• Title/Summary/Keyword: Bulk polymerization

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Ring-Opening Polymerization of L-lactide with Glycidol as Initiator (Glycidol을 개시제로 이용한 L-lactide 개환중합)

  • Yim, Jin-Heong;Kim, Da Hee;Ko, Young Soo
    • Polymer(Korea)
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    • v.37 no.5
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    • pp.606-612
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    • 2013
  • Glycidol-poly(lactide) (Gly-PLA) were synthesized via L-lactide ring opening polymerization with glycidol as an initiator and $Al(O-i-Pr)_3$ catalyst. The structure of Gly-PLA was analyzed and successfully confirmed by 1H NMR. The OH group of glycidol in Gly-PLA was absent according to the $^1H$ NMR analysis, indicating that the terminal OH group of glycidol successfully served as an initiator in the L-lactide polymerization. The solution and bulk polymerizations of L-lactide with glycidol were performed to examine the effect of L-lactide/glycidol molar ratio, polymerization temperature and time on the molecular characteristics of Gly-PLA. The conversion and molecular weight increased with an increase in L-lactide/glycidol molar ratio. Gly-PLA showed the bimodal type DSC curve. The low $T_m$ peak of low molecular weight reduced but the high $T_m$ peak of high molecular weight increased as L-lactide/glycidol molar ratio increased.

Characterization of Poly(ether-block-amide)s Prepared from Oligomeric Polyamide 12 via Dispersion Polymerization (분산중합에 의한 폴리아미드 12 올리고머의 제조와 그를 이용한 Poly(ether-block-amide)의 특성)

  • Kim, Doo-Hyeon;Lee, Ji-Hun;Kim, Hyung-Joong
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.513-518
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    • 2012
  • Polyamide 12 (PA12) oligomers (oPA1) were prepared by dispersion polymerization of ${\omega}$-amino carboxylic acid and dibasic acid in a dispersion medium, thermally stable hydrocarbon liquid paraffin, YK-D130 (a step polymerization). The molecular weight and various properties of other oligomeric PAs (oPA2) obtained by bulk polymerization without the medium were compared with those of oPA1s. The oPA1s showed lighter white color and narrower molecular weight distribution than oPA2s at the same molecular weight. Moreover elastomeric poly(ether-block-amide) (PEBA)s were synthesized with oPA1 and oPA2 as hard segments and poly(tetramethylene glycol) (PTMG) as a soft segment. The molecular weight distribution, and mechanical property of the PEBA originated from the both oligomeric PAs were characterized.

THE EFFECT OF POLYMERIZATION TECHNIQUES ON THE MICROLEAKAGE OF COMPOMER (광중합방식이 콤포머의 변연폐쇄에 미치는 영향)

  • 조옥환;한진순;임미경;이수종
    • Restorative Dentistry and Endodontics
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    • v.26 no.1
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    • pp.32-40
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    • 2001
  • The aim of this study was to evaluate the effect of various polymerization techniques on the microleakage of compomer restorations. Fifty extracted human premolars and molar were used and randomly divided into 5 groups. After cavity preparation, compomer (F2000$^{\circledR}$) was filled according to the manufacturer's directions. All groups, except group 5, were filled using an incremental technique. Group 1 was polymerized for 40 seconds at a continuous 485mW/$\textrm{cm}^2$ with a VIP$^{\circledR}$(Bisco, USA) light cure unit. Group 2 was polymerized for 20 seconds at 345mW/$\textrm{cm}^2$ and then for 20 seconds at 645mW/$\textrm{cm}^2$ with the VIP equation omitted light cure unit. Group 3 was polymerized at 400mW/$\textrm{cm}^2$, gradually increased to 50mW/$\textrm{cm}^2$ 10 seconds until 550mW/$\textrm{cm}^2$ was reached; total 40 seconds with a Spectrum 800$^{\circledR}$ (Dentsply Caulk, USA) light cure unit. Group 4 was polymerized for 3 seconds using an incremental technique with a Flipo$^{\circledR}$ (LOKKi, France) light cure unit. Group 5 was polymerized for 3 seconds using a bulk fill technique with the Flipo$^{\circledR}$ light cure unit. The specimens were embedded with acrylic resin, and were sectioned with diamond saws in a mesiodistal direction along the longitudinal axis of the tooth so as to pass through the center of the restoration, and three surfaces (occlusal, pulpal, and gingival) were examined with SEM. The results were as follows ; 1. Group 5 showed a significantly larger gaps compared to other groups on the gingival, occlusal, and pulpal walls. 2. All groups except group 5 had no statistically significant gap on the gingival, occlusal, and pulpal walls. 3. There was no significant correlation between the amount of enamel on the gingival and occlusal walls and polymerization shrinkage.

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Evaluation of marginal leakage of bulk fill flowable composite resin filling with different curing time using micro-computed tomography technology (Bulk fill 유동성 복합레진의 변연 누출에서 다른 중합시간의 영향에 대해 마이크로시티를 이용한 평가)

  • Kim, Eun-Ji;Lee, Kyu-Bok;Jin, Myoung-Uk
    • Journal of Dental Rehabilitation and Applied Science
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    • v.32 no.3
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    • pp.184-193
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    • 2016
  • Purpose: To evaluate marginal leakage of bulk fill flowable composite resin filling with different curing time by using microcomputed tomography technology. Materials and Methods: 30 previously extracted human molars were randomly divided into 6 groups based upon restorative system and different curing time. Class II cavities (vertical slot cavities) were prepared. An individual metallic matrix was used to build up the proximal wall. The SonicFill or SureFil SDR flow was inserted into the preparation by using 1 bulk increment, followed by light polymerization for different curing times. The different exposure times were 20, 40, and 60 seconds. All specimens were submitted to 5,000 thermal cycles for artificial aging. Micro-CT scanning was performed by using SkyScan 1272. One evaluator assessed microleakage of silver nitrated solution at the resin-dentin interface. The 3D image of each leakage around the restoration was reconstructed with CT-Analyser V.1.14.4. The leakage was analyzed with the Mann-Whitney test. Results: Significant differences were observed between the light curing times, but no significant differences were found between the bulk fill composite resins. Increasing in the photoactivation time resulted in greater microleakage in all the experimental groups. Those subjected to 60 seconds of light curing showed higher microleakage means than those exposed for 20 seconds and 40 seconds. Conclusion: Increasing the photoactivation time is factor that may increase marginal microlekage of the bulk fill composite resins. Further, micro-CT can nondestructively detect leakage around the resin composite restoration in three dimensions.

Multiple Injection Method for Bulk Syndiospecific Polymerization of Styrene with Homogeneous Metallocene Catalyst (메탈로센 촉매를 이용한 신디오탁틱 폴리스타이렌의 벌크 중합에 관한 연구)

  • Yim, Jin-Heong;Son, Young-Gon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.11 no.4
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    • pp.1348-1353
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    • 2010
  • At the early stage of a bulk syndiotactic polymerization of styrene, the homogeneous reactant mixture transforms to a slurry state consisting of a precipitated solid syndiotactic PS and a liquid reactant mixture. As the reaction proceeds, the slurry transforms into a wet and then a dried powder if proper methods are used to prevent agglomeration. When a large amount of catalyst and co-catalyst is added to the styrene to achieve a high conversion rate, the reactant mixture becomes a lumpy agglomeration and further control of the reaction is impossible. In this study, we introduce a novel approach to avoid such agglomeration while maintaining a high conversion rate. Instead of adding the catalyst and co-catalyst at once, the total amount of the catalyst and co-catalyst is divided into several parts and added successively. This method is found to be very effective to avoid the formation of agglomerate and to maintain a fairly high conversion rate of slurry into powdery product (up to 70 %). It is also observed that this method produces syndiotactic PS of a higher molecular weigh.

Preparation of Syndiotactic Poly(vinyl alcohol) Microfibrils with Radiopaque Inorganic Particles (방사선불투과성 무기입자를 첨가한 교대배열 폴리비닐알코올 마이크로피브릴의 제조)

  • Jo, Hye Won;Cha, Jin Wook;Han, Sung Soo;Lee, Joon Seok;Oh, Tae Hwan
    • Polymer(Korea)
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    • v.37 no.5
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    • pp.563-570
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    • 2013
  • Poly(vinyl pivalate) (PVPi) was bulk polymerized to make poly(vinyl alcohol) (PVA) microfibrils to apply for polymeric embolization coils replacing metalic coils. Then, syndiotactic PVA (s-PVA) microfibrils having number-average degree of polymerization of 1100 and s-diad content of 60.4% were prepared via saponification of the PVPi with no separate spinning process. To make s-PVA microfibrils with radiopacity, zirconium dioxide ($ZrO_2$) and barium sulfate ($BaSO_4$) were added into s-PVA microfibrils during saponification. The computed tomography (CT) value indicating radiopacity reached up to over 1000 when the amount of $ZrO_2$ and $BaSO_4$ were 12 and 6 wt%, respectively.

Correlation between Linear polymerization shrinkage & tooth cuspal deflection (교두변위와 선수축량의 연관성 분석)

  • Lee, Soon-Young;Park, Sung-Ho
    • Restorative Dentistry and Endodontics
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    • v.30 no.6
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    • pp.442-449
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    • 2005
  • The purpose of the present study was to evaluate the relationship between the amount of cuspal deflection and linear polymerization shrinkage in resin composite and polyacid modified resin composite, For cuspal defelction and shrinkage measurement, Dyract AP, Compoglass F, Z100, Surefil. Pyramid, Synergy Compact, Heliomolar and Heliomolar HB were used. For measuring polymerization shrinkage, a custom made linometer (R&B, Daejon, Korea) was used The amount of shrinkage among materials was compared using One-way ANOVA analysis and Tukey's test at the $95\%$ of confidence level For measuring cuspal deflection of teeth, standardized MOD cavities were prepared in extracted maxillary premolars. After a self-etching adhesive was applied, cavities were bulk filled with one of the felling materials. Fifteen teeth were used for each material. Cuspal deflection was measured by a custom made cuspal-deflection measuring device. One-way ANOVA analysis and Tukey's test were used to determine differences between the materials at the $95\%$ of confidence level, Correlation of polymerization shrinkage and cuspal deflection were analyzed by regression analysis. The amount of polymerization shrinkage from least to greatest was Heliomolar, Surefil < Heliomolar HB < Z100, Synergy Compact < Dyract AP < Pyramid, Compoglass F (p<0.05). The amount of cuspal deflection from least to greatest was Z100, Heliomolar, Heliomolar HB, Synergy Compact Surefil < Compoglass F < Pyramid, Dyract AP (p < 0.05). The amount of polymerization shrinkage and cuspal deflection showed a correlation (p<0.001).

Bulk Polymerization of L-lactide Using Aluminium Organometallic Compound Supported on Functionalized Silica (표면 기능화된 실리카에 담지된 Al 유기금속화합물을 이용한 L-lactide 벌크중합 특성 연구)

  • Yoo, Ji Yun;Ko, Young Soo
    • Polymer(Korea)
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    • v.36 no.6
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    • pp.693-698
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    • 2012
  • In this study aluminum isopropyl oxide ($Al(O-i-Pr)_3$) was supported on the amine-functionalized surface of silica to synthesize high molecular weight (MW) polylactide (PLA), and it was tested for PLA polymerization behaviors. A silica was funtionalized with silane compound having amine groups, then in-situ treated with $Al(O-i-Pr)_3$. $Al(O-i-Pr)_3$ attached to amine group on silica showed activity only in the presence of MAO (methyl aluminoxane). At the polymerization temperature of $115^{\circ}C$, the conversion and the MW of PLA were increased as the amount of silane was increased. At the polymerization temperature of $130^{\circ}C$, the conversion was decreased while the MW was increased drastically and reached to MW 44000 g/mol when the amine concentration was 3.0 mmol/g. A bimodal type GPC curve was shown at the polymerization temperature of $115^{\circ}C$. As the amount of amine group increased, the peaks of GPC curve were merged. At the polymerization of $130^{\circ}C$, a unimodal GPC curve was shown. $Al(O-i-Pr)_3$ supported on amine-functionalized silica was able to produce higher MW PLA with enhanced activity compared to homogeneous $Al(O-i-Pr)_3$.

Effect of PTMGDA-PEGMA dopant on PVDF ultrafiltration membrane

  • Chen, Gui-E.;Huang, Hui-Hong;Xu, Zhen-Liang;Zhang, Ping-Yun;Wu, Wen-Zhi;Sun, Li;Liu, Yan-Jun
    • Membrane and Water Treatment
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    • v.7 no.6
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    • pp.539-553
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    • 2016
  • As a novel hydrophobic monomer, polytetrahydrofuran diacrylate (PTMGDA) was synthesized by the esterification reaction between polyethylene tetrahydrofuran (PTMG) and acryloyl chloride (AC). In situ free radical polymerization reaction method was utilized to fabricate poly (vinylidene fluoride) (PVDF)-PTMGDA-poly(ethylene oxide) dimethacrylate (PEGMA) ulrafiltration (UF) membranes. The performances of PVDF-PTMGDA-PEGMA UF membranes in terms of morphologies, mechanical properties, separation properties and hydrophilicities were investigated. The introduction of the PTMGDA-PEGMA dopants not only increased the membranes' pure water flux, but also improved their mechanical properties and the dynamic contact angles. The addition of the PTMGDA/PEGMA dopants led to the formation of the finger-like structure in the membrane bulk. With the increase concentration of PTMGDA/PEGMA dopants, the porosity and the mean effective pore size increased. Those performances were coincide with the physicochemical properties of the casting solutions.

Bulk Coordination Polymerization of Dicyclopentadiene (DCPD) by Pd Complexes Containing β-Ketoiminate or β-Diketiminate Ligands

  • Lee, Eung Jun;Kim, Ho Sup;Lee, Byoung Ki;Hwang, Woon Sung;Sung, Ik Kyoung;Lee, Ik Mo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.4131-4136
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    • 2012
  • Several palladium complexes containing ${\beta}$-ketoiminate and ${\beta}$-diketiminate ligands successfully produced poly(DCPD) possibly via vinyl addition. It was found that catalysts with ${\beta}$-diketiminate ligands containing bulkier aryl substituents showed the highest activity in the presence of MAO as a cocatalyst. Purity of DCPD is quite essential for the higher activity and small amount of organic solvent such as $CH_2Cl_2$ and toluene is required to reduce the viscosity of the reactant mixture for the higher activity. $^1H$ NMR spectra of produced polymers with N,N-dimethylanilinium tetra(pentafluorophenyl)borate (N,N-DAPFAr"$_4$) show that 5,6-double bond of DCPD is removed with 2,3-double bond remaining. Produced poly(DCPD) with MAO cocatalyst is quite rigid and insoluble in common organic solvents but rather brittle.