Scale-up synthesis of vinyl polymer-grafted nano-sized silica by radical polymerization of vinyl monomers initiated by surface initiating groups in the solvent-free dry-system |
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Authors: | Jun Ueda Asako Tsunokawa Norio Tsubokawa |
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Institution: | a Graduate School of Science and Technology, Niigata University, 8050 Ikarashi 2-no-cho, Niigata 950-2181, Japan b Department of Material Science and Technology, Faculty of Engineering, Niigata University, 8050 Ikarashi 2-no-cho, Niigata 950-2181, Japan c Center for Transdisciplinary Research, Niigata University, 8050 Ikarashi 2-no-cho, Niigata 950-2181, Japan |
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Abstract: | For the purpose of the prevention of the environmental pollution and the simplification of reaction process, the scale-up radical graft polymerization of vinyl monomers onto nano-sized silica surface initiated by azo groups and peroxycarbonate groups previously introduced onto the surface in the solvent-free dry-system was investigated. The introduction of azo groups onto the silica surface was achieved by the reaction of surface amino groups with 4,4′-azobis(4-cyanopentanoic acid chloride). On the other hand, the introduction of peroxycarbonate groups onto the silica surface was achieved by Michael addition of surface amino groups to t-butylperoxy-2-methacryloyloxyethylcarbonate. The graft polymerization of vinyl monomers onto the surface was successfully achieved by splaying monomers to nano-sized silica having azo and peroxycarbonate groups in solvent-free dry-system. It is interesting to note that the formation of ungrafted polymer was depressed in comparison with graft polymerization in solution: the grafting efficiency was 90-95%. In addition, in the solvent-free dry-system, the grafting of copolymer having pendant peroxycarbonate groups onto the nano-sized silica surface and the radical postgraft polymerization of styrene initiated by the pendant initiating groups of the grafted copolymer chain on the silica surface was investigated. |
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Keywords: | Nano-sized silica Surface grafting Scale-up synthesis Solvent-free dry-system t-Butylperoxy-2-methacryloyloxyethylcarbonate |
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