• Title/Summary/Keyword: polymerization time

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Immobilization of Late Transition Metal Catalyst on the Amino-functionalized Silica and Its Norbornene Polymerization (아미노-기능화된 실리카 위 후전이 금속 촉매 담지 및 이를 이용한 노보넨 중합)

  • Pacia, Rose Mardie P.;Kim, So Hui;Lee, Jeong Suk;Ko, Young Soo
    • Applied Chemistry for Engineering
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    • v.27 no.3
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    • pp.313-318
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    • 2016
  • In this study, an amorphous silica was functionalized with aminosilane, N-[(3-trimethoxysilyl)propyl]ethylenediamine (2NS) and the late transition metal catalysts including ($(DME)NiBr_2$ and $PdCl_2$(COD)) were subsequently immobilized on the functionalized amorphous silica for norbornene polymerization. Effects of the polymerization temperature, polymerization time, Al/Ni molar ratio, and type of co-catalyst on norbornene polymerization were investigated. Unsupported late transition metal catalysts did not show any activities for norbornene polymerization. However, the $SiO_2$/2NS/Ni catayst with MAO system, with increasing polymerization temperature, increased the polymerization activity and decreased the molecular weight of the polynorbornene (PNB). Furthermore, the catalyst when increasing polymerization temperature caused the decrease in both the polymerization activity and molecular weight of PNB. This confirmed that the stability of $SiO_2$/2NS/Ni at a high temperature was greater than that of $SiO_2$/2NS/Pd. Also the longer polymerization time resulted in the higher conversion of norbornene for both catalysts. When the Al : Ni molar ratio was 1000 : 1, the highest activity (15.3 kg-PNB/($({\mu}mol-Ni^*hr$)) but lowest molecular weight ($M_n$ = 124,000 g/mol) of PNB were achieved. Also $SiO_2$/2NS/Ni catalyst with borate/TEAL resulted in diminishing the polymerization activity and molecular weight of PNB with increasing the polymerization temperature.

A STUDY ON THE PHYSICAL PROPERTIES OF RESTORATIVE MATERIALS FOR PHOTO-POLYMERIZATION OF ARGON LASER (아르곤 레이저를 이용한 광중합 수복재의 물리적 성질에 관한 연구)

  • Ju, Sang-Ho;Choi, Hyung-Jun;Kim, Seong-Oh;Lee, Jong-Gap
    • Journal of the korean academy of Pediatric Dentistry
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    • v.25 no.2
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    • pp.368-382
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    • 1998
  • The purpose of this study is to evaluate and compare the results of argon laser for 5 seconds, argon laser for 10 seconds, and visible light for 40 seconds photo-polymerization in compressive strength, microhardness, curing depth, temperature rising during polymerization, and polymerization shrinkage. Hybrid type composite resin(Z-100) and compomer(Dyract) were used to be compared. The compressive strength was measured by an Instron(1mm/min cross head speed) in 60 specimens and the microhardness of the surface was expressed by Vickers Hardness Number(VHN) in 30 specimens. The curing depth was evaluated comparing the different values of upper and lower VHN according to irradiation time and thickness for the light source polymerization in 60 specimens. The temperature rising during photopolymerization was observed by the temperature change with thermocouple sensitizer beneath 40 specimens at the argon laser for 10 seconds and visible light 40 seconds irradiation. The polymerization shinkage was evaluated by calculating the decrease of % volume by using a dilatometer in 30 specimens. The results were as follows ; 1. In the case of compressive strength, the argon laser polymerization groups were higher than visible light group in Z-100 (p<0.05). In Dyract, the argon laser 5 seconds group did not show a significant difference with the visible light 40 seconds group. The argon laser 10 seconds group showed the markedly low value when compared with other groups (p<0.05) 2. In microhardness, Z-100 was better than Dyract when comparing by VHNs (p<0.05); however, there was not a significant difference between two materials in the visible light 40 seconds group and the argon laser 10 seconds group. 3. In the study of curing depth, Z-100 showed the consistent polymerization in argon laser irradiation because there was no difference in the VHN decrease according to the thickness change. Over the thickness control, the results did not show a significant difference between visible light and argon laser group in Z-100; however, in the case of Dyract, the visible light 40 seconds group was better than the argon laser groups(p<0.05). 4. There was a significant difference between the two materials in temperature rising during polymerization (p<0.05), but not a significant difference between irradiation times, 5. There was not a significant difference between the two materials in polymerization shrink age. The argon laser 5 seconds group was smaller than the other groups (p<0.05). It could be concluded that Z-100 polymerization was recommended to use the argon laser for reduction of the irradiation time while Dyract was recommended to use the visible light polymerization.

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Study for Reducement of Polymerization Time and Improvement of Stability in Manufacturing Carboxylated Styrene-butadiene Latex (카르복실화 스티렌-부타디엔 라텍스의 중합시간 단축과 안정성 개선을 위한 연구)

  • Cho, Ur-Ryong
    • Elastomers and Composites
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    • v.37 no.1
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    • pp.31-38
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    • 2002
  • Polymerization of carboxylated styrene-butadiene latex takes longer time than that of acrylic emulsion due to delocalization of radical in butadiene unit having conjugated double bond. A latex stability is the most important properties owing to use intact without separating polymer from base latex. For reducing polymerization time without decreasing any properties of latex, carbon tetra-chloride which has been used as the most popular chain transfer agent was replaced to combination of tert-dodecylmercaptane and ${\alpha}$-methylstyrene dimer. The replacement yielded reducement or 2 hr in polymerization time. In the increment step, charge amount of acrylic acid was limited to 0.3 part to restrain viscosity enhancement. Just after initial step, addition of 0.1 part acrylamide prevent polymer chain from diffusing between two region followed by giving hardness and final good adhesive force to latex particles.

Comparison of Surface Microhardness of the Flowable Bulk-Fill Resin and the Packable Bulk-Fill Resin according to Light Curing Time and Distance

  • Hyung-Min Kim;Moon-Jin Jeong;Hee-Jung Lim;Do-Seon Lim
    • Journal of dental hygiene science
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    • v.23 no.2
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    • pp.123-131
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    • 2023
  • Background: As a restorative material used to treat dental caries, the light-curing type resin is widely used, but it has the disadvantage of polymerization shrinkage. The Bulk-Fill composite resin was developed to solve these shortcomings, but the existing research mainly focused on comparing the physical properties of a composite resin and a Bulk-Fill resin. A study on the light curing time and distance of the Bulk-Fill resin itself tend to be lacking. Methods: This study compares the surface microhardness of specimens prepared by varying the light curing time and distance of smart dentin replacement (SDR) as a flowable Bulk-Fill resin and Tetric N-ceram as a packable Bulk-Fill resin, and confirms the polymerization time and distance that becomes the optimum hardness. To determine the hardness of the specimen, it was measured using the Vickers Hardness Number (Matsuzawa MMT-X, Japan). Results: In SDR, the surface microhardness decreased as the distance increased in all time groups in the change distance from the curing tip. In the change of light curing time with respect to the distance from curing tip, the surface microhardness increased as the time increased. In Tetric N-ceram, the surface microharness showed no significant difference in the change of the distance of curing tip in the group of 20 and 60 second. But in the group of 10 and 40 seconds, decreased as the distance increased. The surface microharness increased as the light curing time increased in all distance groups. Conclusion: When using SDR and Tetric N-ceram in clinical practice, it is considered that as the distance from the polymerization reactor tip increases, a longer light curing time than the polymerization time recommended by the manufacturer is required.

Synthesis and Performance Evaluation of Linear Polycarboxylate Dispersant of Glacial Acrylic Acid - Maleic Acid- Sodium Methallyl Disulfonate for Ceramics

  • Kommanapalli, Kiran Kumar;Lyot, Pierre;Sunkara, Jhansi Rani;Checule, Pierrick
    • Journal of the Korean Ceramic Society
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    • v.55 no.2
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    • pp.126-134
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    • 2018
  • Using aqueous solution free radical polymerization with glacial acrylic acid (GAA), maleic anhydride (MA) and sodium methallyl disulfonate (SMADS), a novel linear polycarboxylate dispersant was synthesized for ceramics. Dispersant linear structural characterization was done by FTIR, $^1H$ NMR, HPLC and GPC, and the ratio of monomers was determined using an orthogonal experiment. This research is focused on the effects of polymerization temperature, monomer mole ratios and dosage of initiator on ceramic slurry viscosity with linear polycarboxylate dispersant for ceramic dosage rate of 0.30% (based on dry slurry), all of which were investigated by single factor test. The best polymerization conditions for linear GAA-MA-SMADS are when n(AA) : n(MA) : n(SMADS) equals 3.0 : 1.0 : 0.5, the molecular weight of the polymer is 4600 daltons, the initiator sodium persulfate accounts for 7% of the total mass of polymerized monomers, the polymerization temperature is $90^{\circ}C$ and the reaction time is 2 h. The ceramic body slurry viscosity drops from $820mPa{\cdot}s$ to $46mPa{\cdot}s$ when the concentration of the polycarboxylate dispersant is 0.30%.

Preparation of Honeycomb-patterned Polyaniline-MWCNT/Polystyrene Composite Film and Studies on DC Conductivity

  • Kim, Won-Jung;Huh, Do-Sung
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2345-2351
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    • 2012
  • Conductive honeycomb-patterned polystyrene (PS) thin films were prepared by the formation of a polyaniline (PANI) thin layer on the surface of the patterned PS thin films using simple one-step chemical oxidative polymerization of aniline. The in situ chemical oxidation polymerization of aniline hydrochloride solution on the patterned structure of the PS films was conducted in the presence of multiwalled carbon nanotubes (MWCNT) to prepare the PANI-MWCNT/PS composite film. The concentration (wt %) of MWCNT was varied in the range of 1%-3% by weight. The dependence of surface morphology of the PANI/PS and PANI-MWCNT/PS composite film to the polymerization time was observed by scanning electron microscopy. The room temperature DC conductivity was obtained by the four-probe technique. The conductivity of the PANI-MWCNT/PS composite film was affected both by the MWCNT concentration and polymerization time. In addition, DC electrical field was loaded during the oxidative polymerization to affect the distribution of the MWCNT included in the composite film, varying the loading voltage in the range of 0.1-3.0 V. The conductivity of the PANI-MWCNT/PS composite film was increased as loading voltage rose. However, this increase stops at a voltage higher than the critical value.

Fabrication and Processing Method of Ophthalmic Hydrogel Tinted Lens Containing Indium Tin Oxide-Composited Materials

  • Lee, Min-Jae;Lee, Kyung-Mun;Sung, A-Young
    • Korean Journal of Materials Research
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    • v.28 no.12
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    • pp.685-690
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    • 2018
  • In this study, a multifunctional ophthalmic lens material with an electromagnetic shielding effect, high oxygen permeability, and high water content is tested, and its applicability is evaluated. Metal oxide nanoparticles are applied to the ophthalmic lens material for vision correction to shield harmful electromagnetic waves; the pyridine group is used to improve the antibacterial effect; and silicone substituted with urethane and acrylate is employed to increase the oxygen permeability and water content. In addition, multifunctional tinted ophthalmic lens materials are studied using lens materials with an excellent antibacterial effect (2,6-difluoropyridine, 2-fluoro-4-pyridinecarboxylic acid) and functional (UV protection, high wettability) lens materials (2,4-dihydroxy benzophenone, 2-hydroxy-4-(methacryloyloxy)benzophenone). To solve problems such as air bubbles generated during the polymerization process for the manufacturing and turbidity of the lens surface, polymerization conditions in which the defect rate is minimized are determined. The results show that the polymerization temperature and time are most appropriate when they are $110^{\circ}C$ and 40 minutes, respectively. The optimum injection amount of the polymerization solution is 350 ms. The turbid phenomenon that appears in lens processing is improved by 10 to 95 % according to the test time and conditions.

THE EFFECT OF MONOMER TO POWDER RATIO ON POLYMERIZATION SHRINKAGE-STRAIN KINETICS OF POLYMER-BASED PROVISIONAL CROWN AND FIXED PARTIAL DENTURE MATERIALS

  • Kim, Sung-Hun
    • The Journal of Korean Academy of Prosthodontics
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    • v.45 no.6
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    • pp.735-742
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    • 2007
  • Statement of problem. Although a number of previous investigations have been carried out on the polymerization shrinkage-strain kinetics of provisional crown and fixed partial denture (FPD) materials, the effect of the changes of liquid monomer to powder ratio on its polymerization shrinkage-strain kinetics has not been reported. Purpose. The purpose of this study was to investigate the influence of liquid monomer to powder ratio of polymer-based provisional crown and FPD materials on the polymerization shrinkage-strain kinetics. Material and methods. Chemically activated acrylic provisional materials (Alike, Jet, Snap) were investigated. Each material was mixed with different liquid monomer to powder ratios by volume (1.0:3.0, 1.0:2.5, 1.0:2.0, 1.0:1.5, 1.0:1.0). Time dependent polymerization shrinkage- strain kinetics of all materials was measured by the bonded-disk method as a function of time at $23^{\circ}C$. Five recordings were taken for each ratio. The results were statistically analyzed using one-way ANOVA and the multiple comparison Scheffe test at the significance level of 0.05. Trends were also examined by linear regression. Results. At 5 minutes after mixing, the polymerization shrinkage-strains of all materials ranged from only 0.01% to 0.49%. At 10 minutes, the shrinkage-strain of Alike was the highest, 3.45% (liquid monomer to powder ratio=1.0:3.0). Jet and Snap were 2.69% (1.0:2.0) and 1.58% (1.0:3.0), respectively (P>0.05). Most shrinkage (94.3%-96.5%) occurred at 30 minutes after mixing for liquid monomer to powder ratio, ranging from 1.0:3.0 to 1.0:1.0. The highest polymerization shrinkage-strain values were observed for the liquid monomer to powder ratio of 1.0:3.0. At 120 minutes after mixing, the shrinkage-strain values were 4.67%, 4.18%, and 3.07% for Jet, Alike, and Snap, respectively. As the liquid monomer to powder ratio increased, the shrinkage-strain values tend to be decreased linearly (r=-0.769 for Alike, -0.717 for Jet, -0.435 for Snap, $r^2=0.592$ for Alike, 0.515 for Jet, 0.189 for Snap; P<0.05). Conclusion. The increase of the liquid monomer to powder ratio from 1.0:3.0 to 1.0:1.0 had a significant effect on the shrinkage-strain kinetics of polymer-based crown and FPD materials investigated. This increased the working time and decreased the shrinkage-strain during polymerization.

Physical property control for a batch polymerization reactor

  • Kim, In-Sun;Ahn, Sung-Mo;Rhee, Hyun-Ku
    • 제어로봇시스템학회:학술대회논문집
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    • 1996.10a
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    • pp.263-266
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    • 1996
  • A method to determine an optimal temperature trajectory that guarantees polymer products having controlled molecular weight distribution and desired values of molecular weight is presented. The coordinate transformation method and the optimal control theory are applied to a batch PMMA polymerization system to calculate the optimal temperature trajectory. Coordinate transformation method converts the original fixed-end-point, free-end-time problem to a free-end-point, fixed-end-time problem. The idea is that by making the reactor temperature track the optimal temperature trajectory one may be able to produce polymer products having the prespecified physical property in a minimum time. The on-line control experiments with the PID control algorithm have been conducted to establish the validity of the scheme proposed in this study. The experimental results show that prespecified polymer product could be obtained with tracking the calculated optimal temperature trajectory.

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Estimating Diffusion-Controlled Reaction Parameters in Photoinitiated Polymerization of Dimethacrylate Macromonomers

  • Choe, Youngson
    • Macromolecular Research
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    • v.11 no.5
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    • pp.311-316
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    • 2003
  • The kinetics of photoinitiated polymerization of dimethacrylate macromonomers have been studied to determine the diffusion-controlled reaction parameters using attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). A predicted kinetic rate expression with a diffusion control factor was employed to estimate an effective rate constant and to define the reaction-controlled and diffusion-controlled regimes in the photopolymerization. An effective rate constant, k$_{e}$, can be obtained from the predicted kinetic rate expression. At the earlier stages of polymerization, the average values of kinetic rate constants do not vary during the reaction time. As the reaction conversion, $\alpha$, reaches the critical conversion, $\alpha$$_{c}$, in the predicted kinetic expression, the reaction becomes to be controlled by diffusion due to the restricted mobility of dimethacrylate macromonomers. A drop in value of effective rate constant causes a drastic decrease of reaction rate at the later stages of polymerization. By determining the effective rate constants, the reaction-controlled and diffusion-controlled regimes were properly defined even in the photopolymerization reaction system.m.m.