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Language: korean

Conflict of Interest: In relation to this article, we declare that there is no conflict of interest.

Publication history: Received April 21, 2017
Accepted May 22, 2017

This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/bync/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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

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

이은주 이종훈 박유진 윤용근¹ 임광희^†

Eun Ju Lee Jong Hoon Lee You Jin Park Yong Keun Yoon¹ Kwang-Hee Lim^†

대구대학교 화학공학과, 38453 경상북도 경산시 진량읍 대구대로 201 ¹㈜페트로산업, 38460 경상북도 경산시 진량읍 공단2로 99

Department of Chemical Engineering, Daegu University, 201, Daegudae-ro, Jillyang-eup, Gyeongsan, Gyeongbuk, 38453, Korea ¹Petro Industry Co., Ltd, 99, Gongdan2-ro, Jillyang-eup, Gyeongsan, Gyeongbuk, 38460, Korea

khlim@daegu.ac.kr

Korean Chemical Engineering Research, June 2017, 55(3), 401-408(8), 10.9713/kcer.2017.55.3.401 Epub 2 June 2017

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Abstract

자가치유성을 갖는 고분자개질 빙수아스팔트-몬모릴로나이트(MMT) composite 제조를 위하여 양이온(Na+)교환 처 리된 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-K 도 동시에 두 개의 저면간격(d001) 특성들을 가짐이 관찰되었고, 그 중에서 부(001) 피크(2θ=3.9~4.2°)와 주(001)피크 (2θ=8.838° 근처)의 면적비(%)를 APS개질도에 대한 기준(criterion)으로 제시하였다. Na-MMT-K의 APS개질에 대한 반 응전 APS 적정용해시간, 적정반응시간, 적정 APS농도 및 적정반응온도는 각각 20 min, 2~3시간, 7.5 w/v% 및 50 °C 가 도출되었다.

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 (d001), among which the area-ratio of a secondary (001) peak (2θ=3.9~4.2°) to a primary (001) peak (2θ~8.838°) 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 °C, respectively.

Keywords

Montmorillonite Silylation-modification Optimal condition Criterion

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