Patent US3691099A successfully refreshed from Google Patents.
US3691099A
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Treatment of aluminosilicate
Assignee: Individual
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Filing: 1970-02-27
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Granted: 1972-09-12
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Expires: 1990-02-27
Abstract
Abstract The properties of aluminum-containing refractory oxides in which at least some of the aluminum atoms are tetra-coordinated are improved and/or retained upon contacting with aqueous acidic media in the presence of slats having cations capable of satisfying the negative charge on the tetra-coordinated aluminum atoms. Further advantage with regard to zeolites is realized when the salt anion is capable of combining, e.g., reacting, complexing etc., with aluminum.
Inventors
- 👤 Dean Arthur Young
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 15:13
CPC Classifications
C; C10; C10G; C10G49/00; C10G49/02; C10G49/08; B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/08; B01J29/084; B01J2229/00; B01J2229/10; B01J2229/16; B01J2229/30; B01J2229/37; B01J2229/40; B01J2229/42; Y; Y10; Y10S; Y10S423/00; Y10S423/21
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
98 words
The composition prepared by treating an ion exchangeable zeolitic aluminosilicate having a silica-to-alumina ratio of at least about 2 and structural aluminum atoms associated with exchangeable cations with an aqueous acidic medium at a pH between about 2 and about 6 containing an ionizable water soluble salt of a cation exchangeable with said cations associated with said structural aluminum atoms at a temperature and for a period of time correlated with the acid stability of said zeolitic aluminosilicate sufficient to react said acid with said structural aluminum atoms yet insufficient to completely destroy the crystallinity of said aluminosilicate.
Claim 2
Dependent Claim
70 words
The method of claim 1 wherein said aqueous acidic medium contains at least one acid selected from the strong mineral acids, formic, acetic, citric, oxalic, malonic, succinic, tartaric and salicylic acids; nitriloacetic acids, and hydroxybenzene-sulfonic acids; the concentration of said salt in said aqueous medium corresponds to at least about 0.8 M, and said zeolitic aluminosilicate is contacted with said solution for a period of at least about 0.5 hours.
Claim 3
Dependent Claim
92 words
The method of claim 3 wherein the concentration of said salt in said aqueous medium corresponds to about 0.3 to about 6 M, said zeolitic aluminosilicate is contacted with said aqueous acidic medium at a temperature of about 30 to about 220* F. for a period of about 0.5 to about 30 hours, and the cation of said salt is selected from ammonium, primary, secondary and tertiary amines having up to about eight carbon atoms per molecule; and the metal cations of periodic Groups IA, IB, IIB, IIA, IIIB, VIIB and VIII.
Claim 4
Dependent Claim
70 words
The composition of claim 2 wherein said aqueous acidic medium contains at least one acid selected from the strong mineral acids, formic, acetic, citric, oxalic, malonic, succinic, tartaric and salicylic acids; nitriloacetic acids, and hydroxybenzene-sulfonic acids; the concentration of said salt in said aqueous medium corresponds to at least about 0.3 M, and said zeolitic aluminosilicate is contacted with said solution for a period of at least about 0.5 hours.
Claim 5
Dependent Claim
92 words
The composition of claim 2 wherein the concentration of said salt in said aqueous medium corresponds to about 0.3 to about 6 M, said zeolitic aluminosilicate is contacted with said aqueous acidic medium at a temperature of about 30 to about 220* F. for a period of about 0.5 to about 30 hours, and the cation of said salt is selected from ammonium; primary, secondary and tertiary amines having up to about eight carbon atoMs per molecule; and the metal cations of periodic Groups IA, IB, IIB, IIA, IIIB, VIIB and VIII.
Claim 6
Dependent Claim
30 words
A catalytic composition comprising a refractory inorganic oxide and a catalytically active amount of the composition of claim 2 characterized by high hydrothermal structural stability and hydrothermally stable acid sites.
Claim 7
Dependent Claim
35 words
The method of claim 1 wherein said medium further comprises at least one salt having an anion selected from chloride, nitrate, phosphate, sulfate, acetate, citrate, oxalate, tartrate, formate, malonate, nitriloacetate, salicylate, hydroxybenzenesulfonate and succinate anions.
Claim 8
Dependent Claim
40 words
The method of claim 1 wherein said cation is selected from ammonium, primary, secondary and tertiary amines having up to eight carbon atoms per molecule and metal cations of Groups IA, IB, IIA, IIB and VIII of the Periodic Table.
Claim 9
Dependent Claim
77 words
The method of claim 8 wherein said aluminosilicate is selected from fantastic-type zeolites having the predominance of structural aluminum atoms associated with one of sodium and ammonium cations, the cation of said salt is selected from ammonium, primary, secondary and tertiary amines having up to eight carbon atoms, and metal cations of Groups IA, IB, IIA, IIB and VIII of the Periodic Chart, and the concentration of said salt is from about 0.3 to about 6 molar.
Claim 10
Dependent Claim
43 words
The method of claim 1 wherein said aluminosilicate is further treated in the presence of additional acid and a pH of from about 1 to about 4 and less than said first pH for an additional period of at least about 30 minutes.
Claim 11
Independent Claim
111 words
The method which comprises contacting one of natural and synthetic crystalline zeolitic aluminosilicates having silica to alumina ratios of at least about 2 in an aqueous acidic medium at a pH of from about 2 to about 5, a temperature of from about 30* to about 220* F. for a period of from about 0.5 to about 30 hours, said pH, temperature and contact time being correlated with the acid stability of said aluminosilicate to abstract aluminum therefrom while substantially retaining the crystalline character of said aluminosilicate, wherein said aqueous acidic medium comprises at least about 5 weight-percent of a salt having a cation exchangeable with the cations of said aluminosilicate.
Claim 12
Dependent Claim
89 words
The method of claim 12 wherein the structural aluminum atoms of said aluminosilicate are associated with cations selected from hydrogen, ammonium, primary, secondary and tertiary amines having up to 8 carbon atoms, and the metal cations of Groups IA, IB, IIA, IIB, IIIB, VIIB and VIII of the Periodic Table, and the cation of said salt is selected from ammonium, primary, secondary and tertiary amines having up to eight carbon atoms, and the metal cations of Groups IA, IB, IIB, IIA, IIIB, VIIB and VIII of the Periodic Chart.
Claim 13
Dependent Claim
30 words
The method of claim 13 wherein the anion of said salt is selected from chloride, nitrate, sulfate, phosphate, acetate, citrate, oxalate, tartrate, formate, malonate, nitriloacetate, salicylate, hydrobenzene sulfonate, and succinate.
Claim 14
Dependent Claim
38 words
The method of claim 13 wherein said aluminosilicate is further contacted at a second pH within the range of from about 1 to about 4 lower than said first pH to further abstract additional aluminum from said aluminosilicate.
Claim 15
Independent Claim
100 words
The method of treating an ion exchangeable aluminosilicate selected from natural and synthetic, crystalline and amorphous aluminosilicates containing tetra-coordinated aluminum atoms by contacting said aluminosilicate with an aqueous acidic medium at a pH within the range of about 2 to about 5 containing an excess of salt cations exchangeable with the cations associated with said tetra-coordinated aluminum atoms at a temperature of about 30* to about 200* F. for a contact time of at least about 0.5 hours, said temperature in contact time being correlated so as to pRevent the complete destruction of the tetra-coordinated combination of said aluminum atoms.
Claim 16
Dependent Claim
61 words
The method of claim 16 wherein said aqueous acidic medium is at least about 50 percent saturated with a water soluble salt having cations exchangeable with the cations of said aluminosilicate and said aluminosilicate is contacted with said acidic aqueous medium at a temperature of about 30* to about 200* F. for a period of about 0.5 to about 30 hours.
Claim 17
Dependent Claim
106 words
The method of claim 16 wherein said aluminosilicate is contacted with said aqueous solution for a period of about 0.5 to about 30 hours, said aqueous solution is at least about 50 percent saturated with a water soluble salt having a cation selected from ammonium, primary, secondary and tertiary amines having up to about eight carbon atoms per molecule and the metal cations of Groups IA, IB, IIB, IIA, IIIB, VIIB and VIII of the Periodic Chart, said acidic aqueous medium contains at least one acid selected from strong mineral acids, formic, acetic, citric, oxalic, malonic, succinic, tartaric and salicylic acids, nitriloacetic acids and hydroxybenzene-sulfonic acids.
Claim 18
Dependent Claim
85 words
The method of claim 16 wherein said tetra-coordinated aluminum atoms of said aluminosilicate are associated with at least one cation selected from hydrogen, ammonium, primary, secondary and tertiary amines having up to about eight carbon atoms per molecule and the metal cations of Groups IA, IB, IIA, IIB, IIIB, VIIB and VIII of the Periodic Table and said aqueous acidic medium is at least 50 percent saturated with a water soluble salt having a cation selected from ammonium and the alkali and alkaline earth metals.
Claim 19
Dependent Claim
19 words
As a composition of matter an aluminosilicate having hydrothermally stable acid sites produced by the method of claim 16.
Claim 20
Dependent Claim
14 words
The aluminosilicate having highly stable acid sites produced by the method of claim 12.
Claim 21
Dependent Claim
23 words
A crystalline aluminosilicate characterized by high hydrothermal structural stability and having highly hydrothermally stable acid sites produced by the method of claim 16.
Claim 22
Dependent Claim
19 words
A highly hydrothermally stable crystalline aluminosilicate characterized by hydrothermally stable acid sites produced by the method of claim 18.
Claim 23
Dependent Claim
27 words
As a hydrocarbon conversion catalyst the composition of claim 20 containing at least one hydrogenation component selected from the Group VI and VIII metals, oxides and sulfides.
Claim 24
Dependent Claim
27 words
As a hydrocarbon conversion catalyst the composition of claim 22 containing at least one hydrogenation component selected from the Group VI and VIII metals, oxides and sulfides.
References Cited (Backward Citations)
US2253285A
Cited
US2971904A
Cited
US3201197A
Cited
US3213038A
Cited
US3375064A
Cited
US3406124A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1975-09-12 | 1976-03-13 | 1976-09-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-09-12 | 1980-03-13 | 1980-09-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-09-12 | 1984-03-13 | 1984-09-12 | $7700.00 | Window Closed / Lapsed |