US4539193A
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Synthesis of crystalline silicate ZSM-12
Assignee: Mobil Oil AS
•
Filing: 1984-05-23
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Granted: 1985-09-03
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Expires: 2004-05-23
Abstract
Abstract This invention relates to a new and improved form of crystalline silicate identified as zeolite ZSM-12, to a new and useful improvement in synthesizing said crystalline silicate and to use of said crystalline silicate prepared in accordance herewith as a catalyst for organic compound, e.g. hydrocarbon compound, conversion.
Inventors
- 👤 Ernest W. Valyocsik
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 01:12
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B39/42; C01B37/00; C01B37/02; Y; Y10; Y10S; Y10S423/00; Y10S423/33
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
176 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: (0.1 to 4)R.sub.2 O:(0.05 to 2)M.sub.2/n O:(0.005 to 2)Al.sub.2 O.sub.3 :(100)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, and R is a cation derived from the monomeric diquaternary bis(dimethylpiperidinium)trimethylene compound having the formula ##STR2## wherein X is an anion, 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 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
60 or greater
H.sub.2 O/SiO.sub.2
5 to 200
OH.sup.- /SiO.sub.2
0.01 to 2.0
M/SiO.sub.2 0.01 to 3.0
R/SiO.sub.2 0.02 to 1.5
______________________________________ wherein M and R are as above defined, and maintaining the mixture at a temperature of from about 80° C. to about 250° C. until crystals of the crystalline silicate are formed.
Claim 2
Independent Claim
176 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: (0.1 to 4)R.sub.2 O:(0.05 to 2)M.sub.2/n O:(0.005 to 2)Al.sub.2 O.sub.3 :(100)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, and R is a cation derived from the monomeric diquaternary bis(dimethylpiperidinium)trimethylene compound having the formula ##STR2## wherein X is an anion, 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 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
60 or greater
H.sub.2 O/SiO.sub.2
5 to 200
OH.sup.- /SiO.sub.2
0.01 to 2.0
M/SiO.sub.2 0.01 to 3.0
R/SiO.sub.2 0.02 to 1.5
______________________________________ wherein M and R are as above defined, and maintaining the mixture at a temperature of from about 80° C. to about 250° C. until crystals of the crystalline silicate are formed.
Claim 3
Dependent Claim
44 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
90 to 15,000
H.sub.2 O/SiO.sub.2 10 to 100
OH.sup.- /SiO.sub.2 0.2 to 1.0
M/SiO.sub.2 0.1 to 1.0
R/SiO.sub.2 0.05 to 0.5
______________________________________
Claim 4
Dependent Claim
21 words
The method of claim 1 wherein said anion is selected from the group consisting of halide, hydroxide, acetate, sulfate and carboxylate.
Claim 5
Dependent Claim
10 words
The method of claim 3 wherein said anion is halide.
Claim 6
Dependent Claim
10 words
The method of claim 4 wherein said halide is iodide.
Claim 7
Dependent Claim
81 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (0.1 to 4)R.sub.2 O:(0.05 to 2)M.sub.2/n O:(0.005 to 2)Al.sub.2 O.sub.3 :(100)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, and R is a cation derived from the monomeric diquaternary bis(dimethylpiperidinium)trimethylene compound having the formula ##STR3## wherein X is an anion, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 8
Dependent Claim
81 words
A synthetic crystalline silicate having a composition in the anhydrous state, expressed in terms of mole ratios of oxides, as follows: (0.1 to 4)R.sub.2 O:(0.05 to 2)M.sub.2/n O:(0.005 to 2)Al.sub.2 O.sub.3 :(100)SiO.sub.2 wherein M is at least one alkali metal cation having the valence n, and R is a cation derived from the monomeric diquaternary bis(dimethylpiperidinium)trimethylene compound having the formula ##STR3## wherein X is an anion, and exhibiting a characteristic X-ray diffraction pattern as shown in Table 1 of the specification.
Claim 9
Dependent Claim
23 words
The synthetic crystalline silicate of claim 6 wherein said anion is selected from the group consisting of halide, hydroxide, acetate, sulfate and carboxylate.
Claim 10
Dependent Claim
12 words
The synthetic crystalline silicate of claim 7 wherein said anion is halide.
Claim 11
Dependent Claim
11 words
The synthetic crystalline silicate of claim 6 wherein M is sodium.
Claim 12
Dependent Claim
66 words
A synthetic crystalline silicate comprising the crystalline silicate of claim 6 wherein said alkali metal cations are replaced, at least in part, by ion exchange with 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.
Claim 13
Dependent Claim
66 words
A synthetic crystalline silicate comprising the crystalline silicate of claim 7 wherein said alkali metal cations are replaced, at least in part, by ion exchange with 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.
Claim 14
Dependent Claim
66 words
A synthetic crystalline silicate comprising the crystalline silicate of claim 8 wherein said alkali metal cations are replaced, at least in part, by ion exchange with a cation or a mixture of cations selected from the group consisting of hydrogen and hydrogen precursors, rare earth metals, and metals form Groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB and VIII of the Periodic Table of Elements.
Claim 15
Dependent Claim
65 words
A synthetic crystalline silicate comprising the crystalline silicate of claim 9 wherein said sodium ions are replaced, at least in part, by ion exchange with 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.
Claim 16
Dependent Claim
17 words
The synthetic crystalline silicate of claim 10 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 17
Dependent Claim
17 words
The synthetic crystalline silicate of claim 11 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 18
Dependent Claim
17 words
The synthetic crystalline silicate of claim 12 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 19
Dependent Claim
17 words
The synthetic crystalline silicate of claim 13 wherein said replacing cation is hydrogen or a hydrogen precursor.
Claim 20
Dependent Claim
19 words
Bis(dimethylpiperidinum) trimethylene-containing ZSM-12 exhibiting an X-ray diffraction pattern having the characteristic lines shown in Table 1 of the specification.
Claim 21
Dependent Claim
19 words
Bis(dimethylpiperidinum) trimethylene-containing ZSM-12 exhibiting an X-ray diffraction pattern having the characteristic lines shown in Table 1 of the specification.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-09-02 | 1989-03-04 | 1989-09-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-09-02 | 1993-03-04 | 1993-09-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-09-02 | 1997-03-04 | 1997-09-03 | $7700.00 | Window Closed / Lapsed |