US5726113A
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Porous clay heterostructures prepared by gallery templated synthesis
Assignee: Michigan State University
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Filing: 1996-03-19
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Granted: 1998-03-10
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Expires: 2016-03-19
Abstract
Abstract A porous clay heterostructure of a 2:1 layered silicate prepared by a gallery templated synthesis method is described. The method uses an inorganic oxide, a neutral amine surfactant and a quaternary onium ion surfactant in the galleries of the 2:1 layered silicate. The structure is then calcined to remove the surfactants which act as a template to produce the porous clay heterostructure. The structure is useful for cracking catalysts, molecular sieves and adsorbents.
Inventors
- 👤 Thomas J. Pinnavaia
- 👤 Anne H. Galarneau
- 👤 Anis F. Barodawalla
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 22:40
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/049; B01J21/00; B01J21/16
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
45 words
A calcinable intermediate to a heterogeneous calcined clay heterostructure which comprises: (a) a porous 2:1 layered silicate clay with galleries between layers of the clay containing a porous polymeric inorganic metal oxide and which is filled with a neutral amine surfactant and quaternary onium ions.
Claim 2
Dependent Claim
45 words
A calcinable intermediate to a heterogeneous calcined clay heterostructure which comprises: (a) a porous 2:1 layered silicate clay with galleries between layers of the clay containing a porous polymeric inorganic metal oxide and which is filled with a neutral amine surfactant and quaternary onium ions.
Claim 3
Dependent Claim
40 words
The intermediate of claim 1 wherein the neutral amine surfactant has the structural formula: R--NH.sub.2, R.sub.2 NH, or R.sub.3 N wherein at least one R group is an organic group with a chain length of 6 to 22 carbon atoms.
Claim 4
Dependent Claim
33 words
The intermediate of claim 1 wherein the neutral amine surfactant has the formula: C.sub.n H.sub.2n+1 NH.sub.2, C.sub.n H.sub.2n+1 NH(CH.sub.3), or C.sub.n H.sub.2n+1 N(CH.sub.3).sub.2 wherein n is an integer between about 6 and 22.
Claim 5
Dependent Claim
23 words
The intermediate of any one of claims 1, 2 or 3 wherein the inorganic oxide is at least in part a silicon oxide.
Claim 6
Dependent Claim
35 words
The intermediate of any one of claims 1, 2 or 3 wherein the 2:1 layered silicate is selected from the group consisting of a smectite clay, a vermiculite, a rectorite, an illite and a mica.
Claim 7
Independent Claim
102 words
A method for the formulation of a calcined, porous 2:1 layered silicate clay heterostructure with galleries between layers of the clay intercalated with a porous inorganic metal oxide having a spacing between the layers of about 2.5 to 7.5 nm and gallery framework confined pores of between about 1.2 and 4.0 nm as determined by the Horvath-Kawazoe N 2 adsorption model which comprises: (a) providing a neutral amine surfactant and a quaternary onium ion in a gallery of said 2:1 layered silicate clay in admixture with a polymeric inorganic metal oxide; and (b) calcining the composition to form the porous clay heterostructure.
Claim 8
Independent Claim
102 words
A method for the formulation of a calcined, porous 2:1 layered silicate clay heterostructure with galleries between layers of the clay intercalated with a porous inorganic metal oxide having a spacing between the layers of about 2.5 to 7.5 nm and gallery framework confined pores of between about 1.2 and 4.0 nm as determined by the Horvath-Kawazoe N 2 adsorption model which comprises: (a) providing a neutral amine surfactant and a quaternary onium ion in a gallery of said 2:1 layered silicate clay in admixture with a polymeric inorganic metal oxide; and (b) calcining the composition to form the porous clay heterostructure.
Claim 9
Dependent Claim
50 words
The method of claim 6 wherein in step (a) the neutral amine is introduced into the galleries of the 2:1 layered silicate clay containing the quaternary onium ion and then a precursor to the polymeric inorganic metal oxide is introduced into the galleries of the clay containing the neutral amine.
Claim 10
Dependent Claim
24 words
The method of claim 7 wherein the neutral amine surfactant is introduced in step (a) at a temperature between about 25° and 100° C.
Claim 11
Dependent Claim
26 words
The method of claim 8 wherein the precursor is introduced in step (a) at a temperature between about 25° and 100° C. in an aqueous solution.
Claim 12
Dependent Claim
29 words
The method of claim 9 wherein the clay containing the polymeric inorganic metal oxide, the quaternary onium ion and the neutral amine surfactant is air dried before step (b).
Claim 13
Independent Claim
28 words
The method of any one of claims 7, 8, 9 or 10 wherein in step (b) the calcining is at a temperature between about 250° and 1000° C.
Claim 14
Independent Claim
36 words
The method of any one of claims 7, 8, 9, or 10 wherein the 2:1 layered silicate is selected from the groups consisting of a smectite clay, a vermiculite, a rectorite, an illite and a mica.
Claim 15
Independent Claim
55 words
A method for the formation of an intermediate to a calcined porous clay heterostructure with galleries between layers of the clay containing a polymeric inorganic metal oxide which comprises: introducing a neutral amine template and a polymerized inorganic metal oxide precursor into a gallery of a 2:1 layered silicate clay containing a quaternary onium ion.
Claim 16
Independent Claim
55 words
A method for the formation of an intermediate to a calcined porous clay heterostructure with galleries between layers of the clay containing a polymeric inorganic metal oxide which comprises: introducing a neutral amine template and a polymerized inorganic metal oxide precursor into a gallery of a 2:1 layered silicate clay containing a quaternary onium ion.
Claim 17
Dependent Claim
44 words
The method of claim 13 wherein the neutral amine template is introduced into the galleries of the 2:1 layered silicate clay containing the quaternary ammonium ion and then the precursor to the polymeric inorganic metal oxide is introduced into the galleries of the clay.
Claim 18
Dependent Claim
21 words
The method of claim 14 wherein the neutral amine surfactant is introduced at a temperature between about 25° and 100° C.
Claim 19
Dependent Claim
19 words
The method of claim 15 wherein the precursor is introduced at a temperature between about 25° and 100° C.
Claim 20
Independent Claim
17 words
The method of any one of claims 13, 14 or 15 wherein the intermediate is air dried.
Claim 21
Independent Claim
41 words
The method of any one of claims 13, 14 or 15 wherein the 2:1 layered silicate is selected from the group consisting of a smectite clay, a vermiculite, a rectorite, an illite and a mica including paragonite, tetrasilica mica and taneolite.
Claim 22
Independent Claim
23 words
The method of any one of claims 6, 7, 13 or 14 where the onium ion is a tertiary or secondary ammonium ion.
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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) | 2001-03-09 | 2001-09-08 | 2002-03-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2005-03-09 | 2005-09-08 | 2006-03-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2009-03-09 | 2009-09-08 | 2010-03-10 | $7700.00 | Window Closed / Lapsed |