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Received October 24, 2010
Accepted November 12, 2010
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실란 커플링제에 의해 표면이 개질된 실리카 나노입자의 분광학적 분석
Spectroscopic Analysis of Silica Nanoparticles Modified with Silane Coupling Agent
계명대학교 화학공학과, 704-701 대구광역시 달서구 신당동 1000
Department of Chemical Engineering, Keimyung University, 1000 Sindang-dong, Dalseo-gu, Daegu 704-701, Korea
Korean Chemical Engineering Research, April 2011, 49(2), 181-186(6), NONE Epub 12 April 2011
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Abstract
본 연구에서는 실리카 나노 입자의 표면 개질을 위해 실란 커플링제인 3-(trimethoxysilyl)propylmethacrylate(MPS)를 사용하여 표면 개질 반응을 수행하였다. 용매의 pH, MPS의 가수 분해 반응시간, 표면 개질 반응시간 및 실리카 표면의 실라놀기(Si-OH)에 대한 MPS의 몰 비를 변화하여 각각의 반응조건이 실리카 표면개질 반응에 미치는 영향을 연구하였다. 개질반응 후 Fourier Transform Infrared Spectroscopy(FTIR), 원소분석(EA) 및 고체 상태 cross-polarization magic angle spinning(CP/MAS) Nuclear Magnetic Resonance Spectroscopy(NMR)법을 사용하여 표면이 개질된 실리_x000D_
카 입자들의 분석을 수행하였다. 연구 결과 용매의 pH가 4.5일 때 MPS가 단량체 형태로 실리카 표면의 실라놀기와 반응하고 이외의 pH에서는 MPS가 이량체, 삼량체 혹은 사량체의 올리고머 형태로 실리카의 실라놀기와 반응함이 우세함을 나타내었다. 가수분해반응 시간을 30분에서 90분으로 증가시키면 MPS가 올리고머 형태로 실리카 표면의 실라놀기와 반응하는 것이 우세하고, 투입한 MPS 몰 비의 증가도 MPS가 올리고머 형태로 실리카 표면의 실라놀기와 반응하는 것이 우세함을 나타내었다.
In this study, we used 3-(trimethoxysilyl)propylmethacrylate(MPS) silane coupling agent for surface modification of silica nanoparticles. We studied effects of reaction conditions such as solvent pH, MPS hydrolysis time, reaction time, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, on the surface modification reactions of silica nanoparticles. Fourier Transform Infrared Spectroscopy(FTIR), Elemental Analysis(EA) and solid state crosspolarization_x000D_
magic angle spinning(CP/MAS) Nuclear Magnetic Resonance Spectroscopy(NMR) techniques were used to determine the type and the degree of surface modification. We found MPS reacts preferentially with Si-OH groups of the silica nanoparticles as monomeric form at solvent pH = 4.5. But increasing hydrolysis time of MPS from 30 mins to 90 mins, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, we found that MPS reacts preferentially with Si-OH groups of the silica nanoparticles as oligomeric form.
Keywords
References
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Park HK, Park KY, Korean Chem. Eng. Res., “Dry synthesis of Nearly Monodisperse Spherical Silica,”, 45(6), 677 (2007)
Song SA, “Surface Modification of Nanosize Fumed Silica,” Master’s degree Dissertation, Korea Advanced Institute of Science and Technology, Republic of Korea, Daejeon (2001)
Park SJ, Cho KS, Polym.(Korea), “Filler-Elastomer Interactions. 8. Influence of Fluorinated Nanoscaled Silicas on Mechanical Interfacial Properties and Thermal Stabilities of Polyurethane Matrix Composites.", 27(2), 91 (2003)
Rosen MR, J. Coating Tech., “From Treating Solution to Filler Surface and Beyond.", 50(644), 70 (1987)
Oh ES, Yang YC, Joeng SB, Chae YB, Yoon PR, Korean Society for Geosystem Engineering., “Surface Properties of Silica Treated with Silane Coupling Agents,”, 39(2), 88 (2002)
Arkles B, Chemtech., “Tailoring Surfaces with Silanes.", 7, 766 (1977)
Technical Bulletin Pigments No. 11, “Basic Characteristics of Aerosil,” Evonik Degussa Corp.
Xie XQ, Ranade SV, DiBenedetto AT, Polymer, 40(23), 6297 (1999)
Innocenzi P, Brusatin G, J. of Non-Crystalline Solids., “A Comparative FTIR Study of Thermal and Photo-polymerization Processes in Hybrid Sol-gel Filmes,”, 333, 137 (2004)
Shin Etsu Silicone: “Silane Coupling Agents,” Catalog.
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Joseph R, Zhang SM, Ford WT, Macromolecules, “Structure and Dynamics of a Colloidal Silica-poly(methyl methacrylate) Composite by 13C and 29Si MAS NMR Spectroscopy.", 29(4), 1305 (1996)
Luo J, Lannutti J, Seghi R, J. Adhesion Sci. Technol., “Solid-state NMR Evaluation of the Silane Structure on Nanoporous Silica Fillers,”, 15(3), 267 (2001)
Chung JS, Kim DJ, Ahn WS, Ko JH, Cheong WJ, Korean J. Chem. Eng., “Synthesis, Characterization, and Applications of Organicinorganic Hybrid Mesoporous Silica.", 21(1), 132 (2004)
