US4637991A
Expired / Lapsed
US
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Pillared interlayered clays
Assignee: Phillips Petroleum Co
•
Filing: 1985-06-10
•
Granted: 1987-01-20
•
Expires: 2005-06-10
Abstract
Abstract Pillared, interlayered clay products suitable as gas separation agents or as substrates for catalyst compositions are prepared by methods that provide an increase in surface area and pore volume as compared to similar products made by prior art methods.
Inventors
- 👤 David R. Battiste
- 👤 Jesse R. Harris
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 12:59
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/049
Claims Analysis
Total Claims: 48
Claim 1
Independent Claim
166 words
A method for preparing a pillared, interlayered clay product comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) dispersing said aluminum-exchanged clay product in water; (f) separating aluminum-exchanged clay product from said distilled water; (g) drying said aluminum-exchanged clay product to obtain a substantially dried aluminum-exchanged clay product; and (h) calcining said substantially dried aluminum-exchanged clay product to obtain a calcined aluminum-exchanged clay product which is a pillared, interlayered clay product.
Claim 2
Independent Claim
166 words
A method for preparing a pillared, interlayered clay product comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) dispersing said aluminum-exchanged clay product in water; (f) separating aluminum-exchanged clay product from said distilled water; (g) drying said aluminum-exchanged clay product to obtain a substantially dried aluminum-exchanged clay product; and (h) calcining said substantially dried aluminum-exchanged clay product to obtain a calcined aluminum-exchanged clay product which is a pillared, interlayered clay product.
Claim 3
Dependent Claim
45 words
A method of claim 1 wherein reacting smectite clay with said aqueous solution comprises agitating said clay and said aqueous solution at a temperature in a range of about 20° C. to about 70° C. for a time sufficient to obtain an aluminum-exchanged smectite product.
Claim 4
Dependent Claim
24 words
A method of claim 1 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 5
Dependent Claim
24 words
A method of claim 2 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 6
Independent Claim
181 words
A method for preparing a calcium-exchanged, pillared, interlayered clay product comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) contacting said aluminum-exchanged clay product with a solution of calcium acetate for a time sufficient to produce a calcium-exchanged clay product; (f) separating calcium-exchanged clay product from said distilled water; (g) drying said calcium-exchanged clay product to obtain a substantially dried calcium-exchanged clay product; and (h) calcining said substantially dried calcium-exchanged clay product to obtain a calcined calcium-exchanged clay product which is a pillared, interlayered clay product.
Claim 7
Independent Claim
181 words
A method for preparing a calcium-exchanged, pillared, interlayered clay product comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) contacting said aluminum-exchanged clay product with a solution of calcium acetate for a time sufficient to produce a calcium-exchanged clay product; (f) separating calcium-exchanged clay product from said distilled water; (g) drying said calcium-exchanged clay product to obtain a substantially dried calcium-exchanged clay product; and (h) calcining said substantially dried calcium-exchanged clay product to obtain a calcined calcium-exchanged clay product which is a pillared, interlayered clay product.
Claim 8
Dependent Claim
45 words
A method of claim 5 wherein reacting smectite clay with said aqueous solution comprises agitating said clay and said aqueous solution at a temperature in a range of about 20° C. to about 70° C. for a time sufficient to obtain an aluminum-exchanged smectite product.
Claim 9
Dependent Claim
24 words
A method of claim 5 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 10
Dependent Claim
24 words
A method of claim 5 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 11
Independent Claim
248 words
A method for preparing a pillared, interlayered clay admixed with zeolite comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) contacting said aluminum-exchanged clay product with sufficient distilled water to provide a washed aluminum-exchanged clay product; (f) recovering washed aluminum-exchanged clay product; (g) agitating washed aluminum-exchanged clay product with aqueous solution containing aluminum hydroxy chloride and zeolite to produce a slurry of a mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite in aqueous liquid; (h) separating said mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite from said aqueous liquid; (i) drying said mixture to obtain a substantially dry mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite; and (j) calcining said mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite to obtain a calcined mixture of said aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite which is a pillared, interlayered clay product.
Claim 12
Independent Claim
248 words
A method for preparing a pillared, interlayered clay admixed with zeolite comprising: (a) diluting an aluminum hydroxy chloride compound with water to obtain an aqueous solution containing from about 0.4 to about 10 weight percent of aluminum hydroxy chloride; (b) maintaining said aqueous solution at a temperature in the range from about 20° C. to about 70° C. for a time sufficient to increase the surface area and pore volume of a pillared, interlayered clay product subsequently obtained by reacting smectite clay with said aqueous solution; (c) reacting smectite clay with said aqueous solution thereby obtaining an aluminum-exchanged clay product in an aqueous liquid; (d) separating said aluminum-exchanged clay product from said aqueous liquid; (e) contacting said aluminum-exchanged clay product with sufficient distilled water to provide a washed aluminum-exchanged clay product; (f) recovering washed aluminum-exchanged clay product; (g) agitating washed aluminum-exchanged clay product with aqueous solution containing aluminum hydroxy chloride and zeolite to produce a slurry of a mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite in aqueous liquid; (h) separating said mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite from said aqueous liquid; (i) drying said mixture to obtain a substantially dry mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite; and (j) calcining said mixture of aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite to obtain a calcined mixture of said aluminum-exchanged clay product and aluminum hydroxy chloride treated zeolite which is a pillared, interlayered clay product.
Claim 13
Dependent Claim
45 words
A method of claim 9 wherein reacting smectite clay with said aqueous solution comprises agitating said clay and said aqueous solution at a temperature in a range of about 20° C. to about 70° C. for a time sufficient to obtain an aluminum-exchanged smectite product.
Claim 14
Dependent Claim
24 words
A method of claim 9 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 15
Dependent Claim
24 words
A method of claim 9 wherein obtaining aluminum-exchanged clay product separated from said aqueous liquid comprises obtaining a filter cake of aluminum-exchanged clay product.
Claim 16
Dependent Claim
72 words
A method for preparing a promoted pillared clay catalyst comprising: (a) contacting a pillared, interlayered clay product prepared by the method of claim 1 with an impregnating solution of catalytically active compound or mixture of compounds for a time sufficient to impregnate said pillared, interlayered clay product with a catalytic amount of said catalytically active compound or mixture of compounds and (b) recovering impregnated pillared, interlayered clay product from said impregnating solution.
Claim 17
Dependent Claim
51 words
A method of claim 13 further comprising: (c) drying said impregnated pillared, interlayered clay product at an elevated temperature for a time sufficient to produce a substantially dried impregnated pillared, interlayered clay product; and (d) calcining said dried impregnated pillared, interlayered clay product provide a calcined impregnated pillared, interlayered clay product.
Claim 18
Dependent Claim
25 words
A method of claim 14 wherein steps (a), (b), (c) and (d) are repeated at least once to increase the degree of impregnation of catalyst.
Claim 19
Dependent Claim
18 words
A method of claim 15 wherein said mixture of impregnating compounds comprises MoO 3 and nickel (II) carbonate.
Claim 20
Dependent Claim
75 words
A method of claim 5 for preparing a promoted pillared clay catalyst comprising: (a) contacting a pillared, interlayered clay product prepared by the method of claim 1 with an impregnating solution of catalytically active compound or mixture of compounds for a time sufficient to impregnate said pillared, interlayered clay product with a catalytic amount of said catalytically active compound or mixture of compounds and (b) recovering impregnated pillared, interlayered clay product from said impregnating solution.
Claim 21
Dependent Claim
51 words
A method for claim 17 further comprising: (c) drying said impregnated pillared, interlayered clay product at an elevated temperature for a time sufficient to produce a substantially dried impregnated pillared, interlayered clay product; and (d) calcining said dried impregnated pillared, interlayered clay product provide a calcined impregnated pillared, interlayered clay product.
Claim 22
Dependent Claim
25 words
A method of claim 17 wherein steps (a), (b), (c), and (d) are repeated at least once to increase the degree of impregnation of catalyst.
Claim 23
Dependent Claim
75 words
A method of claim 9 for preparing a promoted pillared clay catalyst comprising: (a) contacting a pillared, interlayered clay product prepared by the method of claim 1 with an impregnating solution of catalytically active compound or mixture of compounds for a time sufficient to impregnate said pillared, interlayered clay product with a catalytic amount of said catalytically active compound or mixture of compounds and, (b) recovering impregnated pillared, interlayered clay product from said impregnating solution.
Claim 24
Dependent Claim
51 words
A method of claim 20 further comprising: (c) drying said impregnated pillared, interlayered clay product at an elevated temperature for a time sufficient to produce a substantially dried impregnated pillared, interlayered clay product; and (d) calcining said dried impregnating pillared, interlayered clay product provide a calcined impregnated pillared, interlayered clay product.
Claim 25
Dependent Claim
25 words
A method of claim 20 wherein steps (a), (b), (c), and (d) are repeated at least once to increase the degree of impregnation of catalyst.
Claim 26
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 1.
Claim 27
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 2.
Claim 28
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 3.
Claim 29
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 4.
Claim 30
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 5.
Claim 31
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 6.
Claim 32
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 7.
Claim 33
Dependent Claim
12 words
A pillared, interlayered clay product prepared by the method of claim 8.
Claim 34
Dependent Claim
14 words
A pillared, interlayered clay admixed with zeolite prepared by the method of claim 9.
Claim 35
Dependent Claim
14 words
A pillared, interlayered clay admixed with zeolite prepared by the method of claim 10.
Claim 36
Dependent Claim
14 words
A pillared, interlayered clay admixed with zeolite prepared by the method of claim 11.
Claim 37
Dependent Claim
14 words
A pillared, interlayered clay admixed with zeolite prepared by the method of claim 12.
Claim 38
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 13.
Claim 39
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 14.
Claim 40
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 15.
Claim 41
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 16.
Claim 42
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 17.
Claim 43
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 18.
Claim 44
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 19.
Claim 45
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 20.
Claim 46
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 21.
Claim 47
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 22.
Claim 48
Dependent Claim
12 words
A promoted pillared clay catalyst prepared by the method of claim 23.
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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) | 1990-01-19 | 1990-07-21 | 1991-01-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-01-19 | 1994-07-21 | 1995-01-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-01-19 | 1998-07-21 | 1999-01-20 | $7700.00 | Window Closed / Lapsed |