation which generate the free radical, and then it was analyzed by GPC. Reaction temperature hardly have an effect on average molecular weight. Average molecular weight is increased by increasing amount of surfactant, i.e. SDS, but polydispersity is decreased. After 90 minutes of reaction time, increase and decrease of average molecular weight Is repeated. It is proposed that monodisperse polymer is obtained by controlling ultrasonic irradiation time and surfactant concentration.

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Property Control in a Continuous MMA Polymerization Reactor using EKF based Nonlinear Model Predictive Controller

  • Ahn, Sung-Mo;Park, Myung-June;Rhee, Hyun-Ku
    • 제어로봇시스템학회:학술대회논문집
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    • 1998.10a
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    • pp.468-473
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    • 1998
  • A mathematical model was developed for a continuous re-actor in which free radical polymerization of methyl methacrylate (MMA) occurred. Elementary reactions considered in this study were initiation, propagation, termination, and chain transfers to monomer and solvent. The reactor model took into account the density change of the reactor contents and the gel effect. A control system was designed for a continuous reactor using extended Kalman filter (EKF) based non-linear model predictive controller (NLMPC) to control the conversion and the weight average molecular weight of the polymer product. Control input variables were the jacket inlet temperature and the feed flow rate. For the purpose of validation of the control strategy, on-line digital control experiments were conducted with densitometer and viscometer for the measurement of the polymer properties. Despite the com-plex and nonlinear features of the polymerization reaction system, the EKF based NLMPC performed quite satisfactorily for the property control of the continuous polymerization reactor.

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Preparation and Characterization of Monolithic Poly(methacrylic acid - ethylene glycol dimethacrylate) Columns for High Performance Liquid Chromatography

  • Yan, Hong-yuan;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.1
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    • pp.71-76
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    • 2006
  • Porous polymer monolithic columns were prepared by the direct free radical copolymerization of methacrylic acid and ethylene glycol dimethacrylate within the confines of a chromatographic column in the presence of toluene-dodecanol as a porogenic solvent. The separation characteristics of the monolithic columns were tested by a homologous series of xanthine derivatives, theophylline and caffeine. The effects of the polymerization mixture composition and polymerization condition, mobile phase composition, flow rate and temperature on the retention times and separation efficiencies were investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and temperatures. Hydrogen-bonding interaction played an important role in the retention and separation. Compared with conventional particle columns, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency and fast analysis.

Graft Polymerization of Acrylic Acid onto nylon 6

  • Park, Jae ho;Lee, Chong-Kwang
    • Nuclear Engineering and Technology
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    • v.8 no.3
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    • pp.159-168
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    • 1976
  • Acrylic acid has been grafted onto nylon fabric with ceric salts and ${\gamma}$-rays from Co-60 as initiators. The distribution of molecular weight of the grafted polyacrylic acid has been determined and it was found that the ratio of weight-average and number-average molecular weight was higher in room temp. than in low temp. (-184$^{\circ}C$). The weight-average molecular weight of the polyacrylic acid was calculated from viscosity measurements in sodium hydroxide solution. The factors affecting graft polymerization of acrylic acid onto nylon were examined. A possible mechanism that the oxidation of nylon probably takes place at the methylene group attached to nitrogen to give a free-radical was discussed.

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