• Macromolecular Research
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• 제13권3호
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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.

• Macromolecular Research
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• 제13권3호
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• pp.236-242
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• 2005

Three dithioester-derived carboxyl acid functionalized RAFT(reversible addition-fragmentation chain transfer) agents, viz. acetic acid dithiobenzoate, butanoic acid dithiobenzoate and 4-toluic acid dithiobenzoate, were used in the RAFT bulk polymerization of styrene, in order to study the effects of the R-group structure on the living nature of the polymerization. By conducting the polymerization with various concentrations of the RAFT agents and at different temperatures, it was found that the R-group structure of the RAFT agents plays an important role in the RAFT polymerization; the bulky structure and radical stabilizing property of the R-group enhances the living nature of the polymerization and allows the polymerization characteristics to be well controlled.

• 한국섬유공학회:학술대회논문집
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• 한국섬유공학회 2003년도 봄 학술발표회 논문집
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• pp.13-16
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• 2003

Vinyl acetate monomer can be polymerized through bulk, solution, emulsion, and suspension polymerization processes. However, in the preparation of PVA from bulk or solution polymerization, there are several technical limitations for obtaining high yield and high molecular weight simultaneously. Thus, the improvement of polymerization method is necessary to prepare the PVA with high yield and high molecular weight because that the difficulty in control of high viscosity and in removal of the heat of polymerization, which might lead to side reactions like branching. (omitted)

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.236-242
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• 2014

Isospecific propylene polymerization behavior of meta- and para-Lewis base (E) functionalized unbridged zirconocenes ($[1-(E_n-Ph)-3,4-Me_2C_5H_2]_2ZrCl_2$, E = $NMe_2$, OMe; n = 1 or 2) was investigated under bulk conditions. Catalytic activity of the zirconocenes, and molecular weight and isotacticity of polypropylenes are found to be dependent on the position and number of the Lewis base functional groups in the zirconocenes. All the crude polypropylenes possess a broad molecular weight distribution and multi-melting transitions, indicating an involvement of multi-catalytic active species in the polymerization. The highest [mmmm] value of an isotactic portion of the polypropylenes reached 89%, which is higher than that (85%) from the well-known $C_2$-symmetric EBIZr (rac-$Et(Ind)_2ZrCl_2$) catalyst. These results support that the in situ generated, rigid rac-like cation-anion pair through the Lewis acid-base interactions between the functional groups of zirconocenes and methylaluminoxane anion is effective in the formation of isotactic polypropylene under bulk propylene polymerization conditions.

• 치위생과학회지
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• 제23권2호
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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.

• 대한소아치과학회지
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• 제46권1호
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• pp.1-9
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• 2019

이번 연구에서는 저점도 및 고점도 bulk-fill giomer 복합레진의 전환율과 중합수축을 기존 bulk-fill 복합레진 및 전통적 복합레진과 비교 평가해보고자 하였다. Bulk-fill giomer 복합레진 2종류(Beautifil Bulk Restorative(BBR), Beautifil Bulk Flowable(BBF)), bulk-fill 복합레진 2종류(Tetric N-Ceram Bulk-fill(TBF), SureFil SDR flow(SDR)), 전통적 복합레진 2종류(Tetric N-Ceram(TN), Tetric N-flow(TF))를 사용하였다. 중합도 측정은 Fourier transform infrared spectroscopy을 사용하였으며, 중합수축은 linometer을 이용하여 측정하였다. 복합레진 하면의 전환율 측정 결과 2 mm와 4 mm 깊이 모두 BBR에서 가장 낮게 나왔으며, SDR에서 가장 높게 나왔다. 4 mm 깊이에서 고점도 및 저점도 bulk-fill giomer 복합레진의 전환율은 bulk-fill 복합레진에 비해 유의하게 낮은 값을 보였다(p < 0.05). 깊이에 따른 전환율 비교 시 TBF, TN, TF는 유의차를 보였으며(p < 0.05), BBR, BBF, SDR는 유의차를 보이지 않았다. 중합수축은 TF > SDR > BBF > TBF > TN, BBR 순서로 감소 했으며(p < 0.05), bulk-fill giomer 복합레진은 bulk-fill 복합레진보다 낮은 중합수축량을 보였다(p < 0.05). 이번 연구 결과 4 mm 깊이에서 bulk-fill giomer 복합레진 및 TBF는 불충분한 중합을 나타냈으며, 2 mm와 4 mm 모두에서 고점도 및 저점도 bulk-fill giomer 복합레진은 bulk-fill 복합레진에 비해 낮은 전환율을 보였다. 그러므로 bulk-fill giomer 복합레진의 임상적인 적용을 위해서는 이에 대한 충분한 고찰 및 주의가 필요할 것으로 생각된다.

• 대한치과의사협회지
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• 제57권3호
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• pp.162-168
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• 2019

Composite resin restorations in posterior teeth are increasing due to the aesthetic needs of patients and the development of materials. This trend will accelerate in line with domestic insurance policies. However, resin composites generate stresses due to their contraction during the polymerization process. To reduce the polymerization shrinkage stress of resin composites, incremental layering technique has been recommended for decades. This technique reduces stress at the cavity wall interface and allows a more efficient light curing of the material. Bulk-fill resin composites have been designed to simplify the restorative technique because they can be placed into cavities in a single increment of 4-5mm. The simplification of the operative procedures is desirable in clinical daily practice. In this context, bulk-fill resin composites are an attractive alternative for posterior restorations. However, a clearer understanding of the clinical performance of this relatively new class of materials in comparison to conventional resin composites is required. Based on previous studies, the aim of the current review was to present the clinical criteria for the use of bulk-fill composites in direct restorations of posterior teeth.

• 폴리머
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• 제39권3호
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• pp.365-369
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• 2015

본 연구에서는 Al 화합물인 methylaluminoxane(MAO)를 이용하여 L-lactide의 벌크중합 및 용액중합을 실시하였다. 촉매 투입량에 따른 벌크중합 결과, 투입량이 증가할수록 전환율이 증가하였다. 분자량은 촉매 투입량이 0.15 mmol일 때 60800 g/mol로 가장 높은 분자량을 얻었으며 그 이상의 투입량에서는 분자량이 감소하였다. Turnover frequency(TOF)값의 경우 촉매 투입량이 0.15 mmol일 때 가장 크고 촉매 투입량이 증가할수록 감소하였다. 용액중합에서는 30분 가량 induction time이 존재하였다. 중합 시간에 따라 3시간까지 전환율이 선형적으로 증가하였으며 6시간일 때 54700 g/mol로 가장 높은 분자량을 얻었다.

• 대한소아치과학회지
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• 제43권4호
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• pp.365-373
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• 2016

치아우식증을 치료할 때 가장 많이 사용되는 수복재료 중 하나는 레진이다. 하지만 레진은 중합수축, 긴 작업시간, 수분 및 오염에 민감하다는 단점들이 존재하고 어린이를 치료할 때 더 두드러진다. 이러한 단점들을 해결하기 위해 bulk filling이 나타나게 되었고, 이를 가능하게 하는 bulk-fill 복합레진이 개발되었다. 본 연구의 목적은 전통적 복합레진과 bulk-fill 복합레진의 물성을 다양한 방법으로 평가 및 비교하기 위함이다. 전통적 복합레진 3 종류(Filtek Z-350 (Z-350), Unifil Flow (UF), Unifil Loflo Plus (UL)), bulk-fill 복합레진 2종류 (SureFil SDR flow (SDR), Tetric N-Ceram bulk fill (TBF))를 사용하였다. 광중합기는 light-emitting diodes를 사용하였고, 한번 중합할 때 20초간 시행하였다. 재료들의 미세경도는 비커스경도기로 측정하였고, 중합도 측정은 Fourier transform infrared spectroscopy을 사용하였다. 중합수축량은 컴퓨터로 제어되는 linometer를 이용하였다. 굴곡강도 및 굴곡계수는 3점 굽힘 시험법으로 측정하였고, 압축강도 및 압축계수와 함께 Universal testing machine을 이용하여 측정하였다. 통계분석은 ANOVA를 사용하였고, Scheffe의 사후검정을 하였다. 미세경도는 상면에서 Z-350이 가장 높은 값을 나타냈고, 하면은 TBF가 높은 값을 나타냈으나 UL은 상하면 모두에서 가장 낮은 값을 보였다. 상면과 하면의 미세경도 값의 비는 SDR, TBF가 높았다. 중합도는 bulk-fill 복합레진과 유동성 복합레진 상하면 모두에서 높게 나타나고, Z-350는 상하면 모두에서 55% 이하로 나타났다. 압축강도는 Z-350이 가장 높았으며 SDR이 낮게 나타났으나 UL과는 통계학적으로 유의하게 차이는 보이지 않았다. 압축계수는 Z-350이 높게 나타났고, UL이 가장 낮았다. 굴곡강도 및 굴곡계수는 Z-350이 가장 높았다. UL은 굴곡강도 및 굴곡계수 모두 가장 낮게 나타났다. UL이 가장 높은 중합수축을 보였고, Z-350이 가장 낮은 중합수축 값을 나타냈다. 유동성 복합레진이 비유동성 복합레진보다 중합 수축 양이 많았다. 결론적으로 bulk-fill 복합레진의 물성은 전통적 복합레진보다 떨어지지만 bulk filling할 때 중요한 상하면의 미세경도비 및 중합도는 높게 나타나 어린이의 치아우식증 수복치료 시 도움이 될 수 있을 것으로 사료된다.

• Restorative Dentistry and Endodontics
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• 제45권3호
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• pp.32.1-32.12
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• 2020

Objectives: To evaluate the polymerization efficiency of a matrix-modified bulk-fill composite, and compare it to a conventional composite which has a similar filler system. The degree of conversion (DC%) and monomer elution were measured over different storage periods. Additionally, fillers' content was examined. Materials and Methods: Cylindrical specimens were prepared, in bulk and incrementally, from Filtek Bulk Fill (B) and Filtek Supreme XTE (S) composites using a Teflon mold, for each test (n = 6). Using attenuated total reflection method of Fourier transformation infrared spectroscopy, DC% was measured after 24 hours, 7 days, and 30 days. Using high-performance liquid chromatography, elution of hydroxyethyl methacrylate, triethylene glycol dimethacrylate, urethane dimethacrylate, and bisphenol-A glycidyl dimethacrylate was measured after 24 hours, 7 days and 30 days. Filler content was examined by scanning electron microscopy (SEM). Data were analyzed using 2-way mixed-model analysis of variance (α = 0.05). Results: There was no significant difference in DC% over different storage periods between B-bulk and S-incremental. Higher monomer elution was detected significantly from S than B. The elution quantity and rate varied significantly over storage periods and between different monomers. SEM images showed differences in fillers' sizes and agglomeration between both materials. Conclusions: Matrix-modified bulk-fill composites could be packed and cured in bulk with polymerization efficiency similar to conventional composites.