• Title/Summary/Keyword: Dispersion polymerization

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The Effect of Camphorsulfonic Acid in TEMPO-Mediated Bulk and Dispersion Polymerization of Styrene

  • Oh Sejin;Kim Gijung;Ko Narae;Shim Sang Eun;Choe Soonja
    • Macromolecular Research
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    • v.13 no.3
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    • pp.187-193
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    • 2005
  • The TEMPO-mediated living free-radical bulk and dispersion polymerization of styrene in the presence of camphorsulfonic acid (CSA) are investigated. In the absence of TEMPO and CSA in the bulk polymerization, a conversion of $93\%$ is achieved within 6 hr of polymerization. When only TEMPO is involved in this polymerization, the pseudo-living free-radical polymerization is well achieved, however, the polymerization rate becomes quite slow. This retardation of the polymerization rate is solved by the addition of a low concentration of CSA. In the TEMPO-mediated dispersion polymerization in the presence of CSA, similar trends in the conversion, kinetics, and PDI are observed as those observed in the case of bulk polymerization. When only TEMPO is used in the dispersion polymerization, the resulting particle size becomes quite broad, due to the prolonged polymerization time. However, when a 1.0 molar ratio of CSA to TEMPO is added to the TEMPO-mediated dispersion polymerization, fairly mono-disperse PS microspheres having an average size of 5.83 $\mu$m and a CV of 3.4$\%$ are successfully obtained, due to the narrow molecular weight distribution of the intermediate oligomers and shortening of the polymerization time. This result indicates that the addition of CSA to the TEMPO-mediated bulk and the use of dispersion polymerization not only shortens the polymerization time, but also greatly improves the uniformity of the microspheres.

Dispersion Polymerization of Styrene Employing Lyophilic Comonomer in the Absence of Stabilizer: Synthesis of Impurity-free Microspheres

  • Han, Hye-Kyung;Lee, Jeong-Woo;Hong, Jin-Ho;Shim, Sang-Eun
    • Macromolecular Research
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    • v.17 no.7
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    • pp.469-475
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    • 2009
  • We investigated the feasibility of dispersion polymerization without any stabilizer, which has been considered essential for ensuring colloidal stability. By employing small amounts of a lyophilic comonomer, 4-vinyl pyridine, styrene was successfully polymerized by dispersion polymerization in aqueous alcohol without stabilizer to afford stable poly(styrene-co-4-vinyl pyridine) copolymer microspheres. The stable microspheres were produced in the 4-vinyl pyridine range of 2-15 wt% to styrene. Without 4-vinyl pyridine, severely coagulated particles were obtained, implying that the poly(4-vinyl pyridine) moiety endowed colloidal stability. The polymerization kinetics, behavior, and properties of the ultimate particles showed general features of dispersion polymerization. The study results suggest that stabilizer- tree dispersion polymerization is possible, thereby facilitating the synthesis of impurity(stabilizer)-tree polymer particles.

Preparation of Highly Cross-linked, Monodisperse Poly(methyl methacrylate) Microspheres by Dispersion Polymerization; Part I. Batch Processes

  • Lee, Ki-Chang;Lee, Sang-Yun
    • Macromolecular Research
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    • v.15 no.3
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    • pp.244-255
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    • 2007
  • Nucleation is the most sensitive stage in the preparation of highly cross-linked, monodisperse microspheres by dispersion polymerization, since the addition of a small amount of cross-linker results in particle deformation and coagulation. To overcome these problems, $5\;{\mu}m$ poly(methyl methacrylate) seed particles prepared by dispersion polymerization were used in the preparation of mono disperse, cross-linked PMMA particles containing up to 7 wt% divinylbenzene by seeded batch dispersion polymerization. Spherical particles with a narrow size distribution containing up to 8 wt% of EGDMA were prepared by seeded multi-batch dispersion polymerization processes. These particles were identified by scanning electron microscopy and DSC.

Dispersion Polymerization of Acrylamide in Methanol/Water Media

  • Lee, Ki-Chang;Lee, Seung-Eun;Song, Bong-Keun
    • Macromolecular Research
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    • v.10 no.3
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    • pp.140-144
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    • 2002
  • Dispersion polymerization of acrylamide was carried out in the media of methyl alcohol/$H_2O$ mixtures using hydroxypropyl cellulose and ammonium persulfate as steric stabilizer and initiator, respectively. The effects of concentrations of initiator and steric stabilizer, amount of monomer, polymerization temperature, methyl alcohol/$H_2O$ ratio, and purification of monomer and nitrogen purge on the particle size of the latices and molecular weight of the polymers were investigated. The average particle diameter increased with increasing concentration of initiator, water content in methyl alcohol/$H_2O$ media, and polymerization temperature, but decreased with monomer and stabilizer concentrations. The viscosity average molecular weight increased with increasing concentrations of monomer, steric stabilizer, and water content in dispersion media, but decreased with initiator concentration and polymerization temperature. The PAM polymers prepared with the purified monomer and the nitrogen purging before the reaction showed the highest molecular weight.

Dependence of Retardation Dispersion on the Ultraviolet Polarization Direction During Photopolymerization of Self-organized Smectic Reactive Mesogen Molecules

  • Jeong, Jinyoung;Choi, Yu-Jin;Jeong, Kwang-Un;Lee, Ji-Hoon
    • Current Optics and Photonics
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    • v.2 no.3
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    • pp.286-290
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    • 2018
  • We investigated the dependence of the retardation dispersion on the polarization direction of ultraviolet (UV) light during the photopolymerization of self-organized smectic reactive mesogen (RM) molecules. RM retarder film that was photopolymerized with UV light linearly polarized parallel to the layer plane showed negative dispersion (ND) of retardation for a wide range of UV polymerization temperatures. On the other hand, film that was photopolymerized with unpolarized UV light showed negative dispersion in a narrow range of UV polymerization temperatures. With a certain UV polymerization temperature, the dispersion of retardation was converted from positive to negative, depending on the UV polarization.

Dispersion Polymerization of Acrylamide in t-Butyl Alcohol/Water Media

  • Lee, Ki-Chang;Lee, Seung-Eun;Park, Yoo-Jin;Song, Bong-Keun
    • Macromolecular Research
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    • v.12 no.2
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    • pp.213-218
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    • 2004
  • We have performed dispersion polymerization of acrylamide in tert-butyl alcohol/water mixture-using hydroxypropyl cellulose and ammonium persulfate as the stabilizer and the initiator, respectively - to study the effects that the concentration of monomer, initiator, and stabilizer, the tert-butyl alcohol/water ratios as polymerization media, and the reaction temperature have on, among other things, the polymerization kinetics, particle sizes, and molecular weights. The polymerization rate increased upon increasing the concentration of the monomer, initiator, and stabilizer, the water content in the tert-butyl alcohol/water media, and the polymerization temperature. The average particle size of the lattices increased upon increasing the concentration of initiator, the polymerization temperature, and the water content in the tert-butyl alcohol/water media, but it decreased upon increasing the concentration of monomer and stabilizer. The viscosity-average molecular weight increased upon increasing the concentration of monomer and stabilizer and the water content in the tert-butyl alcohol/water media, but it decreased upon increasing both the concentration of initiator and the polymerization temperature.

Topological Analysis on the Dispersion Polymerization of Styrene in Ethanol

  • 손정모;박형석
    • Bulletin of the Korean Chemical Society
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    • v.17 no.3
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    • pp.245-253
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    • 1996
  • A topological theory has been introduced to explain and evaluate the fractional volumes of system materials, the change of the weight and concentration of monomer molecules, molecular weight distribution, and interaction functions of polymer-polymer and polymer-oligomer, etc. for dispersion polymerization. The previous theory of Lu et al. has offered only an incomplete simulation model for dispersion polymer systems, whereas our present one gives a general theoretical model applicable to all the polymerization systems. The theory of Lu et al. considered only the physical property term caused by interaction between matters of low molecular weight (i.e., diluent, monomer, and oligomer) and polymer particles without dealing with physical properties caused by the structure of polymer networks in polymer particles, while our theory deals with all physical effect possible, caused by the displacement of not only entangled points but also junction points in polymer particles. The theoretically predictive values show good agreement with the experimental data for dispersion polymerization systems.

Effect of Parameters on the Particle Size in Dispersion Polymerization of Poly(methy1 methacrylate) (분산중합 변수가 폴리메틸메타크릴레이트의 입자크기에 미치는 영향)

  • Kim, Su-Jin;Wu, Jong-Pyo
    • Journal of the Korean Applied Science and Technology
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    • v.17 no.4
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    • pp.257-261
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    • 2000
  • Monodisperse polymer particles have many industrial applications such as surface coatings for metal panels, chromatographic media, spacers for liquid crystal display panel, and fillers for cosmetics, etc.. Micron-size monodispersed poly(methyl methacrylate) particles were prepared by dispersion polymerization in methanol medium in the presence of poly(vinyl pyrrolidone) and 2,2'-azobis(isobutyronitrile) as steric stabilizer and initiator, respectively. Effects of polymerization parameters, such as monomer and initiator concentration, stabilizer type and concentration, solvent composition on average particle size and size distribution were studied.

In-Situ Synthesis of PS/(-)Silica Composite Particles in Dispersion Polymerization Using An ($\pm$) Amphoteric Initiator

  • Hwang, Deok-Ryul;Hong, Jin-Ho;Lee, Jeong-Woo;Shim, Sang-Eun
    • Macromolecular Research
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    • v.16 no.4
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    • pp.329-336
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    • 2008
  • Core/shell ($\pm$)PS/(-)silica nanocomposite particles were synthesized by dispersion polymerization using an amphoteric initiator, 2,2'-azobis [N-(2-carboxyethyl)-2,2-methylpropionamidine] ($HOOC(CH_2)_2HN$(HN=) $C(CH_3)_2CN$=NC $(CH_3)_2C$(=NH)NH $(CH_2)_2COOH$), VA-057. Negatively charged (-6.9 mV) silica was used as the stabilizer. The effects of silica addition time and silica and initiator concentrations were investigated in terms of polymerization kinetics, ultimate particle morphology, and size/size distribution. Uniform hybrid microspheres with a well-defined, core-shell structure were obtained at the following conditions: silica content = 10-15 wt% to styrene, VA-057 content=above 2 wt% to styrene and silica addition time=0 min after initiation. The delay in silica addition time retarded the polymerization kinetics and broadened the particle size distribution. The rate of polymerization was strongly affected by the silica content: it increased up to 15 wt% silica but then decreased with further increase in silica content. However, the particle size was only marginally influenced by the silica content. The zeta potential of the composite particles slightly decreased with increasing silica content. With increasing VA-057 concentration, the PS microspheres were entirely coated with silica sol above 1.0 wt% initiator.

Dispersion Polymerization of Acrylamide in Ethanol/water Media (에틸 알코올/물 혼합 용매에서 아크릴아미드의 분산 중합)

  • 이기창;이성은;송봉근
    • Polymer(Korea)
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    • v.27 no.4
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    • pp.358-363
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    • 2003
  • Dispersion polymerization of acrylamide was carried out in the media of ethyl alcohol/water mixtures using hydroxypropyl cellulose and ammonium persulfate as steric stabilizer and initiator, respectively. The effects of concentrations of initiator and steric stabilizer, amount of monomer, polymerization temperature, ethyl alcohol/water ratio, and purification of monomer and nitrogen purge on the particle size of the latices and molecular weight of the polymers were investigated. The average particle diameter increased with increasing concentration of initiator, water content in ethyl alcohol/water media, and polymerization temperature, but decreased with monomer and stabilizer concentrations. The viscosity average molecular weight increased with increasing concentrations of monomer, steric stabilizer, and water content in dispersion media, but decreased with initiator concentration and polymerization temperature. The PAM polymers prepared with the purified monomer and the nitrogen purging before the reaction showed the highest molecular weight. In this study, PAM latices of 0.5∼2.4 $\mu\textrm{m}$ with 20000∼335000 in M$\_$v/ were prepared and the resulting PAM latices were all dissolved in water instantly.