Chemistry of inorganic compounds – Zeolite – Organic compound used to form zeolite
Reexamination Certificate
2001-03-20
2003-10-21
Sample, David (Department: 1755)
Chemistry of inorganic compounds
Zeolite
Organic compound used to form zeolite
C423S707000, C423S708000, C423S713000, C423S716000, C502S060000
Reexamination Certificate
active
06635233
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a CFI-type zeolite containing fourteen-membered ring pores useful as a conversion catalyst for organic compounds, a process for the preparation of the zeolite, a catalyst prepared from the zeolite, and a process for the conversion of organic compounds.
2. Description of Related Arts
The CFI-type zeolite is a zeolite containing novel fourteen-membered ring pores invented by Yoshikawa and Devis and also is called CIT-5. Processes for the synthesis and the structure of the zeolite are already disclosed by the following literatures:
Literature 1: WO99/08961
Literature 2:
Chemical Communications,
2179 (1997)
Literature 3:
Journal of Physical Chemistry, B,
102, 7139 (1998)
Literature 4:
Journal of Catalysis,
182, 463 (1999)
Literature 5:
Shokubai,
41, 380 (1999)
Literature 2 describes CIT-5 having a SiO
2
/Al
2
O
3
ratio of 50, but no physical shape thereof. Furthermore, the CIT-5 having a SiO
2
/Al
2
O
3
ratio of 50 could not be prepared according to the process as described therein. As described in Example 5 of literature 1, hydrothermal treatment of the reaction mixture having a known composition (LiOH/SiO
2
=0.1and methylsparteinium hydroxide/SiO
2
=0.2) only produces a mixture containing amorphous materials without forming a finely crystallized CFI-type zeolite from the reaction mixture having a SiO
2
/Al
2
O
3
ratio of 100. The other literatures describe no CIT-5 having a SiO
2
/Al
2
O
3
ratio lower than 100, and also no CIT-5 having an atomic ratio of silicon to a heteroatom that is 45 or less. In literature 1, the synthesis of CIT-5 is carried out by use of the reaction mixture having a Si/Zn ratio of 25, but it is not clear whether zinc is contained in the resulting zeolite.
The CFI-type zeolite (CIT-5) contains a fourteen-membered ring pore which is large of the pore sizes of zeolites, and is expected as a novel material for catalysts. However, the related art has been unable to introduce a number of heteroatoms into the framework of the zeolite, that is, producing only CIT-5 having a small number of catalytic active sites. CIT-5 has a monodimensional pore of fourteen-membered ring size. The monodimensional pore is inferior in diffusion to multi-dimensional pores, and therefore smaller crystals are useful as catalysts. However, the related art has been unable to prepare CIT-5 having a number of active sites and furthermore small crystal size.
SUMMARY OF THE INVENTION
The invention aims at providing CIT-5 having a number of active sites and small crystal size, and more concretely a CFI-type zeolite where the atomic ratio of silicon to the heteroatom is 45 or less, and the long axes of the crystals are 0.7 &mgr;m or less.
The first invention of the invention is the CFI-type zeolite characterized in that the atomic ratio of silicon to the heteroatom is 45 or less, and the long axes of the crystals are 0.7 &mgr;m or less.
The second invention is a process for preparing the CFI-type zeolite characterized in that a reaction mixture satisfying the following both conditions (1) and (2) is subjected to hydrothermal treatment:
(1) LiOH/SiO
2
<0.15 (in molar ratio)
(2) ROH/SiO
2
>0.2 (in molar ratio, ROH represents an alkylsparteinium hydroxide).
The third invention is a catalyst containing the aforesaid CFI-type zeolite.
The fourth invention is a process for the conversion of organic compounds characterized by allowing the aforesaid catalyst to contact with the organic compounds.
REFERENCES:
patent: 4496776 (1985-01-01), Edwards et al.
patent: 4549017 (1985-10-01), McEntire et al.
patent: 4613673 (1986-09-01), McEntire et al.
patent: 4675411 (1987-06-01), Sommer et al.
patent: 4686315 (1987-08-01), Beach et al.
patent: 5271922 (1993-12-01), Nakagawa
patent: WO-9908961 (1999-02-01), None
Kubota et al., “Synthetic investigation of CIT-5 catalyst,” Microporous and Mesoporous Materials, vol. 37, 2000, pp. 291-301.*
Yoshikawa et al., “Synthesis, Characterization, and Structure Solution of CIT-5, a New, High-Silica, Extra-Large-Pore Molecular Sieve,” J. Phys. Chem. B, vol. 102, 1998, pp. 7139-7147.*
Sita L., Xi, R., Yap, G., Liable-Sands, L., and Rheingold, A., “High Yield Synthesis and Characterization of Sn6(&mgr;3-O)4(&mgr;3-OSi(CH3)3)4,” 1997, J. Am. Chem. Soc., 119, 756-760.
K. Tsuji et al, “High-silica molecular sieve syntheses using the sparteine related compounds as structure-directing agents,”Microporous and Mesposorous Materials, Elsevier Science Publishing, New York, vol. 28, No. 3,, May 1999, pp. 461-469, XP004165647, ISSN: 1387-1811.
Martinez-Triguero J. et al., “The Catalytic Performance of 14-Membered Ring Zeolites”,Journal of Catalysis, Academic Press, Dulutj, MN, US, vol. 182, 1999, pp. 463-469, XP001000129, ISSN: 0021-9517.
Iwayama Kazuyoshi
Kato Hajime
Sakaguchi Shin-ichi
Uchiyama Naoyuki
Yoshikawa Masahito
Piper Rudnick LLP
Sample David
Toray Industries Inc.
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