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Crosslinking Amine-Modified Silica Aerogels with Epoxies: Mechanically Strong Lightweight Porous Materials

机译:与环氧树脂交联的胺改性二氧化硅气凝胶:机械强度高的轻质多孔材料

摘要

The mesoporous surfaces of TMOS-derived silica aerogels have been modified with amines by co-polymerization of TMOS with APTES. The amine sites have become anchors for crosslinking the nanoparticles of the skeletal backbone of the aerogel by attachment of di-, tri and tetra-functional epoxies. The resulting conformal coatings increase the density of the native aerogels by a factor of 2-3 but the strength of the resulting materials may increase by more than two orders of magnitude. Processing variables such as amount of APTES used to make the gels, the epoxy type and concentration used for crosslinking, as well as the crosslinking temperature and time were varied according to a multivariable design-of-experiments (DOE) model. It was found that while elastic modulus follows a similar trend with density, maximum strength is attained neither at the maximum density nor at the highest concentration of -NH2 groups, suggesting surface saturation effects. Aerogels crosslinked with the tri-functional epoxide always show improved strength compared with aerogels crosslinked with the other two epoxides under identical conditions. Solid C-13 NMR studies show residual unreacted epoxides, which condense with ne another by heating crosslinked aerogels at 150 C.
机译:TMOS衍生的二氧化硅气凝胶的介孔表面已通过TMOS与APTES的共聚胺进行了改性。胺位点已成为通过连接二官能,三官能和四官能环氧树脂而使气凝胶骨架骨架的纳米颗粒交联的锚点。所得的保形涂层将天然气凝胶的密度增加了2-3倍,但所得材料的强度可能增加了两个数量级以上。根据多变量实验设计(DOE)模型,可改变加工变量,例如用于制备凝胶的APTES的量,用于交联的环氧类型和浓度以及交联温度和时间。已经发现,尽管弹性模量随密度遵循相似的趋势,但是在最大密度或-NH 2基团的最高浓度下均未达到最大强度,这表明表面饱和作用。与在相同条件下与其他两种环氧化物交联的气凝胶相比,与三官能环氧化物交联的气凝胶始终显示出更高的强度。固体C-13 NMR研究表明,残留的未反应的环氧化物通过在150°C加热交联的气凝胶而彼此缩合。

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