Search / Korean Journal of Chemical Engineering
HWAHAK KONGHAK,
Vol.40, No.4, 415-421, 2002
Water-in-Carbon Dioxide 마이크로에멀젼에서 나노 크기의 이산화티탄 합성 및 p-니트로페놀의 광분해에 대한 연구
Study on the Synthesis of TiO2 Nanoparticles in a Water-in-Carbon Dioxide Microemulsion and Their Photocatalytic Activity for p-Nitrophenol Degradation
CO2에 용해 능력이 우수한 PFPE-NH4(ammonium carboxylate perfluoro polyether) 및 PDMAEMA(poly(2-(dimethylamine)-ethyl methacrylate))-b-PFOMA(poly(1H, 1H, 2H, 2H-perfluoroocthyl methacrylate)) 계면활성제를 사용하여 W/C 마이크로에멀젼에 의해 나노 크기의 TiO2를 제조하였다. TGA-DTA, FT-IR, XRD, TEM 등을 이용하여 나노 입자 제조시 Wo(H2O/surfactant molar ratio)비에 따른 입자의 크기 및 결정성 등 물리적 성질을 조사하였다. 또한 제조된 TiO2 나노 입자의 광촉매적 특성을 알아보기 위해 회분식 반응장치를 이용하여 p-니트로페놀의 광활성을 조사하였다. 제조된 TiO2 나노 입자는 소성온도 250-450 ℃ 범위에서 유기물질과 수산화물이 분해되어 450 ℃이상 비결정 구조에서 anatase 구조로 상 전이 되었다. W/C 마이크로에멀젼에서 제조된 나노 입자의 결정성 및 결정크기는 Wo 비가 증가할수록 증가하였다. p-니트로페놀의 광분해반응에서 반응성은 결정크기에 영향을 받았으며, 결정의 크기가 작을수록 반응성이 증가하였다.
Titania nanoparticles were prepared by controlled hydrolysis of titanium tetraisopropoxide(TTIP) in PFPE-NH4(ammonium carboxylate perfluoropolyether) and PDMAEMA(poly(2-(dimethylamino)ethyl methacrylate))-b-PFOMA(poly(1H, 1H, 2H, 2H-perfluoroocthyl methacrylate))/Water-in-CarbonDioxide Microemulsions. The physical properties, such as crystallite size and crystallinity according to Wo ratio have been investigated by TGA-DTA, FT-IR, XRD and TEM. In addition, the photocatalytic degradation of p-nitrophenol has been studied by using batch reactor in the presence of UV light in order to compare the photocatalytic activity of prepared nanosized titania. The residual organic compound and hydroxyl group were completely removed in calcination temperature from the 250-450 ℃ and the amorphous phase changed into anatase structure above 450 ℃. The crystallinity and crystallite size of nanoparticles produced in water-in-carbon dioxide microemulsions increased with an increase of the Wo ratio. In the photocatalytic degradation of p-nitrophenol, the photocatalytic activity is mainly determined by the crystallite size of titania and the reaction rate increased with an decrease of crystallite size.
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