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US4826663A Expired / Lapsed US ⏱️ 0.0 years remaining

Zirconium phosphate and method for its preparation

Assignee: Eni Tecnologie SpA
•
Filing: 1986-05-13
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Granted: 1989-05-02
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Expires: 2006-05-13
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Abstract

Abstract The invention relates to a zirconium phosphate in particles having sizes comprised within the range of from 1 to 100 μm, a lamellar structure with interlayer distance, in the anhydrous state, comprised within the range of from 7.9 to 8.2 Å and a surface area comprised within the range of from 9 to 20 m 2 /g. The method consists in altering the lamellar structure of a zirconium phosphate with layer structure of alpha type by intercalating into it an organic substance containing a proton-acceptor group and water and by a treatment with ultrasounds, in regenerating the hydrogen form of said zirconium phosphate by an acid and in washing the same with diluted acids and/or water.

Inventors

  • 👤 Giulio Alberti
  • 👤 Francesco Bartoli
  • 👤 Umberto Constantino
  • 👤 Francesco Di Gregorio
  • 👤 Claudio Valentini

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-08 15:13
CPC Classifications
C; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/37; C01B25/372; B; B01; B01J; B01J39/00; B01J39/08; B01J39/09; C07; C07D; C07D453/00; C07D453/02; C07D453/04

Claims Analysis

Total Claims: 26
Claim 1
Independent Claim 48 words
Particulate zirconium acid phosphate of modified lamellar structure having a particle size of from 1 to 100 μm, a lamellar structure with interlayer of distance in the anhydrous state of from 7.9 Å to 8.2 Å and a surface area of from 9 to 20 m 2 /g.
Claim 2
Dependent Claim 48 words
Particulate zirconium acid phosphate of modified lamellar structure having a particle size of from 1 to 100 μm, a lamellar structure with interlayer of distance in the anhydrous state of from 7.9 Å to 8.2 Å and a surface area of from 9 to 20 m 2 /g.
Claim 3
Dependent Claim 30 words
Zirconium phosphate according to claim 1 which upon hydration shows an increase of the interlayer distance, which reaches the value of 10.1 Å under conditions of relative humidity of 92%.
Claim 4
Dependent Claim 94 words
A method for the preparation of the zirconium phosphate according to claim 1 comprising (1) intercalating, into crystalline zirconium phosphate α-Zr(HPO 4 ) 2 .H 2 O having interplanar distance of 7.6 Å, an organic substance containing a proton-acceptor group and water until a stable colloidal aqueous suspension of intercalated zirconium phosphate is prepared, (2) treating the colloidal suspension with ultrasounds, (3) thereafter treating the suspension with non-zirconium-complexing acid until a precipitate of zirconium acid phosphate with modified lamellar structure is formed, (4) recovering the precipitate and washing it with dilute acid and/or water.
Claim 5
Dependent Claim 12 words
A method according to claim 3 wherein the acids are mineral acids.
Claim 6
Dependent Claim 22 words
A method according to claim 4, wherein the mineral acids are selected from HCl, H 2 SO 4 and HNO 3 .
Claim 7
Dependent Claim 25 words
A method according to claim 3, wherein the acid treatment of the colloidal suspension is carried out at a pH of from 0 to 3.
Claim 8
Dependent Claim 11 words
A method according to claim 6, wherein the pH is 1.
Claim 9
Dependent Claim 22 words
A method accoridng to claim 3, wherein the treatment with ultrasounds is continued until the optical density of the suspension remains constant.
Claim 10
Dependent Claim 13 words
A method according to claim 3, wherein the organic substance is an amine.
Claim 11
Dependent Claim 15 words
A method according to claim 9, wherein the amine is selected from methylamine and n-propylamine.
Claim 12
Dependent Claim 45 words
A method according to claim 10, wherein the intercalary amine is n-propylamine and is added in an amount ranging from 25% to 75% of the number of gramatoms of the acidic protons present in the amount of zirconium phosphate α-Zr(HPO 4 ).H 2 O used.
Claim 13
Dependent Claim 32 words
A method according to claim 11, wherein the intercalary n-propylamine is added in an amount equal to 50% of the number of gram-atoms of the acidic protons present in the zirconium phosphate.
Claim 14
Dependent Claim 34 words
A method according to claim 3, wherein the stale colloidal aqueous suspension of intercalated zirconium phosphate is obtained by first intercalating the zirconium phosphate in a non-aqueous medium, and then dispersing it in water.
Claim 15
Dependent Claim 14 words
A method according to claim 13, wherein the zirconium phosphate is intercalated with n-propylamine.
Claim 16
Dependent Claim 13 words
A method according to claim 13, wherein the non-aqueous medium is an alcohol.
Claim 17
Dependent Claim 11 words
A method according to claim 15, wherein the alcohol is methanol.
Claim 18
Dependent Claim 17 words
A method according to claim 3, wherein zirconium phosphate with modified lamellar structure is recovered by filtration.
Claim 19
Dependent Claim 25 words
A method according to claim 3, wherein zirconium phosphate with modified lamellar structure is dried after the recovery and washing with dilute acid and/or water.
Claim 20
Dependent Claim 17 words
A method according to claim 18, wherein the drying is carried out in air at room temperature.
Claim 21
Dependent Claim 15 words
A method according to claim 18, wherein the drying is carried out in an oven.
Claim 22
Dependent Claim 14 words
A method according to claim 18, wherein the drying is carried out by spray-drying.
Claim 23
Dependent Claim 14 words
A method according to claim 18, wherein the drying is carried out by freeze-drying.
Claim 24
Dependent Claim 28 words
A process comprising the step of intercalating proton-acceptor organic substances having molecular weights up to 500 Daltons, wherein the zirconium phosphate according to claim 1 is the intercalan.
Claim 25
Dependent Claim 27 words
A process for recovering Cs + and Ba ++ ions by ion exchange, wherein the zirconium phosphate according to claim 1 or 2 is the ion exchanger.
Claim 26
Dependent Claim 22 words
A process comprising the step of using the zirconium phsophate according to claim 1 or 2 as a catalyst or catalyst support.

References Cited (Backward Citations)

GB983211A Cited
US3416884A Cited
US4025608A Cited
US4381289A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-05-01 1992-10-31 1993-05-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-05-01 1996-10-31 1997-05-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-05-01 2000-10-31 2001-05-02 $7700.00 Window Closed / Lapsed

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