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US4080311A Expired / Lapsed US ⏱️ 0.0 years remaining

Thermally stable phosphate containing alumina precipitates and their method of preparation

Assignee: Chevron USA Inc
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Filing: 1976-08-31
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Granted: 1978-03-21
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Expires: 1996-08-31
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Abstract

Abstract Thermally stable composite precipitates containing aluminum phosphate and alumina and having a surface area of from about 100 to about 200 m2/g together with an average pore radius of from 75 to 150 A are defined. These materials are prepared by neutralizing an aqueous solution of aluminum cations and PO4 anions at a controlled pH of between 7 and 10.0, and wherein the neutralizing medium is either ammonia or certain defined amine based materials such as ammonium hydroxide, ammonium carbonate or urea. There is a stoichiometric excess of aluminum to phosphorus over that required to form AlPO4. Due to their thermal stability these alumina-aluminum phosphates are particularly useful as catalyst supports for various reactions, including polymerization of ethylene.

Inventors

  • 👤 William L. Kehl

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 15:54
CPC Classifications
C; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/36; B; B01; B01J; B01J27/00; B01J27/14; B01J27/16; B01J37/00; B01J37/02; B01J37/03; B01J35/00; B01J35/60; B01J35/61; B01J35/615; B01J35/64; B01J35/647

Claims Analysis

Total Claims: 15
Claim 1
Independent Claim 94 words
A thermally stable composite precipitate containing from 10 to 60 mole percent alumina and from 40 to 90 mole percent aluminum phosphate, said composite precipitate being characterized after calcination at 500° C. for 16 hours as: amorphous; having a surface area from about 100 to about 200 m 2 /g; having an average pore radius of from 75 to 150 A; and wherein no more than a 30% decrease in surface area is obtained if said composite precipitate is further calcined at a temperature up to about 900° C. for up to 16 hours.
Claim 2
Dependent Claim 94 words
A thermally stable composite precipitate containing from 10 to 60 mole percent alumina and from 40 to 90 mole percent aluminum phosphate, said composite precipitate being characterized after calcination at 500° C. for 16 hours as: amorphous; having a surface area from about 100 to about 200 m 2 /g; having an average pore radius of from 75 to 150 A; and wherein no more than a 30% decrease in surface area is obtained if said composite precipitate is further calcined at a temperature up to about 900° C. for up to 16 hours.
Claim 3
Dependent Claim 22 words
A composite in accordance with claim 1 wherein the molar ratio of Al 2 O 3 to AlPO 4 is about 1:2.
Claim 4
Dependent Claim 12 words
A composite precipitate according to claim 1 which is a granular precipitate.
Claim 5
Dependent Claim 21 words
A composite precipitate according to claim 1 which is spray-dried prior to calcination to produce a fluid form of composite precipitate.
Claim 6
Dependent Claim 20 words
A composite precipitate in accordance with claim 1 wherein the average pore radius is from 90 A to 150 A.
Claim 7
Dependent Claim 20 words
A composite precipitate in accordance with claim 1 wherein the average pore radius is from 100 A to 130 A.
Claim 8
Dependent Claim 21 words
A composite according to claim 6 wherein the molar ratio of Al 2 O 3 to AlPO 4 is about 1:2.
Claim 9
Independent Claim 214 words
A method of preparing a thermally stable composite precipitate containing from 10 to 60 mole percent alumina and from 40 to 90 mole percent aluminum phosphate, which comprises: forming a first aqueous solution of aluminum cations and PO 4 --- anions wherein the molar ratio of the PO 4 --- anions to the aluminum cations is 0.82:1 to 0.25:1; neutralizing said first aqueous solution with ammonia gas or a second aqueous solution of an ammonia based material selected from the group consisting of ammonium hydroxide, ammonium carbonate, ammonium bicarbonate or urea in such a manner that the pH of the combined first aqueous solution and the neutralizing medium is controlled in the range of 7 to 10.0; recovering said precipitate; drying said precipitate; and calcining said precipitate at a temperature from 300° C. to 500° C. for a time up to 16 hours to form an amorphous aluminum phosphate composite material having a surface area from about 100 to about 200 m 2 /g, an average pore radius from 75 to 150 A and wherein no more than a 30% decrease in surface area is obtained if said composite precipitate is calcined at 500° C. for 16 hours and further calcined at a temperature up to about 900° C. for up to 16 hours.
Claim 10
Independent Claim 214 words
A method of preparing a thermally stable composite precipitate containing from 10 to 60 mole percent alumina and from 40 to 90 mole percent aluminum phosphate, which comprises: forming a first aqueous solution of aluminum cations and PO 4 --- anions wherein the molar ratio of the PO 4 --- anions to the aluminum cations is 0.82:1 to 0.25:1; neutralizing said first aqueous solution with ammonia gas or a second aqueous solution of an ammonia based material selected from the group consisting of ammonium hydroxide, ammonium carbonate, ammonium bicarbonate or urea in such a manner that the pH of the combined first aqueous solution and the neutralizing medium is controlled in the range of 7 to 10.0; recovering said precipitate; drying said precipitate; and calcining said precipitate at a temperature from 300° C. to 500° C. for a time up to 16 hours to form an amorphous aluminum phosphate composite material having a surface area from about 100 to about 200 m 2 /g, an average pore radius from 75 to 150 A and wherein no more than a 30% decrease in surface area is obtained if said composite precipitate is calcined at 500° C. for 16 hours and further calcined at a temperature up to about 900° C. for up to 16 hours.
Claim 11
Dependent Claim 20 words
A method according to claim 8 wherein H 3 PO 4 is used to supply the PO 4 --- anions.
Claim 12
Dependent Claim 20 words
A method according to claim 9 wherein the basic medium used to neutralize said first aqueous solution is ammonia gas.
Claim 13
Dependent Claim 41 words
A method in accordance with claim 9 wherein the amount of aluminum and the amount of phosphoric acid are correlated to result in a final product having a molar ratio of Al 2 O 3 to AlPO 4 of about 1:2.
Claim 14
Dependent Claim 29 words
A method in accordance with claim 10 wherein the aluminum cations are supplied by using an aluminum salt selected from the group consisting of aluminum nitrate and aluminum chloride.
Claim 15
Dependent Claim 23 words
A method in accordance with claim 8 wherein the precipitate is dried by spray-drying to form a fluid type of aluminum phosphate material.

References Cited (Backward Citations)

US2301913A Cited
US2365623A Cited
US2349827A Cited
US3271299A Cited
US3342750A Cited
US3320331A Cited
US3904550A Cited
US3969273A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-03-20 1981-09-19 1982-03-21 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-03-20 1985-09-19 1986-03-21 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-03-20 1989-09-19 1990-03-21 $7700.00 Window Closed / Lapsed

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