Iran Polymer and Petrochemical Institute, P.O. Box 14965/115, Tehran, Iran.
Iran Polymer and Petrochemical Institute, P.O. Box 14965/115, Tehran, Iran.
Dent Mater. 2021 Aug;37(8):1283-1294. doi: 10.1016/j.dental.2021.04.012. Epub 2021 May 19.
To synthesize an amine-modified polyhedral oligomeric silsesquioxane (POSS) nano-structure as a novel co-initiator-crosslinker (co-Ini-Linker) and to determine the effect of the co-Ini-linker on the physical and mechanical behavior of an experimental dental composite.
The amine-methacrylate POSS nano-structures (AMA-POSS) were chemically synthesized by anchoring a tertiary amine functionality on the methacrylate POSS (MA-POSS) branches. Three types of AMA-POSS, having different amine branches in their structures, were synthesized through the Aza Michael reaction. The chemical structure of AMA-POSSs were evaluated byH-NMR spectroscopy. Afterward, the AMA-POSS was incorporated into a dental resin system composed of Bis-GMA, TEGDMA, and photo-initiator. Three resin systems with different AMA-POSS types were then prepared, and their properties were compared with a resin containing DMAEMA as a conventional co-initiator. The degree of conversion evaluated by FTIR spectroscopy and the shrinkage kinetics of the resins were determined through the bonded-disk technique. The flexural properties of the photopolymerized resins were also investigated. The distribution of nano-structures in the matrix resin was analyzed using EDX analysis.
The modified POSS structure and the number of amine branches were confirmed withH-NMR spectroscopy. The resin containing 8 amine branches (P8) showed the same degree of conversion (DC%) as the resin containing DMAEMA (P > 0.05). Decreasing the amine branches in the POSS structure, however, revealed an increasing trend in DC%. The resin containing P8 showed the lowest shrinkage strain. By incorporating AMA-POSS into the resin system, the water sorption significantly decreased (P < 0.05). The flexural strength and modulus increased by adding P3 into the resin system (P < 0.05). EDX Si-map revealed that the co-Ini-linker was well dispersed in the resin matrix.
The synthesized novel amine-methacrylate POSS nanostructures not only act as an amine co-initiator but also work as a reinforcing filler and a cross-linking agent.
合成一种胺改性的多面体低聚倍半硅氧烷（POSS）纳米结构作为新型的共引发剂-交联剂（co-Ini-Linker），并确定共引发剂交联剂对实验性牙科复合材料物理力学性能的影响。
通过在甲基丙烯酰基 POSS（MA-POSS）支链上锚定叔胺官能团，化学合成了胺-甲基丙烯酸酯 POSS 纳米结构（AMA-POSS）。通过氮杂迈克尔加成反应合成了具有不同胺支链结构的三种 AMA-POSS。通过 1H-NMR 光谱评估 AMA-POSS 的化学结构。然后，将 AMA-POSS 掺入由 Bis-GMA、TEGDMA 和光引发剂组成的牙科树脂体系中。然后制备了三种具有不同 AMA-POSS 类型的树脂体系，并将其性能与含有 DMAEMA 的树脂进行了比较，DMAEMA 是一种常规的共引发剂。通过傅里叶变换红外光谱（FTIR）评估转化率，通过键合盘技术测定树脂的收缩动力学。还研究了光聚合树脂的弯曲性能。使用 EDX 分析分析纳米结构在基质树脂中的分布。
通过 1H-NMR 光谱证实了改性 POSS 结构和胺支链的数量。含有 8 个胺支链的树脂（P8）与含有 DMAEMA 的树脂具有相同的转化率（DC%）（P > 0.05）。然而，降低 POSS 结构中的胺支链数量则显示出 DC%的增加趋势。含有 P8 的树脂显示出最低的收缩应变。通过将 AMA-POSS 掺入树脂体系中，吸水率显著降低（P < 0.05）。将 P3 加入树脂体系中可提高弯曲强度和模量（P < 0.05）。EDX Si 映射显示共引发剂交联剂在树脂基质中均匀分散。
合成的新型胺-甲基丙烯酸酯 POSS 纳米结构不仅可以作为胺共引发剂，还可以作为增强填料和交联剂。
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