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Issue
Korean Chemical Engineering Research,
Vol.49, No.2, 181-186, 2011
실란 커플링제에 의해 표면이 개질된 실리카 나노입자의 분광학적 분석
Spectroscopic Analysis of Silica Nanoparticles Modified with Silane Coupling Agent
송성규, 김정혜, 황기섭, 하기룡
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 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 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: Silica; Silane Coupling Agent; FTIR; NMR
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[Cited By]
  1. Joo J, Kim HS, Kim JT, Yoo HJ, Lee JR, Cheong IW, Korean Chemical Engineering Research, 50(2), 371, 2012
  2. Sim HS, Kim GS, Shin JH, Lee KH, Polymer(Korea), 36(3), 268, 2012
  3. Ryu HS, Lee YS, Lee JC, Ha K, Polymer(Korea), 37(3), 308, 2013
  4. Choi BK, Kim HG, Seo MK, Park SJ, Applied Chemistry for Engineering, 25(5), 520, 2014
  5. Seo B, Park S, Kim S, Ha KR, Polymer(Korea), 40(3), 421, 2016
  6. Yang Y, Park S, Kim H, Hwang KS, Ha KR, Korean Chemical Engineering Research, 55(1), 60, 2017
  7. Yang JH, Song KC, Korean Chemical Engineering Research, 55(6), 754, 2017
  8. Yang YK, KiM HN, Lim KH, Ha KR, Polymer(Korea), 42(1), 147, 2018
  9. Nam YS, Yu JK, Park GW, Kim HJ, Kim DG, Kim MG, Hyun K, Polymer(Korea), 43(4), 567, 2019
  10. Sung SH, Lee MJ, Cho YS, Korean Chemical Engineering Research, 59(4), 596, 2021
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