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Received October 1, 2014
Accepted December 26, 2014
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MWCNT 표면에 Michael 부가 반응으로 자유 라디칼 중합 가능한 Methacrylate기 도입에 대한 최적 개질 조건
Optimum Conditions for Introducing Free Radical Polymerizable Methacrylate Groups on the MWCNT Surface by Michael Addition Reaction
계명대학교 화학공학과, 704-701 대구광역시 달서구 달구벌대로 1095
Department of Chemical Engineering, Keimyung University, 1095 Dalgubeol-daero, Dalseo-gu, Daegu 704-701, Korea
Korean Chemical Engineering Research, February 2015, 53(1), 83-90(8), 10.9713/kcer.2015.53.1.83 Epub 3 February 2015
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Abstract
본 연구에서는 multi-walled carbon nanotube (MWCNT) 표면에 자유 라디칼 중합 가능한 methacrylate기를 다량으로 도입하기 위한 연구를 수행하였다. 먼저, MWCNT 표면에 카르복실기(-COOH)를 도입하기 위하여 황산과 질산의 혼산으로 초음파로 처리하면서 2시간 산화시켜 MWCNT-COOH를 합성하였다. 합성된 MWCNT-COOH를 염화티오닐(thionyl chloride)와 반응시켜 MWCNT-COCl을 합성하고, triethylenetetramine (TETA)와 반응시켜 MWCNT-NH2를 합성하였다. 합성된 MWCNT-NH2와 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM)의 투입 몰 비를 변화시키_x000D_
면서 Michael 부가 반응으로 MWCNT 표면에 methacrylate기가 도입된 MWCNT-AHM을 합성하였다. MWCNT의 표면 개질정도는 fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA)와 원소분석(elemental analysis, EA) 분석을 통해 개질 반응의 진행 정도와 최적 개질 조건을 확인하였다. 그 결과 MWCNT-NH2에 접목되어 있는 TETA에 대하여 AHM의 반응 몰 비를 1:10로 하고 8시간 반응시켰을 때 methacrylate기가 가장 많이 도입되는 조건임을 확인하였다.
In this study, we investigated optimum conditions for the introduction of a lot of free radical polymerizable methacrylate groups on the multi-walled carbon nanotube (MWCNT) surface. Carboxyl groups were introduced first on MWCNT surfaces by treating with a mixture of sulfuric acid and nitric acid with ultrasonic bath for 2 hours, and oxidized MWCNTs were reacted further with thionyl chloride followed by triethylenetetramine (TETA) to introduce amino groups on_x000D_
the oxidized MWCNT surface, to make MWCNT-NH2. To introduce free radical polymerizable methacrylate groups on the MWCNT-NH2, MWCNT-NH2 was reacted with 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) by Michael addition reaction. We investigated progress of modification reactions for MWCNT by fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and elemental analysis (EA). We found maximum degree of Michael addition reactions between AHM and TETA grafted on MWCNT-NH2 for 10:1 mol ratio and 8 hour reaction time in our reaction conditions.
Keywords
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Shao L, Bai YP, Huang X, Gao ZF, Meng LH, Huang YD, Ma J, Mater. Chem. Phys., 116(2-3), 323 (2009)
Lee SM, Ha KR, Polymer(Korea), 38(2), 1 (2013)
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Brindaban CR, Suvendu SD, Alakananda H, ARKIVOC, 7, 76 (2002)
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Larkin P, Infrared and Raman Spectroscopy: Principles and Spectral Interpretation, 1st ed., Elsevier, New York, 107 (2011)
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Socrates G, Infrared Characteristic Group Frequencies: Table and Chart, 2nd ed., John Wiley & Sons, New York, 105 (1994)
