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US4713227A
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Method for the synthesis of metallophosphoaluminates
Assignee: Mobil Oil AS
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Filing: 1986-06-25
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Granted: 1987-12-15
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Expires: 2006-06-25
Abstract
Abstract Crystalline metallophosphoaluminates are prepared by hydrothermal crystallization utilizing a reaction mixture containing a substantially water-immiscible organic solvent wherein one of the aluminum, phosphorus or oxide sources is soluble in the organic solvent.
Inventors
- 👤 Eric G. Derouane
- 👤 Roland V. Ballmoos
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 17:34
CPC Classifications
B; B01; B01J; B01J39/00; B01J39/08; B01J39/12; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; B01J23/00; B01J23/02; B01J23/04; B01J29/00; B01J29/82; B01J29/84; B01J29/85; C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B37/00; C01B37/06; C01B37/08; Y; Y10; Y10S; Y10S423/00; Y10S423/30
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
275 words
A method for synthesis of crystalline metallophosphoaluminate characterized by a composition, in the anhydrous state, as follows: A.sub.v :Q.sub.i :(AlO.sub.2.sup.-).sub.1-x :(PO.sub.2.sup.+).sub.1-y :(MO.sub.2.sup.m-4).sub.x+y :T.sub.j wherein A is occluded organic solvent and directing agent, v is the number of moles A, Q is an alkali metal cation, T is a monovalent anion, and M is one or more elements other than aluminum or phosphorus of valence m, and x, y, i and j are numbers which satisfy the relationship: i-j=y-x+(4-m)·(x+y), said metallophosphoaluminate having an ion exchange capacity of at least about 0.002 meq/g, which comprises: providing a reaction mixture comprising components in the following relationship: (D).sub.a :(Q.sub.2 O).sub.b :(Al.sub.2 O.sub.3).sub.c :(P.sub.2 O.sub.5).sub.d :(MO.sub.m/2).sub.e :(So).sub.f :(T).sub.g :(H.sub.2 O).sub.h wherein D is an organic directing agent, So is a substantially water-immiscible organic solvent and a, b, c, d, e, f, g, and h are numbers satisfying the following relationships: a/(c+d+e) is greater than 0 but less than 4, b/(c+d+e) is less than 2, e/(c+d) is greater than 0 but less than 2, f/(c+d+e) is from 0.1 to 15, g/(c+d+e) is less than 2, and h/(c+d+e) is from 3 to 150, wherein upon initial provision of said reaction mixture the source of one of the M, Al or P oxides is dispersed or dissolved in the substantially water-immiscible organic solvent; heating said reaction mixture at a rate of from about 5° C. to about 200° C. per hour to a temperature of from about 80° C. to about 300° C.; maintaining said reaction mixture at a temperature of from about 80° C. to about 300° C. and a pH of from about 2 to about 9; and recovering said metallophosphoaluminate.
Claim 2
Independent Claim
275 words
A method for synthesis of crystalline metallophosphoaluminate characterized by a composition, in the anhydrous state, as follows: A.sub.v :Q.sub.i :(AlO.sub.2.sup.-).sub.1-x :(PO.sub.2.sup.+).sub.1-y :(MO.sub.2.sup.m-4).sub.x+y :T.sub.j wherein A is occluded organic solvent and directing agent, v is the number of moles A, Q is an alkali metal cation, T is a monovalent anion, and M is one or more elements other than aluminum or phosphorus of valence m, and x, y, i and j are numbers which satisfy the relationship: i-j=y-x+(4-m)·(x+y), said metallophosphoaluminate having an ion exchange capacity of at least about 0.002 meq/g, which comprises: providing a reaction mixture comprising components in the following relationship: (D).sub.a :(Q.sub.2 O).sub.b :(Al.sub.2 O.sub.3).sub.c :(P.sub.2 O.sub.5).sub.d :(MO.sub.m/2).sub.e :(So).sub.f :(T).sub.g :(H.sub.2 O).sub.h wherein D is an organic directing agent, So is a substantially water-immiscible organic solvent and a, b, c, d, e, f, g, and h are numbers satisfying the following relationships: a/(c+d+e) is greater than 0 but less than 4, b/(c+d+e) is less than 2, e/(c+d) is greater than 0 but less than 2, f/(c+d+e) is from 0.1 to 15, g/(c+d+e) is less than 2, and h/(c+d+e) is from 3 to 150, wherein upon initial provision of said reaction mixture the source of one of the M, Al or P oxides is dispersed or dissolved in the substantially water-immiscible organic solvent; heating said reaction mixture at a rate of from about 5° C. to about 200° C. per hour to a temperature of from about 80° C. to about 300° C.; maintaining said reaction mixture at a temperature of from about 80° C. to about 300° C. and a pH of from about 2 to about 9; and recovering said metallophosphoaluminate.
Claim 3
Dependent Claim
17 words
The method of claim 1, wherein the components of the reaction mixture are admixed with each other.
Claim 4
Dependent Claim
27 words
The method of claim 1, wherein M is characterized by an oxidation number of +2 to +6 and an ionic Radius Ratio of from 0.15 to 0.73.
Claim 5
Dependent Claim
19 words
The method of claim 1, wherein the pH of the reaction mixture is from about 6 to about 9.
Claim 6
Dependent Claim
11 words
The method of claim 4, wherein the pH is about 8.
Claim 7
Dependent Claim
61 words
The method of claim 1, which comprises the additional step of heating the recovered metallophosphoaluminate at a temperature of from about 200° to about 1000° C.; and wherein the heated metallophosphoaluminate is characterized by a composition, in the anhydrous state, as follows: Q.sub.i :(AlO.sub.2.sup.-).sub.1-x :(PO.sub.2.sup.+).sub.1-y :(MO.sub.2.sup.m-4).sub.x+y :T.sub.j said heated metallophosphoaluminate having an ion exchange capacity of at least about 0.002 meq/g.
Claim 8
Dependent Claim
26 words
The method of claim 1, which comprises the additional step of replacing original alkali metal cations or monovalent anions of said recovered metallophosphoaluminate with other ions.
Claim 9
Dependent Claim
33 words
The method of claim 7, which comprises the additional step of heating said metallophosphoaluminate, having original ions replaced with other ions, at a temperature of from about 200° C. to about 1000° C.
Claim 10
Dependent Claim
46 words
The method of claim 7, wherein alkali metal cations are replaced and said other ions are cations selected from the group consisting of hydrogen, hydrogen precursor, rare earth metal and metal of Groups IIA, IIIA, IVA, IB, IIB, IIIB, VIB and VIII of the Periodic Table.
Claim 11
Dependent Claim
15 words
The method of claim 1, wherein the recovered metallophosphoaluminate is combined with a binder material.
Claim 12
Dependent Claim
16 words
The method of claim 5, wherein the heated recovered metallophosphoaluminate is combined with a binder material.
Claim 13
Dependent Claim
150 words
A reaction mixture for use in synthesis of a crystalline metallophosphoaluminate comprising components in the relationship: (D).sub.a :(Q.sub.2 O).sub.b :(Al.sub.2 O.sub.3).sub.c :(P.sub.2 O.sub.5).sub.d :(MO.sub.m/2).sub.e :(So).sub.f :(T).sub.g :(H.sub.2 O).sub.h a, b, c, d, e, f, g and h are numbers satisfying the following relationships: a/(c+d+e) is greater than 0 but less than 4, b/(c+d+e) is less than 2, e/(c+d) is greater than 0 but less than 2, f/(c+d+e) is from 0.1 to 15, g/(c+d+e) is less than 2, and h/(c+d+e) is from 3 to 150, wherein D is an organic directing agent, Q is an alkali metal cation, M is one or more elements other than aluminum or phosphorus of valence m and So is a substantially water-immiscible organic solvent and T is a monovalent inorganic anion and wherein the source of one of the M, Al or P oxides is initially dispersed or dissolved in the substantially water-immiscible organic solvent.
Claim 14
Dependent Claim
150 words
A reaction mixture for use in synthesis of a crystalline metallophosphoaluminate comprising components in the relationship: (D).sub.a :(Q.sub.2 O).sub.b :(Al.sub.2 O.sub.3).sub.c :(P.sub.2 O.sub.5).sub.d :(MO.sub.m/2).sub.e :(So).sub.f :(T).sub.g :(H.sub.2 O).sub.h a, b, c, d, e, f, g and h are numbers satisfying the following relationships: a/(c+d+e) is greater than 0 but less than 4, b/(c+d+e) is less than 2, e/(c+d) is greater than 0 but less than 2, f/(c+d+e) is from 0.1 to 15, g/(c+d+e) is less than 2, and h/(c+d+e) is from 3 to 150, wherein D is an organic directing agent, Q is an alkali metal cation, M is one or more elements other than aluminum or phosphorus of valence m and So is a substantially water-immiscible organic solvent and T is a monovalent inorganic anion and wherein the source of one of the M, Al or P oxides is initially dispersed or dissolved in the substantially water-immiscible organic solvent.
Claim 15
Dependent Claim
29 words
The reaction mixture of claim 12, wherein M is characterized by an oxidation number of from +2 to +6 and an ionic Radius Ratio of from 0.15 to 0.73.
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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) | 1990-12-14 | 1991-06-15 | 1991-12-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-12-14 | 1995-06-15 | 1995-12-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-12-14 | 1999-06-15 | 1999-12-15 | $7700.00 | Window Closed / Lapsed |