US4552731A
Expired / Lapsed
US
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Process for preparing crystalline zeolite composition ERC-2
Assignee: ExxonMobil Technology and Engineering Co
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Filing: 1983-11-10
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Granted: 1985-11-12
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Expires: 2003-11-10
Abstract
Abstract A synthetic crystalline zeolite is provided characterized by having a composition, in terms of mole ratios of oxides, in the range: 0.9 to 1.1 M2/nO:Al2O3:2.5 to 5.1 SiO2:xH2O wherein M is at least one exchangeable cation, n is the valence of M, and x is 0 to 6, and characterized by having a specified X-ray powder diffraction pattern. The zeolite may be prepared by crystallization from a reaction mixture of KOH (and optionally a minor amount of NaOH), water, a source of silica, and a source of alumina preferably derived from kaolin or halloysite. Most preferably, the source of alumina is metakaolin and the source of silica is potassium silicate.
Inventors
- 👤 David E. Vaughan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 13:09
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/60; B01J29/70; C; C01; C01B; C01B39/00; C01B39/02; C01B39/32
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
192 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.9 to 1.1 M.sub.2 O:Al.sub.2 O.sub.3 :2.5 to 5.1 SiO.sub.2 :0 to 6 H.sub.2 O where M is K or a mixture of K and Na, where Na is no more than 30 mole percent of the mixture, and characterized by having an X-ray powder diffraction pattern essentially identical to that given in Table IV which is characteristic of zeolite L, which comprises: (a) preparing a reaction mixture comprising water, a source of silica, metakaolin, KOH and up to about 30 mole percent of NaOH based on total moles of KOH and NaOH, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________
M'.sub.2 O:Al.sub.2 O.sub.3
1.0 to 1.6
SiO.sub.2 :Al.sub.2 O.sub.3
2.5 to 5.1
H.sub.2 O:Al.sub.2 O.sub.3
80 to 140
______________________________________ where M' is either K or a mixture of K and Na; and (b) maintaining the reaction mixture at between about 140° and 300° C. under autogeneous pressure for a sufficient period of time so as to form crystals of the zeolite.
Claim 2
Dependent Claim
192 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.9 to 1.1 M.sub.2 O:Al.sub.2 O.sub.3 :2.5 to 5.1 SiO.sub.2 :0 to 6 H.sub.2 O where M is K or a mixture of K and Na, where Na is no more than 30 mole percent of the mixture, and characterized by having an X-ray powder diffraction pattern essentially identical to that given in Table IV which is characteristic of zeolite L, which comprises: (a) preparing a reaction mixture comprising water, a source of silica, metakaolin, KOH and up to about 30 mole percent of NaOH based on total moles of KOH and NaOH, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________
M'.sub.2 O:Al.sub.2 O.sub.3
1.0 to 1.6
SiO.sub.2 :Al.sub.2 O.sub.3
2.5 to 5.1
H.sub.2 O:Al.sub.2 O.sub.3
80 to 140
______________________________________ where M' is either K or a mixture of K and Na; and (b) maintaining the reaction mixture at between about 140° and 300° C. under autogeneous pressure for a sufficient period of time so as to form crystals of the zeolite.
Claim 3
Dependent Claim
14 words
The process of claim 1 where NaOH is not employed in the reaction mixture.
Claim 4
Dependent Claim
25 words
The process of claim 1 wherein after step (a) but before step (b) the reaction mixture is blended sufficiently to form a substantially homogeneous mixture.
Claim 5
Dependent Claim
26 words
The process of claim 1 wherein during step (b) the reaction mixture is stirred at a rate less than 60 rpm to maintain substantial homogeneity thereof.
Claim 6
Dependent Claim
39 words
The process of claim 1 wherein the composition of then reaction mixture in step (a) is adjusted to produce a crystalline zeolite product having a composition in the range: 0.9 to 1.1 K.sub.2 O:Al.sub.2 O.sub.3 :2.8 to 4.8 SiO.sub.2.
Claim 7
Dependent Claim
13 words
The process of claim 1 wherein the source of silica is potassium silicate.
Claim 8
Dependent Claim
16 words
The process of claim 1 wherein the reaction mixture is maintained between 160° and 240° C.
Claim 9
Dependent Claim
17 words
The process of claim 7 wherein the reaction mixture is maintained between said temperatures for 2-8 days.
Claim 10
Dependent Claim
36 words
The process of claim 1 wherein prior to step (b) microcrystals of a zeolite are added to the blended reaction mixture in an amount of from 0.1 to 10% by weight based on silica and alumina.
Claim 11
Dependent Claim
34 words
The process of claim 1 wherein prior to step (b) at least a portion of the blended reaction mixture is maintained at about 10° to 100° C. for about 6 hours to 6 days.
Claim 12
Dependent Claim
147 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.9 to 1.1K.sub.2 O:Al.sub.2 O.sub.3 :2.8 to 4.8SiO.sub.2 and having atoms arranged in a hexagonal unit cell such that the X-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table IV, which comprises: (a) preparing a reaction mixture comprising KOH, water, potassium silicate and metakaolin, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________
K.sub.2 O:Al.sub.2 O.sub.3
1.0 to 1.6
SiO.sub.2 :Al.sub.2 O.sub.3
3 to 5
H.sub.2 O:Al.sub.2 O.sub.3
90 to 120
______________________________________ (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; and (c) maintaining the blended reaction mixture at between 160° and 240° C. under autogenous pressure for a sufficient period of time to form crystals of the zeolite.
Claim 13
Dependent Claim
147 words
A process for preparing a crystalline zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.9 to 1.1K.sub.2 O:Al.sub.2 O.sub.3 :2.8 to 4.8SiO.sub.2 and having atoms arranged in a hexagonal unit cell such that the X-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table IV, which comprises: (a) preparing a reaction mixture comprising KOH, water, potassium silicate and metakaolin, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________
K.sub.2 O:Al.sub.2 O.sub.3
1.0 to 1.6
SiO.sub.2 :Al.sub.2 O.sub.3
3 to 5
H.sub.2 O:Al.sub.2 O.sub.3
90 to 120
______________________________________ (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; and (c) maintaining the blended reaction mixture at between 160° and 240° C. under autogenous pressure for a sufficient period of time to form crystals of the zeolite.
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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) | 1988-11-11 | 1989-05-13 | 1989-11-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-11-11 | 1993-05-13 | 1993-11-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-11-11 | 1997-05-13 | 1997-11-12 | $7700.00 | Window Closed / Lapsed |