나노크기의 티타늄실리카라이트-1(TS-1) 제올라이트를 결정성장 관찰과 결정크기의 조절이 가능한 상압, 100℃ 이하에서 수열합성법으로 합성하였다. 반응온도가 낮아질수록 유도기간이 길어졌고 결정화속도와 얻어진 최종 입자크기가 감소하였다. 각 합성온도에서 결정화 진행 중의 평균 결정크기는 시간에 따라 직선적인 증가 형태를 나타내었고 결정화에 대한 겉보기 활성화에너지는 86.7kJ/mol였다. 80℃에서 반응시 60시간에 약 50 nm의 결정성을 지닌 TS-1 입자들을 얻었다. 이러한 나노크기의 TS-1 제올라이트는 750℃까지 Ti이 골격에 치환된 MFI 구조를 갖고 있었으며 새로운 분야에 응용을 가능케 할 것이다.

Nano-sized titanium silicalite-1(TS-1) zeolite was synthesized by using hydrothermal synthesis at the atmospheric pressure and the temperatures lower than 100℃. This systhetic method makes it possible to control the particle size of TS-1. As the reaction temperature decreased, the induction period increased and the rate of crystallization and the final crystal size decreased. During the crystallization, average crystal size of TS-1 zeolite was linearly increased with reaction time. The apparent activation energy of crystallization was 86.7kJ/mol. When the reaction time was 70 hours at 80℃, average particle size of TS-1 with 50nm in diameter was obtained, which have TS-1 zeolite crystallinity up to 750℃. Nanosized TS-1 zeolite may be applicable to the new field of zeolite.

TS-1 Zeolite Nano Technology MFI Intergrowth ²⁹Si-CP/MAS NMR

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