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首页> 外文期刊>Journal of Applied Polymer Science >Cationic UV curing behavior and thermal properties of oxetane-modified polysiloxane prepared from tetraethyl orthosilicate
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Cationic UV curing behavior and thermal properties of oxetane-modified polysiloxane prepared from tetraethyl orthosilicate

机译：四乙基原硅酸酯制备的氧杂环丁烷改性聚硅氧烷的阳离子紫外固化行为和热性能

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摘要

The oxetane-modified polysiloxane (Oxe-PSiO) was synthesized via the partial hydrolysis/condensation of tetraethyl orthosilicate (TEOS) and then transesterification reaction with 3-ethyl-3-(hydroxymethyl)oxetane (EHO), and characterized by FT-IR, ~1H NMR, ~(13)C NMR, and ~(29)Si NMR spectroscopy. Using the water/TEOS molar ratios of 0.8-1.2, the number-average molecular weights and polydispersity indices were obtained by GPC to range from 1.013 to 2.716 g mol~(-1) and around 2.0, respectively. The viscosity of Oxe-PSiO prepared from the water/TEOS molar ratio of 1.2 sharply increased to 177,545 cps from 438 cps of that from the molar ratio of 0.8. A series of cationic UV-curable formulations were prepared by blending the Oxe-PSiO synthesized with the water/TEOS molar ratio of 1.0 into an commercial oxetane-based resin, 3,3′-[oxydi(methylene)]bis(3- ethyloxetane), in different weight ratios. The photopolymerization kinetics studied by photo-DSC in the presence of triphenylsulphonium hexafluoroantimonate as a cationic photoinitiator showed that both the maximum photopolymerization rate and final oxetane conversion in the cured film decreased with increasing Oxe-PSiO loading mainly due to the sharp increase in viscosity. The DMTA and DSC results both indicated the improvement in thermal stability, showing 12 and 13.4°C, respectively, higher T_g for the cured film with 50 wt % Oxe-PSiO loading compared with the pure polymer. Moreover, the temperatures (T10% and T_(50%)) at the weight loss of 10 and 50% and final char yields measured by TGA increased with increasing Oxe-PSiO content. After adding 50 wt % Oxe-PSiO, compared with the pure polymer the T_(10%) increased from 349 to 361°C, while the T_(50%) increased from 409 to 424°C, and with a char yield increase of 8.2% at 800°C. In addition, its greatly increased crosslinking density due to the formation of silica network resulted in the enhancement in pencil hardness from B of the pure polymer to 2H grade.
机译：氧杂环丁烷改性的聚硅氧烷（Oxe-PSiO）是通过原硅酸四乙酯（TEOS）的部分水解/缩合然后与3-乙基-3-（羟甲基）氧杂环丁烷（EHO）进行酯交换反应合成的，并通过FT-IR表征， 〜1H NMR，〜（13）C NMR和〜（29）Si NMR光谱。使用0.8 / 1.2的水/ TEOS摩尔比，通过GPC获得的数均分子量和多分散指数分别为1.013至2.716g mol·（-1）和约2.0。由1.2的水/ TEOS摩尔比制备的Oxe-PSiO的粘度从由0.8的摩尔比急剧增加至177,545cps。通过将合成的Oxe-PSiO（水/ TEOS摩尔比为1.0）掺入市售的基于氧杂环丁烷的树脂3,3'-[氧二（亚甲基）]双（3-乙基氧杂环丁烷）中，制备了一系列阳离子UV固化配方），不同的重量比。在六氟锑酸三苯磺酸钠作为阳离子光引发剂的情况下，通过光DSC研究的光聚合动力学表明，随着Oxe-PSiO负载量的增加，固化膜中的最大光聚合速率和最终氧杂环丁烷转化率均下降，这主要是由于粘度的急剧增加。 DMTA和DSC结果均表明了热稳定性的改善，与纯聚合物相比，具有50wt％的Oxe-PSiO负载的固化膜分别显示了12和13.4℃的更高的T_g。此外，随着Oxe-PSiO含量的增加，重量损失为10％和50％时的温度（T10％和T_（50％））以及通过TGA测量的最终炭收率都增加了。加入50 wt％的Oxe-PSiO后，与纯聚合物相比，T_（10％）从349°C升高至361°C，而T_（50％）从409°C升高至424°C，且炭产率提高了在800°C时为8.2％。此外，由于形成了二氧化硅网络，其交联密度大大提高，从而导致铅笔硬度从纯聚合物的B提高到2H级。

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