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Crosslinked epoxy microspheres: Preparation, surface-initiated polymerization, and use as macroporous silica porogen

机译:交联的环氧微球:制备,表面引发的聚合反应以及用作大孔二氧化硅致孔剂

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In this article, we report the preparation of crosslinked epoxy microspheres with diameters of 5-10 μm prepared via phase-inverted phase separation induced by polymerization in the thermosetting blend of epoxy and poly(ε-caprolactone). The surfaces of the epoxy microspheres were functionalized to bear 2-bromopropionyl groups, which were further used as initiators to obtain poly(glycidyl methacrylate) (PGMA) grafted epoxy microspheres via the surface-initiated atom transfer radical polymerization approach. The PGMA-grafted epoxy microspheres were then employed to react with 3-aminopropyltrimethoxylsilane (APTMS) to obtain the functionalized epoxy microspheres, the surface of which contained a great number of trimethoxysilane groups. A co-sol-gel process between the APTMS-functionalized epoxy microspheres and tetraethoxysilane was performed, and organic-inorganic glassy solids were obtained. The organic-inorganic glasses were used as precursors for accessing macroporous silica materials via pyrolysis at elevated temperatures. The hierarchical porosity of the resulting macroporous silica was investigated by means of field emission scanning electronic microscopy, transmission electronic microscopy, and surface-area Brunauer-Emmett-Teller (BET) measurements. We found that the macroporous silica possessed BET surface areas in the range 183.9-235.2 m~2/g, depending on the compositions of their precursors.
机译:在本文中,我们报告了通过在环氧树脂和聚(ε-己内酯)的热固性共混物中聚合引发的相转化相分离制备直径为5-10μm的交联环氧微球的方法。将环氧微球的表面官能化以带有2-溴丙酰基,将其进一步用作引发剂,通过表面引发的原子转移自由基聚合方法获得聚甲基丙烯酸环氧丙酯(PGMA)接枝的环氧微球。然后将PGMA接枝的环氧微球与3-氨基丙基三甲氧基硅烷(APTMS)反应以获得官能化的环氧微球,其表面包含大量的三甲氧基硅烷基团。在APTMS官能化的环氧微球与四乙氧基硅烷之间进行助溶胶-凝胶工艺,获得有机-无机玻璃状固体。有机-无机玻璃用作在高温下通过热解获得大孔二氧化硅材料的前体。通过场发射扫描电子显微镜,透射电子显微镜和表面积Brunauer-Emmett-Teller(BET)测量研究了所得大孔二氧化硅的分级孔隙率。我们发现,根据其前体的组成,大孔二氧化硅的BET表面积为183.9-235.2 m2 / g。

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