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Received May 6, 2010
Accepted June 8, 2010
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페놀의 수산화 반응에 사용한 TS-1 촉매의 효과적인 재생 방법(소성 온도 의존성)
Regeneration of TS-1 Catalyst During Phenol Hydroxylation (Calcination temperature dependence)
1한국화학연구원 그린화학연구단, 305-600 대전광역시 유성구 장동 100 2서강대학교 화공생명공학과, 121-742 서울시 마포구 신수동 1 3선경워텍(주), 689-896 울산광역시 울주군 온산읍 화산리 322
1Green Chemistry Division, KRICT, P.O. Box 107, Yusung-gu, Daejeon 305-600, Korea 2Department of Chemical and Biomolecular Engineering, Sogang University, 1 Sinsu-dong, Mapo-gu, Seoul 121-742, Korea 3Sunkyung Watech, 322, Hwasan-ri, Onsan-eup, Ulju-gun, Ulsan 689-896, Korea
chulwee@krict.re.kr
Korean Chemical Engineering Research, December 2010, 48(6), 679-683(5), NONE Epub 11 January 2011
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Abstract
본 연구에서는 과산화수소수에 의한 페놀의 수산화 반응에서 사용한 TS-1 촉매를 효과적으로 재사용할 때, 소성 온도가 촉매의 특성에 미치는 영향에 대해서 연구하였다. TS-1 촉매를 5회 재생시켜 반복 사용하였는데, 매회 마다 550 ℃ 및 700 ℃에서 각각 소성하였다. Fresh한 촉매의 페놀 전환율은 22.9%이었는데, 550 ℃에서 소성한 촉매에서는 5회 재생하였을 때 15.1%로 감소하였고, 700 ℃에서 소성한 촉매는 5회 재생하였을 때 18.8%로 감소하였다. 그리고 카테콜/하이드로퀴논의 생성비가 550 ℃에서 5회 재생 후에는 1.45, 700 ℃에서 5회 재생 후에는 1.2가 되었다. 소성 온도에 따른 재생 전·후 촉매에 대한 XRD, UV-vis spectra, N2 흡착/탈착 시험, TGA 등과 같은 특성 분석 및 촉매 성능(페놀전환율 및 생성물의 선택도)을 비교함으로써 촉매의 비활성화 원인을 예측하였다.
In this study, calcination temperature dependence of TS-1 catalyst was investigated in the hydroxylation of phenol with hydrogen peroxide during the regeneration of catalyst. Catalyst was regenerated 5 times by calcining at 550 ℃ and 700 ℃, respectively. When the catalyst was regenerated at 550 ℃ after 5th regeneration phenol conversion was decreased from 22.9% to 15.1% and at 700 ℃ after 5th regeneration phenol conversion was decreased from 22.9% to 18.8%. For formation ratio of catechol/hydroquinone was increased from 1.28 to 1.45 after 5th regeneration at 550 ℃, and from 1.28 to 1.20 after 5th regeneration at 700 ℃. The main reasons for deactivation of the catalyst were suggested by analyzing chemical/physical properties with XRD, UV-vis spectra, N2 adsorption/desorption and TGA, and evaluating the catalytic activity such as phenol conversion and product selectivity.
Keywords
References
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