US4665045A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Pillared and delaminated clays containing chromium
Assignee: Michigan State University
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Filing: 1985-04-16
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Granted: 1987-05-12
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Expires: 2005-04-16
Abstract
Abstract A process for preparing a pillared layered lattice clay, comprising the steps of preparing a hydrolyzed solution of chromium ion by reacting a solution of a salt of the said metal with a base at temperatures above 60 DEG C., aging the solution at or above the said temperatures to develop the hydrolyzed pillaring agent, and contacting an aqueous slurry of a smectite, vermiculite, or flurohectorite with the hydrolyzed solution, and recovering the intercalated pillared clay product. The resultant products have unit cells containing from 1.2 to 4.2 chromium ions per cell, and have a repeating spacing of from about 18 to 28 Angstroms. The products are uniquely active catalysts for numerous applications, e.g., in the petrochemical industry.
Inventors
- 👤 Thomas J. Pinnavaia
- 👤 Ming S. Tzou
- 👤 Steven D. Landau
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 18:56
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/049; B01J21/00; B01J21/16; B01J23/00; B01J23/16; B01J23/24; B01J23/26
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
87 words
A process for preparing a pillared layered lattice clay, comprising the steps of: (a) preparing a hydrolyzed solution of chromium ion by reacting a solution of a salt of the said metal with a base at temperatures above 60° C., and aging the solution at or above said temperatures to develop the hydrolyzed pillaring agent; (b) contacting an aqueous slurry of a layer lattice clay selected from the group consisting of smectites, vermiculite, and flurohectorite with said hydrolyzed solution; and (c) recovering the intercalated pillared clay product.
Claim 2
Dependent Claim
87 words
A process for preparing a pillared layered lattice clay, comprising the steps of: (a) preparing a hydrolyzed solution of chromium ion by reacting a solution of a salt of the said metal with a base at temperatures above 60° C., and aging the solution at or above said temperatures to develop the hydrolyzed pillaring agent; (b) contacting an aqueous slurry of a layer lattice clay selected from the group consisting of smectites, vermiculite, and flurohectorite with said hydrolyzed solution; and (c) recovering the intercalated pillared clay product.
Claim 3
Dependent Claim
13 words
A method in accordance with claim 1, wherein said base is sodium carbonate.
Claim 4
Dependent Claim
23 words
A method in accordance with claim 2, wherein said base is in a solution which is added to a solution of said salt.
Claim 5
Dependent Claim
26 words
A method in accordance with claim 1, wherein said reaction temperatures and said aging temperatures are in the range of from about 90° to 100° C.
Claim 6
Dependent Claim
29 words
A method in accordance with claim 1, wherein the ratio of equivalents of base to moles of chromium ion is in the range of from about 1.5 to 2.5.
Claim 7
Dependent Claim
16 words
A method in accordance with claim 4, wherein said temperatures are maintained at about 95° C.
Claim 8
Dependent Claim
18 words
A method in accordance with claim 1, wherein said aging is carried out from 1 to 72 hours.
Claim 9
Dependent Claim
18 words
A method in accordance with claim 4, wherein said aging is carried out from 1 to 3 hours.
Claim 10
Dependent Claim
13 words
A method in accordance with claim 2, wherein said salt is chromium nitrate.
Claim 11
Dependent Claim
16 words
A method in accordance with claim 1, wherein said intercalated pillared product is recovered by centrifuging.
Claim 12
Dependent Claim
17 words
A method in accordance with claim 9, wherein said product recovered by centrifuging is washed and air-dried.
Claim 13
Dependent Claim
40 words
A method in accordance with claim 1, wherein said clay is a trioctahedral smectite having an average particle size of up to about 500 Angstroms and a generally lath-shaped morphology and wherein said recovered product is subjected to freeze drying.
Claim 14
Dependent Claim
31 words
A method in accordance with claim 1, wherein the amount of chromium ion in step (b), is at least one chromium ion per equivalent of a said clay in the slurry.
Claim 15
Dependent Claim
36 words
A method in accordance with claim 13, wherein the amount of chromium ion in step (b), is sufficient to provide a unit cell containing from 1.2 to 4.2 chromium ions per cell, based on chemical analysis.
Claim 16
Dependent Claim
41 words
A pillared clay selected from the group consisting of smectites, flurohectorite and vermiculite, intercalated with chromium polyoxycations to provide a unit cell containing from 1.2 to 4.2 chromium ions per cell, and having a repeating spacing of at least 18 Angstroms.
Claim 17
Dependent Claim
41 words
A pillared clay selected from the group consisting of smectites, flurohectorite and vermiculite, intercalated with chromium polyoxycations to provide a unit cell containing from 1.2 to 4.2 chromium ions per cell, and having a repeating spacing of at least 18 Angstroms.
Claim 18
Dependent Claim
21 words
A product in accordance with claim 14, wherein the repeating spacing is in a range of from 18 to 28 Angstroms.
Claim 19
Dependent Claim
24 words
A pillared clay product in accordance with claim 16, wherein the surface area of said product is at least 140 square meters per gram.
Claim 20
Dependent Claim
36 words
A product in accordance with claim 15, wherein said clay is a trioctahedral smectite having an average particle size of up to about 500 Angstroms and a generally lath-shaped morphology; and which is substantially completely delaminated.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-05-11 | 1990-11-10 | 1991-05-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-05-11 | 1994-11-10 | 1995-05-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-05-11 | 1998-11-10 | 1999-05-12 | $7700.00 | Window Closed / Lapsed |