• Restorative Dentistry and Endodontics
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• v.42 no.1
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• pp.27-33
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• 2017

Objectives: To determine the optimal timing for post space preparation of root canals sealed with epoxy resin-based AH Plus sealer in terms of its polymerization and influence on apical leakage. Materials and Methods: The epoxy polymerization of AH Plus (Dentsply DeTrey) as a function of time after mixing (8, 24, and 72 hours, and 1 week) was evaluated using Fourier transform infrared (FTIR) spectroscopy and microhardness measurements. The change in the glass transition temperature ($T_g$) of the material with time was also investigated using differential scanning calorimetry (DSC). Fifty extracted human single-rooted premolars were filled with gutta-percha and AH Plus, and randomly separated into five groups (n = 10) based on post space preparation timing (immediately after root canal obturation and 8, 24, and 72 hours, and 1 week after root canal obturation). The extent of apical leakage (mm) of the five groups was compared using a dye leakage test. Each dataset was statistically analyzed by one-way analysis of variance and Tukey's post hoc test (${\alpha}=0.05$). Results: Continuous epoxy polymerization of the material with time was observed. Although the $T_g$ values of the material gradually increased with time, the specimens presented no clear $T_g$ value at 1 week after mixing. When the post space was prepared 1 week after root canal obturation, the leakage was significantly higher than in the other groups (p < 0.05), among which there was no significant difference in leakage. Conclusions: Poor apical seal was detected when post space preparation was delayed until 1 week after root canal obturation.

• Polymer(Korea)
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• v.36 no.1
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• pp.65-70
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• 2012

Glycidyl methacrylate (GMA) was used to introduce epoxy groups on the surface of polypropylene (PP) plate, used as a substrate, through plasma-induced graft copolymerization. Emulsion polymerization was applied for graft copolymerization of GMA and was compared with conventional solution polymerization to confirm its effect. Plasma treatment conditions under one atmospheric pressure were fixed as follows; the RF power of 200 W, the treatment time of 30 sec, the Ar gas flow rate of 6 LPM, and the exposure time of treated PP samples in air of 5 min. For graft-copolymerization, GMA concentration, reaction temperature, and reaction time was optimized to maximize the grafting degree of GMA. The maximum grafting degree of GMA was obtained at the condition of 12%-GMA concentration, $90^{\circ}C$ reaction temperature, and 5 hr-reaction time. Analysis results supported that the emulsion polymerization was more effective than the solution polymerization for grafting more GMAs on the surface of PP plate under the same reaction conditions.

• Elastomers and Composites
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• v.44 no.1
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• pp.55-62
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• 2009

In this study, investigation on the polymerization characteristics of isoprene through nitroxide mediated controlled/"living" radical polymerization techniques was attempted. In the presence of acetol, linear increase of isoprene conversion with time and low polydispersities of the resulting polymers ($M_w/M_n$ < 1.5) were observed, which suggest successful controlled/"living" radical polymerization of isoprene. The microstructure of the resulting polyisoprene was composed of $\sim$ 22% of 3, 4, $\sim$30% of 1, 4-cis and $\sim$ 48% of 1, 4-trans. The optimum polymerization temperature was 145 $^{circ}C$, below which no significant polymerization behavior was observed. Non-cyclic nitroxide, such as di-tert-butyl nitroxide (DTBN) could not mediate the polymerization, whereas cyclic nitroxides (2, 2, 6, 6-tetramethyl-1-peperidine 1-oxyl (TEMPO) and 4-oxo-2, 2, 6, 6-tetramethyl-1-peperidine 1-oxyl (oxoTEMPO)) were successfully employed for the polymerization. However, isoprene dimerization reaction through Diels-Alder process was also observed at the given polymerization condition, which afforded a significant amount of limonene. Isoprene thermal autoinitiation was also possible, which was, however, considered to be not significant under the given polymerization condition.

• Applied Chemistry for Engineering
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• v.20 no.3
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• pp.322-328
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• 2009

Emulsion polymerization of octamethylcyclotetrasiloxane (OMCTS) was conducted under ultrasonic irradiation. Two sources of ultrasound with different intensities and frequencies of 20 KHz and 40 KHz were used for horn and bath type reactor, respectively. A combined process of horn and bath was also investigated. The effectiveness of the reaction systems was investigated by measuring conversion as well as intrinsic viscosity of the products. The influence of reaction temperature and sonication time on the progress of sonochemical polymerization was examined. It was found that conversion of greater than 80% and high viscosity were achieved within a few minutes of sonication in a horn type reactor, however, conversion and viscosity showed maximum values depending upon the sonication time. In a bath type reactor where a relatively weak intensity was maintained, longer duration time of more than one hour of sonication was required to reach a high level of conversion and viscosity. Compared with the horn type system, the conversion and viscosity in the bath type reactor were increased along with the sonication time. When the polymerization was carried out in a combined system of horn and bath, the evolution of conversion and molecular weight was quite different from the other cases. For the given geometry of reaction system, acoustic analysis using a commercial software was carried out and the results were correlated with experimental observation.

• Restorative Dentistry and Endodontics
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• v.33 no.4
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• pp.341-351
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• 2008

This study investigated the effect of intermittent polymerization on the rate of polymerization shrinkage and cuspal deflection in composite resins. The linear polymerization shrinkage of each composite was measured using the custom-made linometer along with the light shutter specially devised to block the light at the previously determined interval. Samples were divided into 4 groups by light curing method; Group 1) continuous light (60s with light on); Group 2) intermittent light (cycles of 3s with 2s light on & 1s with light off for 90s): Group 3) intermittent light (cycles of 2s with 1s light on & 1s with light off for 120s); Group 4) intermittent light (cycles of 3s with 1s light on & 2s with light off for 180s). The amount of linear polymerization shrinkage was measured and its maximum rate (Rmax) and peak time (PT) in the first 15 seconds were calculated. For the measurement of cuspal deflection of teeth, MOD cavities were prepared in 10 extracted maxillary premolars. Reduction in the intercuspal distance was measured by the custom-made cuspal deflection measuring machine. ANOVA analysis was used for the comparison of the light curing groups and t-test was used to determine significant difference between the composite resins. Pyramid showed the greater amount of polymerization shrinkage than Heliomolar (p < 0.05). There was no significant difference in the linear polymerization shrinkage among the groups. The Rmax was group 4 < 3, 2 < 1 in Heliomolar and group 3 < 4 < 2, 1 in Pyramid (p < 0.05). Pyramid demonstrated greater cuspal deflection than Heliomolar. The cuspal deflection in Heliomolar was group 4 < 3 < 2, 1 and group 4, 3 < 2, 1 in Pyramid (p < 0.05). It was concluded that the reduced rate of polymerization shrinkage by intermittent polymerization can help to decrease the cuspal deflection.

• Transactions on Control, Automation and Systems Engineering
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• v.4 no.1
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• pp.62-74
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• 2002

The tracking of a reference temperature trajectory in a polymerization batch reactor is a common problem and has critical importance because the quality control of a batch reactor is usually achieved by implementing the trajectory precisely. In this study, only energy balances around a reactor are considered as a design model for control synthesis, and material balances describing concentration variations of involved components are treated as unknown disturbances, of which the effects appear as time-varying parameters in the design model. For the synthesis of a tracking controller, a method combining the input-output linearization of a time-variant system with the parameter estimation is proposed. The parameter estimation method provides parameter estimates such that the estimated outputs asymptotically follow the measured outputs in a specified way. Since other unknown external disturbances or uncertainties can be lumped into existing parameters or considered as another separate parameters, the method is useful in practices exposed to diverse uncertainties and disturbances, and the designed controller becomes robust. And the design procedure and setting of tuning parameters are simple and clear due to the resulted linear design equations. The performances and the effectiveness of the proposed method are demonstrated via simulation studies.

• 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.

• Journal of the Korean Applied Science and Technology
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• v.6 no.1
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• pp.1-7
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• 1989

To developed new process for obtaining maximum molecular weight of anionic acrylamide and acrylic acid copolymer by inverse emulsion polymerization. Concentration of initiator, reducing agent, surfactant and mole ratio of acrylamide-acrylic acid were studied for the process. Semi-batch processes with method of redox, control of reaction temperature, feeding method of monomer and reaction time, was suitable for maximum molecular weight of P(AMAC) from this process obtained $3.09\;{\time}\;10^6({\bar{M}}n.)$ and $4.41\;{\time}\;10^6({\bar{M}}w.)$ in molecular weight measured by the intrinsic viscosity method. inverse emulsion polymerization mechanism of P(AMAC) does not followed the Smith-Ewart and Medvedev theory, but selected for concentration of initiator, reducing agent, surfactant, water solubility of monomer.

• Journal of the Korea Institute of Military Science and Technology
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• v.12 no.2
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• pp.228-235
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• 2009

We synthesized glycidyl azide monomer(GAM) as a monomer for polymerization of glycidy azide polymer(GAP) which is a promising energetic prepolymer for a plastic-bonded explosive. Using quantitative real-tim in-situ infrared(in-situ IR) spectroscopy, kinetic study on the cationic ring opening polymerization of GAM was carried out. The reaction rate was obtained from monitoring the change of ether C-O stretching band($1050cm^{-1}$) in series IR spectra. The reaction was in accordance with the first-order reaction law for each of reaction temperature at 100/1 mole ratio of [GAM]/[$BF_3*etherate$]. In the ring opening polymerization of GAM, with ratio of [GAM]/[$BF_3*etherate$] to equal 100/1 at various temperature, the activation parameters obtained from the evaluation of kinetic data were ${\Delta}H^*$=14.34kcal/mol, ${\Delta}S^*=-12.31cal/mol{\cdot}K$ and $E_a$=14.89kcal/mol.

• Elastomers and Composites
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• v.48 no.1
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• pp.2-9
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• 2013

We synthesized polyethylene, poly(ethylene-co-1-decene), poly(ethylene-co-p-methylstyrene), and poly(ethylene-ter-1-decene-ter-p-methystyrene) using a rac-$Et(Ind)_2ZrCl_2$ metallocene catalyst and a methylaluminoxane cocatalyst system. The materials were characterized using nuclear magnetic spectroscopy and fourier transform infrared spectroscopy. To identify suitable reaction conditions for terpolymerization, we studied the effects of catalyst content, cocatalyst/catalyst molar ratio, polymerization time, and polymerization temperature. As the catalyst content increased, the catalytic activity and the molecular weight of the terpolymers increased. The catalytic activity sharply increased but little change was observed after a polymerization time of 30 min. The increase in the cocatalyst/catalyst molar ratio resulted in a decrease in the molecular weight of the terpolymers and an increase in the catalytic activity to some degree. The catalytic activity increased with increasing polymerization temperature, while the molecular weight of the terpolymers decreased.