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US4554145A
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Preparation of crystalline silicate zeolite Beta
Assignee: Mobil Oil AS
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Filing: 1984-04-16
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Granted: 1985-11-19
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Expires: 2004-04-16
Abstract
Abstract This invention relates to a new method for synthesis of zeolite Beta, to the zeolite Beta product of that new method and to use of said zeolite Beta prepared in accordance herewith as a catalyst for organic compound, e.g. hydrocarbon compound, conversion. In the disclosed method for preparing zeolite Beta a dibenzyl-1,4-diazabicyclo [2.2.2] octane compound is added to the synthesis reaction mixture.
Inventors
- 👤 Mae K. Rubin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 06:10
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B39/46; C01B39/48; B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; B01J29/7007; Y; Y10; Y10S; Y10S423/00; Y10S423/27
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
161 words
A method for synthesizing a crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification, which comprises preparing a mixture containing sources of alkali metal oxide, an oxide of aluminum, an organic nitrogen-containing cation, an oxide of silicon and water and having a composition, in terms of mole ratios, within the following ranges: ______________________________________
SiO.sub.2 /Al.sub.2 O.sub.3
5-250
H.sub.2 O/SiO.sub.2
10-100
OH.sup.- /SiO.sub.2
0.09-0.8
R/(R + M) 0.1-0.8
______________________________________ wherein M and R are as above defined, and maintaining the mixture at a temperature of from about 80° C. to about 150° C. until crystals of the crystalline silicate are formed.
Claim 2
Independent Claim
161 words
A method for synthesizing a crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification, which comprises preparing a mixture containing sources of alkali metal oxide, an oxide of aluminum, an organic nitrogen-containing cation, an oxide of silicon and water and having a composition, in terms of mole ratios, within the following ranges: ______________________________________
SiO.sub.2 /Al.sub.2 O.sub.3
5-250
H.sub.2 O/SiO.sub.2
10-100
OH.sup.- /SiO.sub.2
0.09-0.8
R/(R + M) 0.1-0.8
______________________________________ wherein M and R are as above defined, and maintaining the mixture at a temperature of from about 80° C. to about 150° C. until crystals of the crystalline silicate are formed.
Claim 3
Dependent Claim
34 words
The method of claim 1 wherein said mixture has a composition, in terms of mole ratios, as follows: ______________________________________
SiO.sub.2 /Al.sub.2 O.sub.3
10-50
H.sub.2 O/SiO.sub.2
20-80
OH.sup.- /SiO.sub.2
0.2-0.6
R/(R + M) 0.1-0.6
______________________________________
Claim 4
Dependent Claim
20 words
The method of claim 1 wherein said organic nitrogen containing compound is the halide or hydroxide form of dibenzyl- 1,4-diazabicyclo[2.2.2]octane.
Claim 5
Dependent Claim
13 words
The method of claim 3, wherein said dibenzyl-1,4-diazabicyclo[2.2.2]octane is in the halide form.
Claim 6
Dependent Claim
10 words
The method of claim 4 wherein said halide is chloride.
Claim 7
Dependent Claim
72 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 8
Dependent Claim
72 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 9
Dependent Claim
11 words
The synthetic crystalline silicate of claim 6 wherein M is sodium.
Claim 10
Dependent Claim
158 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, wherein M is (a), (b) or mixtures of (a) and (b) and n is the valence of M wherein (a) is at least one alkali metal cation, and wherein (b) is a cation or a mixture of cations selected from the group consisting of hydrogen and hydrogen precursors, rare earth metals, and metals from Groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB and VIII of the Periodic Table of Elements, wherein M is (a) in the as-synthesized synthetic crystalline silicate and wherein M is (b) by ion-exchange of the as-synthesized synthetic crystalline silicate, and which synthetic crystalline silicate exhibits a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 11
Dependent Claim
158 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (1 to 25)R.sub.2 O:(0 to 0.8)M.sub.2/n O:Al.sub.2 O.sub.3 :(x)SiO.sub.2 wherein R is dibenzyl-1,4-diazabicyclo[2.2.2]octane and x is from about 5 to greater than about 200, wherein M is (a), (b) or mixtures of (a) and (b) and n is the valence of M wherein (a) is at least one alkali metal cation, and wherein (b) is a cation or a mixture of cations selected from the group consisting of hydrogen and hydrogen precursors, rare earth metals, and metals from Groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB and VIII of the Periodic Table of Elements, wherein M is (a) in the as-synthesized synthetic crystalline silicate and wherein M is (b) by ion-exchange of the as-synthesized synthetic crystalline silicate, and which synthetic crystalline silicate exhibits a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 12
Dependent Claim
17 words
The synthetic crystalline silicate of claim 8 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 13
Dependent Claim
17 words
The synthetic crystalline silicate of claim 11 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 14
Dependent Claim
11 words
The synthetic crystalline silicate of claim 8, wherein M is sodium.
Claim 15
Dependent Claim
78 words
A reaction mixture for use in synthesis of a crystalline silicate which comprises one or more sources of alkali metal oxide, an oxide of aluminum, an organic nitrogen-containing cation, an oxide of silicon and water whereby the mixture composition, in terms of mole ratios, is within the following ranges: ______________________________________
SiO.sub.2 /Al.sub.2 O.sub.3
5-250
H.sub.2 O/SiO.sub.2
10-100
OH.sup.- /SiO.sub.2
0.09-0.8
R/(R + M) 0.1-0.8
______________________________________ wherein M is at least one alkali metal cation and R comprises dibenzyl-1,4-diazabicyclo[2.2.2]octane.
Claim 16
Dependent Claim
78 words
A reaction mixture for use in synthesis of a crystalline silicate which comprises one or more sources of alkali metal oxide, an oxide of aluminum, an organic nitrogen-containing cation, an oxide of silicon and water whereby the mixture composition, in terms of mole ratios, is within the following ranges: ______________________________________
SiO.sub.2 /Al.sub.2 O.sub.3
5-250
H.sub.2 O/SiO.sub.2
10-100
OH.sup.- /SiO.sub.2
0.09-0.8
R/(R + M) 0.1-0.8
______________________________________ wherein M is at least one alkali metal cation and R comprises dibenzyl-1,4-diazabicyclo[2.2.2]octane.
References Cited (Backward Citations)
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| 3.5 Years (Year 4) | 1988-11-18 | 1989-05-20 | 1989-11-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-11-18 | 1993-05-20 | 1993-11-19 | $3760.00 | Window Closed / Lapsed |
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