Chemistry of inorganic compounds – Zeolite – Organic compound used to form zeolite
Reexamination Certificate
2002-12-26
2004-05-11
Sample, David R (Department: 1755)
Chemistry of inorganic compounds
Zeolite
Organic compound used to form zeolite
C423S718000, C423SDIG002
Reexamination Certificate
active
06733742
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to new crystalline molecular sieve SSZ-63, a method for preparing SSZ-63 using N-cyclodecyl-N-methyl-pyrrolidinium cation as a structure directing agent and the use of SSZ-63 in catalysts for, e.g., hydrocarbon conversion reactions.
2. State of the Art
Because of their unique sieving characteristics, as well as their catalytic properties, crystalline molecular sieves and zeolites are especially useful in applications such as hydrocarbon conversion, gas drying and separation. Although many different crystalline molecular sieves have been disclosed, there is a continuing need for new zeolites with desirable properties for gas separation and drying, hydrocarbon and chemical conversions, and other applications. New zeolites may contain novel internal pore architectures, providing enhanced selectivities in these processes.
Crystalline aluminosilicates are usually prepared from aqueous reaction mixtures containing alkali or alkaline earth metal oxides, silica, and alumina. Crystalline borosilicates are usually prepared under similar reaction conditions except that boron is used in place of aluminum. By varying the synthesis conditions and the composition of the reaction mixture, different zeolites can often be formed.
SUMMARY OF THE INVENTION
The present invention is directed to a family of crystalline molecular sieves with unique properties, referred to herein as “molecular sieve SSZ-63” or simply “SSZ-63”. Preferably, SSZ-63 is obtained in its'silicate, aluminosilicate, titanosilicate, germanosilicate, vanadosilicate or borosilicate form. The term “silicate” refers to a molecular sieve having a high mole ratio of silicon oxide relative to aluminum oxide, preferably a mole ratio greater than 100, including molecular sieves comprised entirely of silicon oxide. As used herein, the term “aluminosilicate” refers to a molecular sieve containing both alumina and silica and the term “borosilicate” refers to a molecular sieve containing oxides of both boron and silicon.
In accordance with this invention, there is provided a molecular sieve having a mole ratio greater than about 15 of (1) an oxide of a first tetravalent element to (2) an oxide of a trivalent element, pentavalent element, second tetravalent element different from said first tetravalent element or mixture thereof and having, after calcination, the X-ray diffraction lines of Table II.
Further, in accordance with this invention, there is provided a molecular sieve having a mole ratio greater than about 15 of (1) an oxide selected from silicon oxide, germanium oxide and mixtures thereof to (2) an oxide selected from aluminum oxide, gallium oxide, iron oxide, boron oxide, titanium oxide, indium oxide, vanadium oxide and mixtures thereof and having, after calcination, the X-ray diffraction lines of Table II below. It should be noted that the mole ratio of the first oxide or mixture of first oxides to the second oxide can be infinity, i.e., there is no second oxide in the molecular sieve. In these cases, the molecular sieve is an all-silica molecular sieve or a germanosilicate.
The present invention further provides such a molecular sieve having a composition, as synthesized and in the anhydrous state, in terms of mole ratios as follows:
YO
2
/W
c
O
d
15-∞
M
2/a
/YO
2
0.01-0.03
Q/YO
2
0.02-0.05
wherein Y is silicon, germanium or a mixture thereof; W is aluminum, gallium, iron, boron, titanium, indium, vanadium or mixtures thereof; c is 1 or 2; d is 2 when c is 1 (i.e., W is tetravalent) or d is 3 or 5 when c is 2 (i.e., d is 3 when W is trivalent or 5 when W is pentavalent); M is an alkali metal cation, alkaline earth metal cation or mixtures thereof; n is the valence of M (i.e., 1 or 2); and Q is N-cyclodecyl-N-methyl-pyrrolidinium cation.
In accordance with this invention, there is also provided a molecular sieve prepared by thermally treating a zeolite having a mole ratio of an oxide selected from silicon oxide, germanium oxide and mixtures thereof to an oxide selected from aluminum oxide, gallium oxide, iron oxide, boron oxide, titanium oxide, indium oxide, vanadium oxide and mixtures thereof greater than about 15 at a temperature of from about 200° C. to about 800° C., the thus-prepared zeolite having the X-ray diffraction lines of Table II. The present invention also includes this thus-prepared molecular sieve which is predominantly in the hydrogen form, which hydrogen form is prepared by ion exchanging with an acid or with a solution of an ammonium salt followed by a second calcination.
Also provided in accordance with the present invention is a method of preparing a crystalline material comprising (1) an oxide of a first tetravalent element and (2) an oxide of a trivalent element, pentavalent element, second tetravalent element which is different from said first tetravalent element, or mixture thereof and having mole ratio of the first oxide to the second oxide greater than 15, said method comprising contacting under crystallization conditions sources of said oxides and a structure directing agent comprising N-cyclodecyl-N-methyl-pyrrolidinium cation. The method of this invention can be used to synthesize crystalline materials having, after calcination, the X-ray diffraction lines of Table II, as well as crystalline materials having the BEA* crystal structure.
REFERENCES:
patent: 6080382 (2000-06-01), Lee et al.
patent: 6649141 (2003-11-01), Camblor Fernandez et al.
patent: 2003/0185751 (2003-10-01), Chester et al.
patent: WO-2000/37360 (2000-06-01), None
patent: WO-2002/030819 (2003-10-01), None
Corma et al., “Pure Polymorph C of Zeolite Beta Synthesized by Using Framework Isomorphous Substitution as a Structure-Directing Mechanism,” Angew. Chem., Int Ed., vol. 40, No. 12, pp. 2277-2280, Jun. 2001.*
Higgins et al., “The Framework Topology of Zeolite Beta”,Zeolites, 1988, vol. 8, pp. 446-452.
Higgins et al., “The Framework Topology of Zeolite Beta—A Correction”,Zeolites, 1989, vol. 9, p. 358.
Chevron U.S.A. Inc.
Sample David R
Sheridan Richard J.
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