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Patent US4717560A successfully refreshed from Google Patents.
US4717560A
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Crystalline zeolite composition (ECR-5) having a cancrinite-like structure and process for its preparation
Assignee: ExxonMobil Technology and Engineering Co
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Filing: 1985-02-04
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Granted: 1988-01-05
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Expires: 2005-02-04
Abstract
Abstract A crystalline zeolite may be prepared which has a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na2O:Al2O3:2.1 to 8.0 SiO2 and having a cancrinite-like structure in which the twelveing channel thereof is not blocked by, for example, salt molecules. The preferred compositions are of the formula: 1.1 to 1.3 Na2O:Al2O3:2.4 to 3.1 SiO2 This zeolite may be prepared from crystallization of an aged reaction mixture containing aqueous ammonia, a source of silica, a source of alumina and sodium hydroxide.
Inventors
- 👤 David E. W. Vaughan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 18:10
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2869; C01B33/2892
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
49 words
A crystalline zeolite, being isostructural to cancrinite, in which the twelve-ring channel has a sorption of greater than about 1% by weight hexane, said crystalline zeolite having a composition, in terms of mole ratios of oxides in the range: 1.0 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.1 to 8.0 SiO.sub.2.
Claim 2
Dependent Claim
49 words
A crystalline zeolite, being isostructural to cancrinite, in which the twelve-ring channel has a sorption of greater than about 1% by weight hexane, said crystalline zeolite having a composition, in terms of mole ratios of oxides in the range: 1.0 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.1 to 8.0 SiO.sub.2.
Claim 3
Dependent Claim
28 words
The zeolite of claim 1 having a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.4 to 6.0 SiO.sub.2.
Claim 4
Dependent Claim
28 words
The zeolite of claim 1 having a composition, in terms of mole ratios of oxides, in the range: 1.1 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.4 to 3.1 SiO.sub.2.
Claim 5
Dependent Claim
176 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.1 to 8.0 SiO.sub.2 and being isostructural to cancrinite, in which the twelve-ring channel thereof has a sorption of greater than about 1% by weight hexane, comprising the steps of: (a) preparing a reaction mixture comprising aqueous ammonia, a source of silica-alumina, and sodium hydroxide, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the ammonia is present in the reaction mixture in an amount of 15 to 30 percent, based on total moles of H 2 O; and (b) maintaining the reaction mixture at a temperature between about 70° and 180° C. and for a time of about 1 to 10 days.
Claim 6
Dependent Claim
176 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na.sub.2 O:Al.sub.2 O.sub.3 :2.1 to 8.0 SiO.sub.2 and being isostructural to cancrinite, in which the twelve-ring channel thereof has a sorption of greater than about 1% by weight hexane, comprising the steps of: (a) preparing a reaction mixture comprising aqueous ammonia, a source of silica-alumina, and sodium hydroxide, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the ammonia is present in the reaction mixture in an amount of 15 to 30 percent, based on total moles of H 2 O; and (b) maintaining the reaction mixture at a temperature between about 70° and 180° C. and for a time of about 1 to 10 days.
Claim 7
Dependent Claim
20 words
The process of claim 4 wherein the source of silica is a natural or synthetic amorphous aluminosilicate gel or glass.
Claim 8
Dependent Claim
26 words
The process of claim 4 wherein the sources of silica and alumina are a preformed silica-alumina gel having a Si/Al ratio of from 2.2 to 5.0.
Claim 9
Dependent Claim
19 words
The process of claim 6 wherein the preformed silica-alumina gel has a Si/Al ratio of from 1 to 20.
Claim 10
Dependent Claim
53 words
The process of claim 6 wherein the preformed silica-alumina gel is prepared from a reaction mixture comprising sodium silicate, aluminum sulfate, sulfuric acid, water and sodium hydroxide, which has been adjusted to a pH of from 5 to 10, and aged at about 15° to 50° C. for at least about 5 minutes.
Claim 11
Dependent Claim
25 words
The process of claim 4 wherein after step (a) but before step (b) the reaction mixture is blended sufficiently to form a substantially homogeneous mixture.
Claim 12
Dependent Claim
19 words
The process of claim 4 wherein microcrystalline ECR-5 seeds are added to the reaction mixture prior to step (b).
Claim 13
Dependent Claim
17 words
The process of claim 4 wherein the aqueous ammonia contains at least about 15% by weight ammonia.
Claim 14
Dependent Claim
198 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na.sub.2 O.sub.3 :Al.sub.2 O.sub.3 :2.2 to 6.0 SiO.sub.2 and being isostructural with cancrinite, in which the twelve-ring channel thereof has a sorption greater than about 1% by weight hexane, which process comprises: (a) preparing a reaction mixture comprising aqueous ammonia, a preformed alumina-silica gel having a Al/Si ratio of 1 to 10, and sodium hydroxide, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2.0 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the aqueous ammonia is present in the reaction mixture in an amount of about 15 to 30 percent, based on total moles of H 2 O; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; and (c) maintaining the reaction mixture at a temperature of 70° to 180° C. for 1 to 10 days until crystals of the zeolite are formed.
Claim 15
Dependent Claim
198 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 1.0 to 1.3 Na.sub.2 O.sub.3 :Al.sub.2 O.sub.3 :2.2 to 6.0 SiO.sub.2 and being isostructural with cancrinite, in which the twelve-ring channel thereof has a sorption greater than about 1% by weight hexane, which process comprises: (a) preparing a reaction mixture comprising aqueous ammonia, a preformed alumina-silica gel having a Al/Si ratio of 1 to 10, and sodium hydroxide, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2.0 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the aqueous ammonia is present in the reaction mixture in an amount of about 15 to 30 percent, based on total moles of H 2 O; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; and (c) maintaining the reaction mixture at a temperature of 70° to 180° C. for 1 to 10 days until crystals of the zeolite are formed.
Claim 16
Dependent Claim
152 words
A process for preparing a crystalline cancrinite zeolite in which the twelve-ring channel thereof has a sorption greater than about 1% by weight hexane, which process comprises the steps of: (a) preparing a reaction mixture comprising aqueous ammonia, a source of silica, metakaolin, sodium hydroxide, said reaction mixture having a composition, in terms of mole ratio of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the ammonia is present in the reaction mixture in an amount of 15 to 30 percent, based on total moles of H 2 O; and (b) maintaining the reaction mixture at a temperature between about 70° and 180° C. for 1 to 10 days until crystals of the zeolite are formed.
Claim 17
Dependent Claim
152 words
A process for preparing a crystalline cancrinite zeolite in which the twelve-ring channel thereof has a sorption greater than about 1% by weight hexane, which process comprises the steps of: (a) preparing a reaction mixture comprising aqueous ammonia, a source of silica, metakaolin, sodium hydroxide, said reaction mixture having a composition, in terms of mole ratio of oxides, within the following ranges: Na 2 O:Al 2 O 3 :2 to 17 SiO 2 :Al 2 O 3 :2 to 25 H 2 O:Al 2 O 3 :30 to 450 (H 2 O+NH 3 ):Al 2 O 3 :50 to 600 wherein the ammonia is present in the reaction mixture in an amount of 15 to 30 percent, based on total moles of H 2 O; and (b) maintaining the reaction mixture at a temperature between about 70° and 180° C. for 1 to 10 days until crystals of the zeolite are formed.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-01-04 | 1991-07-06 | 1992-01-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-01-04 | 1995-07-06 | 1996-01-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-01-04 | 1999-07-06 | 2000-01-05 | $7700.00 | Window Closed / Lapsed |