US4331641A
Expired / Lapsed
US
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Synthetic crystalline metal silicate compositions and preparation thereof
Assignee: Equistar Chemicals LP
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Filing: 1979-11-07
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Granted: 1982-05-25
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Expires: 1999-11-07
Abstract
Abstract Crystalline metal silicate compositions are prepared from a silica containing mixture which is substantially free of aluminum ions and which contains a chelating agent by digesting a reaction mixture comprising, a tetraalkylammonium compound, sodium hydroxide, a metal compound, an oxide of silicon, a chelating agent and water, with the reaction mixture containing less than about 100 ppm aluminum. Crystalline borosilicate compositions are of special interest. A method for activating the new crystalline compositions to enhance their usefulness for certain conversion processes is also disclosed.
Inventors
- 👤 James A. Hinnenkamp
- 👤 Vernon V. Walatka, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 01:58
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/03; B01J29/035; B01J29/86; C; C01; C01B; C01B35/00; C01B35/08; C01B35/10; C01B35/1009
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
200 words
A method of preparing a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 / n O:W 2 O 3 :5 to 500 SiO 2 :0 to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises preparing a reaction mixture which is substantially free of aluminum ions and which contains tetraalkylammonium compound, sodium hydroxide, an oxide of the desired metal, an oxide of silicon, water and an aluminum chelating agent effective to provide a catalytically active crystalline metal silicate, maintaining the mixture at an elevated temperature until crystals of said metal silicate are formed and separating and recovering said crystals, and in terms of mole ratios falling within the following ranges, the reaction mixture contains: ______________________________________
OH.sup.- /Si O.sub.2
.05-3
R.sub.4 N.sup.+ /(R.sub.4 N.sup.+ + Na.sup.+)
0.1--H.sub.2 O/OH 10-500
SiO.sub.2 /W.sub.2 O.sub.3
5-500
SiO.sub.2 /Chelating agent
1-1000
______________________________________ wherein R is propyl.
Claim 2
Independent Claim
200 words
A method of preparing a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 / n O:W 2 O 3 :5 to 500 SiO 2 :0 to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises preparing a reaction mixture which is substantially free of aluminum ions and which contains tetraalkylammonium compound, sodium hydroxide, an oxide of the desired metal, an oxide of silicon, water and an aluminum chelating agent effective to provide a catalytically active crystalline metal silicate, maintaining the mixture at an elevated temperature until crystals of said metal silicate are formed and separating and recovering said crystals, and in terms of mole ratios falling within the following ranges, the reaction mixture contains: ______________________________________
OH.sup.- /Si O.sub.2
.05-3
R.sub.4 N.sup.+ /(R.sub.4 N.sup.+ + Na.sup.+)
0.1--H.sub.2 O/OH 10-500
SiO.sub.2 /W.sub.2 O.sub.3
5-500
SiO.sub.2 /Chelating agent
1-1000
______________________________________ wherein R is propyl.
Claim 3
Dependent Claim
34 words
A method as in claim 1 wherein the metal is boron and the aluminum content is an amount of less than about 100 wppm based on the weight of silica in the reaction mixture.
Claim 4
Dependent Claim
25 words
A method as in claim 2 wherein the chelating agent is selected from the group consisting of ethylene diamine tetraacetic acid, nitrilioriacetic acid and 8-hydroxyquinoline.
Claim 5
Dependent Claim
15 words
A method as in claim 3 wherein the chelating agent is ethylene diamine tetraacetic acid.
Claim 6
Independent Claim
139 words
A method of activating a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 /nO:W 2 O 3 :5 to 500 SiO 2 :O to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises: (1) Heat treating the dried silicate composition at about 200° to 900° C. (2) Treating the heated silicate with a reducing agent for about 1 to 80 hours at about 200° to 900° C.; and (3) Heat treating the reduced silicate following the procedure of step (1).
Claim 7
Independent Claim
139 words
A method of activating a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 /nO:W 2 O 3 :5 to 500 SiO 2 :O to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises: (1) Heat treating the dried silicate composition at about 200° to 900° C. (2) Treating the heated silicate with a reducing agent for about 1 to 80 hours at about 200° to 900° C.; and (3) Heat treating the reduced silicate following the procedure of step (1).
Claim 8
Dependent Claim
20 words
A method as in claim 5 wherein the silicate heat treated in step (1) is in the hydrogen ion form.
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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) | 1985-05-24 | 1985-11-23 | 1986-05-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-05-24 | 1989-11-23 | 1990-05-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-05-24 | 1993-11-23 | 1994-05-25 | $7700.00 | Window Closed / Lapsed |