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: 1. Silylation Characteristics of Montmorillonite (K-10) Using 3-aminopropyltriethoxysilane and its Optimal Condition According to a Criterion by XRD Analysis

자가치유성을 갖는 고분자개질 방수아스팔트-몬모릴로나이트 composite 제조: 1. 3-aminopropyltriethoxysilane에 의한 몬모릴로나이트(K-10)의 실란화 특성 및 XRD 분석의 기준에 따른 최적화

  • 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 XRD analysis on silylation-modified Na-MMT-K (S-Na-MMT-K) under various conditions. According to XRD results, it was confirmed that peaks of Na-MMT-K were simultaneously consistent with those of K-10 and natural or Ca-MMT modified Na-MMT. Similarly, S-Na-MMT-K was observed to have two basal spacings ($d_{001}$), among which the area-ratio of a secondary (001) peak ($2{\theta}=3.9{\sim}4.2^{\circ}$) to a primary (001) peak ($2{\theta}{\sim}8.838^{\circ}$) was suggested to be a criterion to represent a degree of APS silylation-modification. Then, the optimal conditions on APS-stirring period prior to APS-MMT reaction, APS-MMT reaction period, APS concentration and reaction temperature at the highest area-ratio were turned out to be 20 min, 2~3 hr, 7.5 w/v% and $50^{\circ}C$, respectively.

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 XRD 분석을 통하여 제시하였다. APS 개질된 Na-MMT-K (S-Na-MMT-K)에 대한 XRD 분석결과로서, Na-MMT-K는 K-10과 자연유래 또는 Ca-MMT에서 개질된 Na-MMT의 피크 특성들을 동시에 가지는 것이 확인되었다. 또한 S-Na-MMT-K도 동시에 두 개의 저면간격($d_{001}$) 특성들을 가짐이 관찰되었고, 그 중에서 부(001) 피크($2{\theta}=3.9{\sim}4.2^{\circ}$)와 주(001)피크($2{\theta}=8.838^{\circ}$ 근처)의 면적비(%)를 APS개질도에 대한 기준(criterion)으로 제시하였다. Na-MMT-K의 APS개질에 대한 반응전 APS 적정용해시간, 적정반응시간, 적정 APS농도 및 적정반응온도는 각각 20 min, 2~3시간, 7.5 w/v% 및 $50^{\circ}C$가 도출되었다.

Keywords

References

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