Synthesis, characterization, shrinkage and curing kinetics of a new low-shrinkage urethane dimethacrylate monomer for dental applications
Synthesis, characterization, shrinkage and curing kinetics of a new low-shrinkage urethane dimethacrylate monomer for dental applications
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DOI：
10.1016/j.dental.2007.03.004
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发表时间：
2007-08-01
期刊：
影响因子：
5
通讯作者：
Watts, David C.
中科院分区：
文献类型：
--
作者：
Atai, Mohammad;Ahmadi, Mehdi;Watts, David C.
目标.合成了异佛尔酮基聚氨酯二甲基丙烯酸酯（IP-UDMA）树脂单体，并对其进行了表征，研究了IP-UDMA树脂单体的收缩和固化动力学。通过聚乙二醇400和异佛尔酮二异氰酸酯反应，然后与HEMA反应以甲基丙烯酸酯端基封端来合成IP-UDMA单体。使用标准返滴定法和FTIR光谱法跟踪反应。采用FTIR、1H NMR、元素分析和折光率测定对最终产物进行了纯化和表征。使用粘合盘技术在23、35和45 ℃下测量在约700 mW/cm（2）下光聚合的样品的收缩应变。初始收缩应变速率通过收缩应变数据相对于时间的数值微分获得。使用FTIR光谱测量样品的转化度。用差示扫描量热法（DSC）研究了单体的热固化动力学。表征方法证实了建议的反应路线和合成的单体。新单体获得了约4%的低收缩-应变。结果表明，单体的收缩应变速率符合Kamal和Sourour的自催化模型[Kamal MR，Sourour S.热固材料固化动力学和热特性。Polym Eng Sci 1973;13（1）：59-64]，其用于描述热固性树脂的反应动力学。通过方程线性化计算模型参数。模型预测值与实验值吻合较好。新单体的性能与市售树脂的性能相比是有利的。(c)2007年，牙科材料学院。由爱思唯尔有限公司出版。保留所有权利。
Objectives. The aim of the study was to synthesize and characterize an isophorone-based urethane dimethacrylate (IP-UDMA) resin-monomer and to investigate its shrinkage and curing kinetics.Methods. The IP-UDMA monomer was synthesized through the reaction of polyethylene glycol 400 and isophorone diisocyanate followed by reacting with HEMA to terminate it with methacrylate end groups. The reaction was followed using a standard back titration method and FTIR spectroscopy. The final product was purified and characterized using FTIR, H-1 NMR, elemental analysis and refractive index measurement. The shrinkage-strain of the specimens photopolymerized at circa 700 mW/cm(2) was measured using the bonded-disk technique at 23, 35, and 45 degrees C. Initial shrinkage-strain-rates were obtained by numerical differentiation of shrinkage- strain data with respect to time. Degree-of-conversion of the specimens was measured using FTIR spectroscopy. The thermal curing kinetics of the monomer were also studied by differential scanning calorimetry (DSC).Results. The characterization methods confirmed the suggested reaction route and the synthesized monomer. A low shrinkage- strain of about 4% was obtained for the new monomer. The results showed that the shrinkage-strain-rate of the monomer followed the autocatalytic model of Kamal and Sourour [Kamal MR, Sourour S. Kinetic and thermal characterization of thermoset cure. Polym Eng Sci 1973;13(1):59-64], which is used to describe the reaction kinetics of thermoset resins. The model parameters were calculated by linearization of the equation.Significance. The model prediction was in a good agreement with the experimental data. The properties of the new monomer compare favorably with properties of the commercially available resins. (c) 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.