• 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.

• Bulletin of the Korean Chemical Society
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• v.30 no.3
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• pp.722-725
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• 2009

• Bulletin of the Korean Chemical Society
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• v.30 no.12
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• pp.3127-3130
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• 2009

• Elastomers and Composites
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• v.43 no.3
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• pp.157-165
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• 2008

Suspension polymerization was carried out to synthesize poly(butyl methacrylate) (PBMA) composite particles containing carbon black. Water was selected as a reaction medium, hydrophobic silica as a stabilizer and azobisisobutyronitrile as an initiator. Concentration of stabilizer was varied from 0.67 to 2.55 weight% with respect to the water, and that of initiator was varied from 0.25 to 3.00 weight% with respect to the butyl methacrylate (BMA) monomer. All polymerization reactions were conducted at 75$^{\circ}C$. It is found that stabilizer concentration has no impact on reaction kinetics, while an increase in initiator concentration enhances polymerization reaction rate. Increase of carbon black concentration from 1 to 3 to 5 wt% into PBMA displayed progressive decrease in reaction conversion. The particle diameter of PBMA composite particles containing carbon black was found to be between 5 and 30 ${\mu}m$. Glass transition was determined to range from 23.8 to 24.7$^{\circ}C$, irrespective of variation in the concentration of stabilizer, initiator or carbon black.

• Elastomers and Composites
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• v.47 no.1
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• pp.43-53
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• 2012

A suspension copolymerization of styrene and butyl methacrylate (BMA) in the aqueous phase was conducted at a selected temperature between 65 and $95^{\circ}C$. Hydrophobic silica was selected as a stabilizer and azobisisobutyronitrile (AIBN) as an initiator. Optimum dispersion of silica in water was obtained at pH 10 while polymerization reaction was run at pH 7. TGA and EDS measurements revealed that 90% of silica functioned as a stabilizer and 10% were incorporated into polymeric particles. Average particle diameter decreased with increasing amounts of stabilizer. Molecular weights displayed an increase when the stabilizer concentration reached 1.67 wt%. An increase in the initiator concentration and/or reaction temperature raised the reaction rate but decreased molecular weights. Particle diameter was nearly independent of the initiator concentration and reaction temperature. An increase in the BMA proportion decreased the glass transition temperature and increased the particle diameter with irregularity in shape. Incorporation of carbon black into the particles composed of styrene and BMA prolonged the reaction time before reaching completion. We have confirmed that a suspension copolymerization of styrene and BMA with hydrophobic silica as a stabilizer can produce spherical composite particles with $1-30{\mu}m$ in diameter containing carbon black.

• Bulletin of the Korean Chemical Society
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• v.31 no.10
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• pp.2943-2948
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• 2010

Silica monolith powders were prepared by a new procedure where ground powders of proper size distribution were obtained without sieving. An initiator was attached to this ground monolith and polystyrene was bound by reversible addition-fragmentation chain transfer polymerization to give a new stationary phase. The separation efficiency of this phase was found better than that of the polystyrene bound phase based on conventional silica particles and that of the C18 bound silica monolith powders.

• Applied Chemistry for Engineering
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• v.21 no.3
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• pp.353-355
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• 2010

Poly(methyl methacrylate) (PMMA) particles were prepared by soap-free emulsion polymerization of MMA in the presence of a cationic initiator, 2,2'-azobis(2-methylpropionamidine) (AIBA). The Stober method has been adopted to coat silica on the surface of these cationic particles. Negatively charged silica precursors were coated onto cationic particle surfaces by electronic interaction. During the coating process, hollow particles were directly obtained by dissolution of PMMA.

• Polymer(Korea)
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• v.30 no.6
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• pp.498-504
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• 2006

A suspension polymerization of styrene In aqueous phase was employed to study if polystyrene particles ranging from 1 to $20{\mu}m$ can be produced. Hydrophobic silica was selected as a stabilizer and azo-bisisobutyronitrile (AIBN) as an initiator. Polymerization reaction was carried out at a selected temperature in the range of $65{\sim}95^{\circ}C$. Stabilizer concentration was varied from 0.17 to 3.33 wt% compared to the water while the concentration of the initiator was raised from 0.13 to 6.0 wt% compared to the monomer. Dispersion of hydrophobic silica into the water phase was achieved by precise control of pH. Optimum dispersion of silica was obtained at pH 10. Average particle diameter decreased with increasing amounts of stabilizer concentration initially, exhibiting the minimum average diameter at 1.67 wt% of stabilizer concentration, after which it started to Increase. It is speculated that an excessive presence of stabilizer encouraged a secondary reaction in the reaction medium, which led to particle agglomeration, and as a result an increase in average particle diameter. Molecular weight was found to be independent of stabilizer concentration between 0.13 and 1.00 wt% whereas, it increased when stabilizer concentration exceeded 1.67 wt%. Variation of molecular weight was probably caused by the reduced activity and efficiency of initiator due to the high concentration of silica, and the secondary reaction in the reaction medium, as well. An increase in the Initiator concentration and/or reaction temperature resulted in an increase in both reaction rate and particle diameter. Consequently, we have confirmed that spherical polystyrene particles with $1{\sim}20{\mu}m$ in diameter can be prepared by careful selection of the concentration of stabilizer, initiator, pH and reaction temperature.

• Polymer(Korea)
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• v.33 no.5
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• pp.477-484
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• 2009

Suspension polymerization with hydrophobic silica as a stabilizer and AIBN as an initiator was conducted to synthesize PBMA particles and PBMA composite particles containing carbon black. Surface modification of silica particles by controlling pH revealed that 90% of them functioned as stabilizer and 10% were incorporated into PBMA particles. While stabilizer concentration had no impact on reaction kinetics and particle diameter, an increase in stabilizer concentration displayed an increase in molecular weights when it exceeded 1.67 wt%. An increase in initiator concentration and reaction temperature decreased molecular weights in close agreement with the theoretical equation. An increase in carbon black concentration from 1 to 7 wt%, relative to the monomer, showed a progressive decrease in reaction conversion. As carbon black was increased from 3 to 5 wt%, glass transition showed a $4^{\circ}C$ increase. The presence of carbon black was confirmed by TEM while its concentration was measured by TGA.

• Applied Chemistry for Engineering
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• v.21 no.1
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• pp.34-39
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• 2010

Methacryloxypropyltrimethoxysilane (MPTMS) was used for the surface modification of silica nanoparticles in the toluene dispersion system for 8 h (MPSN). Then, methacryloxypropyl-modified silica nanoparticles were successfully prepared by solutioun polymerization in the ethanol solution at $60^{\circ}C$ for 14 h with adding AIBN initiator. The modification of ultra-fine particles (SiOx-PAA nanospheres) was investigated via EA, XPS, FTIR, TGA, SEM and TEM. The mean diameter of the bare silica nanoparticles, MPSN and SiOx-PAA monodisperse nanoparticles was about 25, 30 and 35 nm, respectively.