Synthesis and characterization of poly(methyl methacrylate)-grafted silica microparticles

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作者：
Derouet, Daniel [1 ]
Chi, Nhan Ha Thuc [1 ]
机构：
[1] LCOM, Chimie des Polymères (UMR du CNRS UCO2M No 6011), Faculté des Sciences, Avenue Olivier Messiaen, 72085 Le Mans Cedex 9, France
来源：
Journal of Applied Polymer Science | 2008年 / 109卷 / 04期
关键词：
A procedure to synthesize poly(methyl methacrylate)-grafted silica microparticles was developed by using radical photopolymerization of methyl methacrylate (MMA) initiated from N; N-diethyldithiocarbamate (DEDT) groups previously bound to the silica surface (grafting from). The functionalization of silica microparticles with DEDT groups was performed in two steps: introduction of chlorinated functions onto the surface of silica particles; and then nucleophilic substitution of chlorines by DEDT functions via a SN2 mechanism. The study was performed with a Kieselgel S silica which was initially chlorinated in surface; either by direct chlorination of silanols with thionyl chloride; or by using a condensation reaction between silanols and a chlorofunctional trialkoxysilane reagent; 4-(chloromethyl) phenyltrimethoxysilane and chloromethyltriethoxysilane; respectively. Three types of DEDT-functionalized silica microparticles were prepared with a good control of the reactions; and then characterized by solid-state 13C and 29Si CP/MAS NMR. Their ability to initiate MMA photopolymerization was studied. The kinetics of MMA photopolymerization was followed by HPLC and 1H-NMR. Whatever the silica used the grafting progresses very slowly. On the other hand; the conversion of MMA in PMMA grafts is depending on the structure of the DEDT-functionalized Kieselgel S used. Poly(methyl methacrylate)-grafted silica microparticles bearing high length grafts (DPn about 100) were synthesized. © 2008 Wiley Periodicals; Inc;
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页码：2113 / 2127
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