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Search / Korean Journal of Chemical Engineering
HWAHAK KONGHAK,
Vol.40, No.1, 1-8, 2002
티타늄 함유 제올라이트 베타 촉매의 합성, 물성조사 및 반응특성 연구
Synthesis, Characterization and Catalytic Properties of Titanium-containing Zeolite Beta Catalysts
윤보상, 안희승
티타늄 함유 제올라이트 베타(Ti-beta) 촉매를 5가지 수열합성 방법과 알콕사이드 또는 메탈로센을 티타늄 원으로 이용한 2가지 후처리 grafting방법으로 제조하여 제조 방법에 따른 물성 차이를 연구하였다. 모든 촉매의 UV-Vis 스펙트럼에는 제올라이트 격자구조 내에 고립되어 존재하는 티타늄에 해당하는 220 nm의 흡수밴드가 관찰되었으며, grafting 시킨 경우 나노 크기의 TiO2 cluster에 기인하는 240-320 nm의 흡수 밴드가 함께 관찰되었다. 결정 입자는 dry-gel 방법과 seed를 사용한 경우 50 nm이하, 액상 전구체의 수열합성에 의한 기존 방법이나 TiO2/SiO2 xerogel 전구체를 사용한 경우는 200 nm, 불산 분위기 합성에서는 2-5 μm의 평균 입자 크기를 나타내었으며, 분자체 결정에 대한 수율은 Ti-beta(F-)>Ti-beta(seed)>Ti-Al-beta(xerogel)>Ti-Al-beta(dry-gel)>Ti-Al-beta(conventional)의 순서로 조사되었다. Cyclohexene의 epoxidation 반응은 Ti-Al-beta(conventional), Ti-beta(seed)>Ti-Al-beta(xerogel), Ti-Al-beta(dry-gel)>Ti-beta(F-)의 순서로 전화율이 나타났으며, epoxide에 대한 선택성은 Ti-Al-beta(xerogel)
A critical evaluation of synthesis recipes reported for the large pore zeolite Ti-beta was conducted after a series of titanium containing zeolite beta were prepared by five different hydrothermal synthesis and in two post-synthetic grafting methods using alkoxide or metallocene as a titanium precursor. All Ti-beta prepared by different synthesis routes showed a narrow charge transfer band centered at ca. 220 nm in UV-Vis spectra, typical of Ti sites isolated in zeolite framework. For those prepared by grafting, the absorption band at 240-320 nm attributed to nano-sized TiO2 clusters were also detected. Particle size of Ti-Al-beta(dry-gel) and Ti-beta(seed) were below 20 nm; Ti-Al-beta(conventional) and Ti-Al-beta(xerogel) below 200 nm; and Ti-beta(F-) ca. 2-5 μm. Yield of zeolite crystals decreased in the order Ti-beta(F-)>Ti-beta (seed)>Ti-Al-beta(xerogel)>Ti-Al-beta(dry-gel)>Ti-Al-beta(conventional). For cyclohexene epoxidation, conversions varied in the order Ti-Al-beta (conventional), Ti-beta(seed)>Ti-Al-beta(xerogel), Ti-Al-beta(dry-gel)>Ti-beta(F-) with epoxide selectivity in the order Ti-Al-beta(xerogel)
Keywords: Ti-beta; Hydrothermal Synthesis; Grafting; Cyclohexene Epoxidation
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[Cited By]
  1. Ban HJ, Lee KY, Lee JK, Chung ST, Ahn WS, Korean Chemical Engineering Research, 44(2), 121, 2006
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