• 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.

• Restorative Dentistry and Endodontics
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• v.27 no.2
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• pp.135-141
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• 2002

Objectives : The aim of this study is to evaluate the effect of light intensity variation on the polymerization rate of composite resin using IB system (the experimental equipment designed by Dr. IB Lee) by which real-time volumetric change of composite can be measured. Methods : Three commercial composite resins [Z100(Z1), AeliteFil(AF), SureFil(SF)] were photopolymerized with Variable Intensity Polymerizer unit (Bisco, U.S.A.) under the variable light intensity (75/150/225/300/375/450mW$^2$) during 20 sec. Polymerization shrinkage of samples was detected continuously by IB system during 110 sec and the rate of polymerization shrinkage was obtained by its shrinkage data. Peak time(P.T.) showing the maximum rate of polymerization shrinkage was used to compare the polymerization rate. Results : Peak time decreased with increasing light intensity(p<0.05). Maximum rate of polymerization shrinkage increased with increasing light intensity(p<0.05). Statistical analysis revealed a significant positive correlation between peak time and inverse square root of the light intensity (AF:R=0.965, Zl:R=0.974, SF:R=0.927). Statistical analysis revealed a significant negative correlation between the maximum rate of polymerization shrinkage and peak time(AF:R=-0.933, Zl:R=-0.892, SF:R=-0.883), and a significant positive correlation between the maximum rate of polymerization shrinkage and square root of the light intensity (AF:R=0.988, Zl:R=0.974, SF:R=0.946). Discussion and Conclusions : The polymerization rate of composite resins used in this study was proportional to the square root of light intensity Maximum rate of polymerization shrinkage as well as peak time can be used to compare the polymerization rate. Real-time volume method using IB system can be a simple alternative method to obtain the polymerization rate of composite resins.

• Textile Coloration and Finishing
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• v.7 no.1
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• pp.43-50
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• 1995

The grafting of methacrylonitrile(MAN) onto Kevlar 49 filament surface was carried out by anionic polymerization using sodium methylsulfinylcarbanion formed from sodium hydride and dimethyl sulfoxide(DMSO). The effects of reaction conditions on the grafting percentage(GP) and on the tensile strength of the fiber were investgated. GP marktedly increased with increasing metalation time, and NaH concentration, polymerization temperature and time. The tensile strength of fiber decrased with increasing metalation time, and NaH concentration, polymerization temperature and time. The optimum conditions to increase over 40% of GP with below 10% reduction rate of tensile strength of fiber : NaH concentration ; 30.6 mmol/l/0.5g Kevlar, metalation time : 10min, polymerization tempera- ture : 5$0^{\circ}C$, polymerization time: 20 sec, monomer concentration : 1.12mol/l/0.5g Kevlar.

• Polymer(Korea)
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• v.39 no.3
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• pp.365-369
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• 2015

In this study, the bulk and solution polymerizations of L-lactide using an aluminium compound, methylaluminoxane (MAO), were performed. In the bulk polymerization, the conversion of polymerization was increased with increasing the amount of catalyst in feed. The largest molecular weight (Mw), 60800 g/mol, was shown at the MAO amount in feed of 0.15 mmol, and Mw was decreased above 0.15 mmol of MAO in feed. At the 0.15 mmol of MAO in feed, turn of frequency (TOF) was the highest, and it was decreased with increasing MAO amount in feed. In the solution polymerization, the induction time of 30 min was shown. The conversion of polymerization was linearly increased with the polymerization time, and the highest Mw, 54700 g/mol, was achieved at the polymerization time of 6 h.

• Restorative Dentistry and Endodontics
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• v.26 no.2
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• pp.134-140
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• 2001

The polymerization shrinkage of composite resins is an important drawback although the composites have many advantages-more esthetic and conservative than metallic restoratives etc. The purposes of this research were to develop a new measurement method and to manufacture an instrument that can measure the initial dynamic volumetric shrinkage of composite resins during polymerization. The instrument was basically an electromagnetic balance that constructed with a force transducer using position sensitive photo detector(PSPD) and a negative feedback servo amplifier of proportional-derivative(PD) controller. The volumetric change of composites during polymerization was detected continuously as buoyancy change in distilled water by means of Archimedes's principle. It was converted to continuous electrical voltage signal in real time. The signal was properly conditioned and filtered and then it was stored in computer by a data acquisition(DAQ) board. By using this electronic instrument. the dynamic patterns of the polymerization shrinkage of eight commercial(Z-100, DenFil, AeliteFil, Z-250, P-60, SureFil, Synergy compact, and Tetric ceram) composite resins were measured and compared. The results were as follows. 1. From this project of developing instrument, the ability has been achieved that can acquire and process data of electrical signal transformed from various physical phenomenon by using temperature, displacement. photo. and force transducer. As a consequence, the instrumentation and measurement system used to analyze the physical characteristics of various dental materials in dental research field can be designed, manufactured and implemented in lab. 2. This instrument has some advantages. It was insensible to temperature change and could measure true dynamic volumetric shrinkage in real time without complicated process. It showed accuracy and high precision results with small standard deviation. 3. The polymerization shrinkage of composites was significantly different between brands and ranged from 2.47％ to 3.89％, The order of polymerization shrinkage was as follows, in order of increasing shrinkage, SureFil, P60, Z250, Z100, Synergy compact. DenFil, Tetric ceram, and AeliteFil. 4. The polymerization shrinkage rate per unit time, dVol％/dt, showed that the instrument can provide an indirect research method for polymerization reaction kinetics.

• Restorative Dentistry and Endodontics
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• v.10 no.1
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• pp.145-152
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• 1984

The purpose of this study was to compare combinations of the four visible light irradiating appliances (Translux, Heliomat, Pluraflex HL 150, Omega) and the four visible light activated composite resins (Durafil, Heliosit, Plurafil-super, Silux) to determine the depth of polymerization of each combination. Twenty samples were made with Durafil. Five samples were polymerized for 20 seconds using Translux, five with Heliomat, five with Pluraflex HL 150, five with Omega. Twenty samples were made with Heliosit, twenty with Plurafil-super, and twenty samples with Silux. A 20-second polymerization time was applied with each of 4 visible light irradiating appliances to 5 samples of each material. Eighty samples were treated in a like manner, but polymerization was extended to 40 seconds. Depth of polymerization were measured with caliper. The results were as follows. 1) Of the two time exposures, 40-second exposure provided a significantly greater depth of polymerization than 20-second for each light with each material. 2) Durafill-Translux system showed minimum depth of polymerization, and Plurafil-Pluraflex system showed maximum depth of polymerization. 3) Visible light irradiating appliances were able to harden the resins cured by tire visible lights of other makers' apparatuses. 4) In all circumstances, depth of polymerization was between 3.0-3.8mm.

• Journal of the Korean Society of Clothing and Textiles
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• v.13 no.1 s.29
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• pp.89-97
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• 1989

Graft polymerization of MMA onto cotton fiber was carried out in two ways, two step graft polymerization and one step emulsion graft polymerization, using tetravalent cerium ion as an initiator. At two step graft polymerization, the first step was the pretreatment of cotton fiber with an aqueous initiator solution and the second was the grafting pretreated cotton fiber in the monomer solution. In case of one step emulsion graft polymerization, MMA was emulsified with SLS in initiator solution. Under the various graft polymerization conditions, graft yield, graft efficiency and from the Arrhenius plot the apparent activation energy were compared. The results of this study were as follows: 1. Graft yield and graft efficiency of emulsion graft polymerization were higher than those of two step graft polymerization. 2. In case of two step graft polymerization, graft yield was affected by the pretreatment time of cotton fiber with an aqueous initiator solution. And graft yield of emulsion graft polymerization was increased with the concentration of emulsifier below cmc of SLS and was decreased thereafter. 3. Elevation of temperature resulted increase in graft yield for both grafting methods. The apparent activation energy of emulsion graft pelymerzation was lower than that of two step graft polymerization. 4. Increased reaction time increased in graft yield, but decreased in graft efficiency. 5. Moisture regain of grafted cotton was decreased with graft yield.

• Korean Chemical Engineering Research
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• v.49 no.5
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• pp.676-680
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• 2011

Investigated was the effect of the crucial polymerization conditions such as methyl acrylate(MA) mole fraction in feed, polymerization temperature and time on Atom Radical Transfer Polymerization(ATRP) behavior of styrene and methyl acrylate(MA). As MA mole fraction in feed increased, molecular weight(MW) of the resulting copolymer increased. At polymerization time of 3 hrs the composition of MA in the resulting copolymer was shown to have a linear relationship with the mole fraction of MA in feed. MW was increased and the composition of MA in copolymer was decreased as the polymerization time increased, showing the characteristics of ATRP. MW was also increased as polymerization temperature increased, and the composition of MA in copolymer was shown to be increased drastically at polymerization temperature of $110^{\circ}C$.

• Journal of Industrial and Engineering Chemistry
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• v.68
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• pp.1-5
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• 2018

In this study, we designed and synthesized novel thermal radical initiators of BTAP (1-phenyl-3,3-dipropyltriazene), BTACP (1-(phenyldiazenyl)pyrrolidine), BTACH (1-(phenyldiazenyl)piperidine), and BTACH7 (1-(phenyldiazenyl)azepane) based on a triazene moiety to provide a thermal initiator for radical polymerization. The synthetic method is valuable due to the simplicity. In addition, the synthesized thermal initiator did not affect the color of the polymer. Among the four initiators, the polymerization time for the BTACH of the 6-membered ring decreased by 67%, as opposed to the polymerization time without initiator. Conversion after polymerization was over 92%. DSC experiments also showed that the initiator with hexagonal rings had the lowest peak polymerization temperature of $160^{\circ}C$. Our study suggests a promising new initiator system that is effective for radical polymerization.

• Journal of Technologic Dentistry
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• v.35 no.2
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• pp.127-136
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• 2013

Purpose: In order to find out the impact of changes in polymerization conditions of orthodontic acrylic resin on maximum load. Methods: While maintaining mixing ratio 3:1 of polymer and monomer in spray-on way in the production condition of polymerization temperature $25^{\circ}C$ or $37^{\circ}C$ for 10 minutes or 30 minutes of polymerization time by pressure $3kfg/cm^2$ or $6kfg/cm^2$ in the lab maintaining $25^{\circ}C$ of room temperature, the change in maximum load rise rate was tested by producing 5 acrylic resin specimens for orthodontics per group to meet the standards of $25mm{\times}2mm{\times}2mm$ and using INSTRON with the 3rd bar 2mm in diameter and parallel support bending device of $15{\pm}0.1mm$ as test equipment showing 30.00mm/min of crosshead speed, $50{\pm}16$ N/min of load ratio in the laboratory of $24^{\circ}C$ room temperature and as a result, the following results were obtained. Results: 1. When increasing pressure from $3kfg/cm^2$ to $6kfg/cm^2$, maximum load was lowered by -4.285%. 2. When increasing polymerization time from 10 minutes to 30 minutes, maximum load rose by 3.848%. 3. When increasing polymerization temperature from $27^{\circ}C$ to $37^{\circ}C$, maximum load rose by 5.854%. Conclusion: Considering the above test results that polymerization time and polymerization temperature when polymerizing acrylic resin for orthodontics according to changes in working conditions had an impact on the rate of rise of maximum load values but the rate of rise was lowered when increasing pressure from $3kfg/cm^2$ to $6kfg/cm^2$, we came to a conclusion that high pressure more than necessary does not affect the rate of rise of maximum load.