Korean Chemical Engineering Research

The Korean Institute of Chemical Engineers (한국화학공학회)
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Preparation of Self-repairing Polymer-modified Waterproofing Asphalt-montmorillonite Composite: 2. Validation of Optimized Silylation of Montmorillonite (K-10) Using 3-aminopropyltriethoxysilane

자가치유성을 갖는 고분자개질 방수아스팔트-몬모릴로나이트 composite 제조: 2. 3-aminopropyltriethoxysilane에 의한 몬모릴로나이트(K-10)의 실란화 최적화 검증

  • Lee, Eun Ju (Department of Chemical Engineering, Daegu University) ;
  • Lee, Jong Hoon (Department of Chemical Engineering, Daegu University) ;
  • Lim, Kwang-Hee (Department of Chemical Engineering, Daegu University)
  • Received : 2017.04.21
  • Accepted : 2017.05.22
  • Published : 2017.06.01
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Abstract

In preparation of self-repairing polymer-modified waterproofing asphalt-montmorillonite (MMT) composite, silylation-modification characteristics of cation ($Na^+$) exchanged K-10 (Na-MMT-K) using 3-aminopropyltriethoxysilane (APS) were studied and the optimal conditions of its silylation-modification process were proposed by use of the results of instrumental analysis, including FTIR, XRD, NMR and TGA, on silylation-modified Na-MMT-K (S-Na-MMT-K) under various conditions. According to FTIR analysis on S-Na-MMT-K, its peak-strengths of Si-O, -$NH_2$, -$CH_2$- and -OH, correlated with APS silylation-modification reaction, were compared each other. As a result, its optimal conditions including APS-MMT reacting period, APS-stirring period prior to APS-MMT reaction, APS concentration and reaction temperature were turned out to be 2~3 h, 20 min, 7.5 w/v% and $50^{\circ}C$, respectively. In addition, the optimal conditions induced from the results of TGA were also nearly consistent to those according to the results of FTIR analyses. These optimal conditions were turned out to be almost consistent to those drawn according to a criterion from XRD results suggested previously by Lee et al., by which the criterion was validated.

자가치유성을 갖는 고분자개질 빙수아스팔트-몬모릴로나이트(MMT) composite 제조를 위하여 양이온($Na^+$)교환 처리된 K-10 (Na-MMT-K)에 대한 3-aminopropyltriethoxysilane (APS) 개질의 특성을 규명하고 적정개질조건을 FTIR, XRD, NMR 및 TGA 등의 분석을 통하여 제시되었다. APS 개질된 Na-MMT-K (S-Na-MMT-K)에 대한 FTIR 분석에서 실란화 반응과 관련된 실록산 결합(Si-O), 아민기, -$CH_2$- 및 -OH 기의 피크의 세기를 비교하였다. 그 결과로서 적정 반응시간, 적정교반시간, 적정농도 및 적정반응온도는 각각 2~3 h, 20 min, 7.5 w/v% 및 $50^{\circ}C$가 도출되었다. 또한 TGA 결과로부터 도출된 적정개질조건도 FTIR 분석에서 도출한 적정개질조건과 거의 일치하였다. 이 도출된 적정개질조건들은 Lee 등의 XRD 분석에서 제시된 기준(criterion)에 의해 도출된 적정반응시간, 적정교반시간, 적정 APS농도 및 적정반응온도와 거의 일치하였다. 따라서 XRD 분석에서 제시된 기준(criterion)이 검증되었다.

Keywords

References

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