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Synthesis and Crystallographic Studies of Highly NH4+-exchanged, Fully Deaminated, and Fully Tl+-exchanged Zeolite Y (FAU, Si/Al = 1.56)

등록일
2009년 8월 14일 12시 36분 59초
접수번호
0905
발표코드
34P87포 이곳을 클릭하시면 발표코드에 대한 설명을 보실 수 있습니다.
발표시간
목 <발표Ⅰ>
발표형식
포스터
발표분야
물리화학
저자 및
공동저자
서성만, 임우택
안동대학교 응용화학과, Korea
Single crystals of zeolite Y, |Na75|[Si117Al75O384]-FAU, with diameters up to 0.30 mm were grown from gels; Si/Al = 1.56. They were ion exchanged and fully dehydrated to generate |(NH4)67H5Na3|[Si117Al75O384]-FAU (crystal 1, partially deaminated), |H72Na3|[Si117Al75O384]-FAU (crystal 2, fully deaminated at 473 K) and |Tl75|[Si117Al75O384]-FAU (crystal 3). Their structures were determined crystallographically at 294 K using synchrotron X-radiation in the cubic space group Fd3-m. They were refined to the final error indices R1/wR2 = 0.037/0.126, 0.055/0.190, and 0.044/0.121 using 884, 723, and 851 reflections with Fo > 4σ(Fo) for crystals 1, 2, and 3, respectively. In crystal 1, 67 NH4+ and 3 Na+ ions per unit cell are found at four different crystallographic sites. Six NH4+ ions were found at the centers of double 6-rings (site I; N···O = 2.888(3) Å). Filling site I' are 32 NH4+ ions (N···O = 2.774(5) Å); each is recessed 1.59 Å into the sodalite cavity from the plane of the three oxygens to which it bonds. Filling site II in the supercages are 29 NH4+ and 3 Na+ ions, each of which extends 1.69 Å and 1.10 Å, respectively, into the supercage from its 3-oxygen plane (N···O = 2.818(5) Å, Na-O = 2.512(19) Å). The remaining 5 of the 72 NH4+ ions originally present per unit cell have apparently been deaminated by vacuum dehydration at 294 K. NH4+ ions simultaneously occupy sites I and I' as K+ ions did in |K71|[Si121Al71O384]-FAU; the internitrogen distance is 3.36 Å. In crystal 2, three Na+ ions per unit cell are found at site I' (Na-O = 2.207(13) Å); no other cations were found so the deamination of NH4+ is complete at 473 K. In crystal 3, 30, 30, 9, 4, and 2 Tl+ ions were found at sites I', II, and three sites III' per unit cell, respectively. The total, 75, agrees with the results of EDX analysis to establish the framework composition (the Si/Al ratio) of these crystals.

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