Elastomers and Composites

The Rubber Society of Korea (한국고무학회)
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Characterization and Formation of Chemical Bonds of Silica-Coupling Agent-Rubber

실리카-커플링제-고무의 화학 결합 형성과 특성 분석

  • Received : 2014.08.19
  • Accepted : 2014.08.26
  • Published : 2014.09.30
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Abstract

Reaction between silica and silane coupling agent without solvent was investigated using transmission mode Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). Bis[3-(triethoxysilylpropyl) tetrasulfide] (TESPT) was used as a silane coupling agent. After removing the unreacted TESPT, formation of chemical bonds was analyzed using FTIR and content of reacted TESPT was determined using TGA. Content of the coupling agent bonded to silica increased with increase in the coupling agent content, but the oligomers were formed by condensation reaction between coupling agents when the coupling agent was used to excess. In order to identify bonds formed among silica, coupling agent, and rubber, a silica-coupling agent-BR model composite was prepared by reaction of the modified silica with liquid BR of low molecular weight and chemical bond formation of silica-coupling agent-BR was investigated. Unreacted rubber was removed with solvent and analysis was performed using FTIR and TGA. BR was reacted with the coupling agent of the modified silica to form chemical bonds. Polarity of silica surface was strikingly reduced and particle size of silica was increased by chemical bond formation of silica-coupling agent-BR.

용매를 사용하지 않고 실리카와 실란커플링제의 반응을 투과 방식 휴리에 변환 적외선 분광법(FTIR)과 열중량 분석법(TGA)을 이용하여 조사하였다. 실란커플링제로 bis[3-(triethoxysilylpropyl) tetrasulfide] (TESPT)를 사용하였다. 미반응 TESPT를 제거한 후, FTIR로 화학 결합 형성을 분석하였고 TGA로 반응한 TESPT 함량을 결정하였다. 커플링제의 함량이 증가할수록 실리카에 결합한 커플링제의 양이 증가하였으나, 커플링제를 과량으로 첨가하면 커플링제 간의 축합반응에 의해 올리고머를 형성하였다. 실리카와 커플링제 그리고 고무의 결합을 확인하기 위하여 개질 실리카와 저분자량 액상 BR을 반응시켜 실리카-커플링제-BR 모델 복합체를 제조하여 화학 결합 형성을 조사하였다. 미반응 고무는 용매를 사용하여 제거하였고 FTIR과 TGA로 분석하였다. BR은 개질 실리카의 커플링제와 반응하여 화학 결합을 형성하였다. 실리카-커플링제-BR의 화학 결합 형성으로 인해 실리카 표면의 극성은 크게 낮아졌고 실리카 입자 크기는 커지는 효과를 보였다.

Keywords

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