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US4361501A
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Preparation of vanadium phosphorus catalysts using a mixed phosphorus source
Assignee: Standard Oil Co
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Filing: 1980-12-29
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Granted: 1982-11-30
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Expires: 2000-12-29
Abstract
Abstract The present invention provides a process for the preparation of oxidation catalysts containing mixed oxides of vanadium and phosphorus, which catalysts are particularly effective in the oxidation of n-butane, n-butenes, 1,3-butadiene or a mixture thereof with molecular oxygen or an oxygen-containing gas in the vapor phase to produce high yields of maleic anhydride with good selectivity. A vanadium compound is introduced into a liquid medium, a mixed phosphorus component comprising orthophosphoric acid and pyrophosphoric acid is added to the liquid medium, reduction of at least a portion of the vanadium to a +4 valence state is effected either prior to or subsequent to the addition of the mixed phosphorus component, and the resulting vanadium-phosphorus oxide catalyst precursor is recovered, dried and calcined.
Inventors
- 👤 Patricia R. Blum
- 👤 Ernest C. Milberger
- 👤 Noel J. Bremer
- 👤 Dennis E. Dria
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 10:15
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/16; C07C51/21; C07C51/25; C07C51/252; B; B01; B01J; B01J27/00; B01J27/14; B01J27/16; B01J27/18; B01J23/00; B01J23/002; B01J23/16; B01J23/20; B01J23/22; B01J27/186; B01J27/195; B01J27/198; C07C51/215; C07D; C07D307/00; C07D307/02; C07D307/34; C07D307/56; C07D307/60; B01J2523/00
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
104 words
A process for the preparation of oxidation catalysts containing the mixed oxides of vanadium and phosphorus which comprises (a) introducing a pentavalent vanadium-containing compound into a liquid medium, capable of reducing the valence state of said vanadium; (b) effecting reduction of at least a portion of said vanadium to a valence state of about +4; (c) adding a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid to said medium prior to or subsequent to effecting said reduction to form a catalyst precursor; (d) recovering the catalyst precursor; (e) drying the catalyst precursor; (f) calcining the catalyst precursor.
Claim 2
Dependent Claim
104 words
A process for the preparation of oxidation catalysts containing the mixed oxides of vanadium and phosphorus which comprises (a) introducing a pentavalent vanadium-containing compound into a liquid medium, capable of reducing the valence state of said vanadium; (b) effecting reduction of at least a portion of said vanadium to a valence state of about +4; (c) adding a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid to said medium prior to or subsequent to effecting said reduction to form a catalyst precursor; (d) recovering the catalyst precursor; (e) drying the catalyst precursor; (f) calcining the catalyst precursor.
Claim 3
Dependent Claim
22 words
A process as recited in claim 1 wherein said reduction of vanadium is effected in the presence of the mixed phosphorus component.
Claim 4
Dependent Claim
74 words
A process for the preparation of an oxidation catalyst containing the mixed oxides of vanadium and phosphorus from at least one pentavalent vanadium-containing compound and a mixed phosphorus component, wherein the pentavalent vanadium is reduced to an average valence state of about +3.5 to about +4.6, including the step of contacting the vanadium with said mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid in a liquid medium.
Claim 5
Dependent Claim
74 words
A process for the preparation of an oxidation catalyst containing the mixed oxides of vanadium and phosphorus from at least one pentavalent vanadium-containing compound and a mixed phosphorus component, wherein the pentavalent vanadium is reduced to an average valence state of about +3.5 to about +4.6, including the step of contacting the vanadium with said mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid in a liquid medium.
Claim 6
Dependent Claim
126 words
A process for the preparation of oxidation catalysts containing the mixed oxides of vanadium and phosphorus which comprises (a) introducing a pentavalent vanadium-compound into a liquid medium capable of at least partially solubilizing the vanadium and of reducing the valence state of said vanadium; (b) effecting reduction of at least a portion of said vanadium to a valence state of about +4; (c) removing unsolubilized vanadium-containing compounds having a particle size greater than about 0.1 mm diameter; (d) adding a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid to the reaction medium resulting from step (c) to form a catalyst precursor precipitate; (e) recovering said catalyst precursor precipitate; (f) drying said catalyst precursor precipitate; and (g) calcining said precipitate.
Claim 7
Dependent Claim
126 words
A process for the preparation of oxidation catalysts containing the mixed oxides of vanadium and phosphorus which comprises (a) introducing a pentavalent vanadium-compound into a liquid medium capable of at least partially solubilizing the vanadium and of reducing the valence state of said vanadium; (b) effecting reduction of at least a portion of said vanadium to a valence state of about +4; (c) removing unsolubilized vanadium-containing compounds having a particle size greater than about 0.1 mm diameter; (d) adding a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid to the reaction medium resulting from step (c) to form a catalyst precursor precipitate; (e) recovering said catalyst precursor precipitate; (f) drying said catalyst precursor precipitate; and (g) calcining said precipitate.
Claim 8
Dependent Claim
19 words
A process as recited in claims 1, 3 or 4 wherein said liquid medium comprises an organic liquid medium.
Claim 9
Dependent Claim
15 words
A process as recited in claim 5 wherein said organic liquid medium is essentially anhydrous.
Claim 10
Dependent Claim
14 words
A process as recited in claim 5 wherein said organic liquid medium comprises isobutanol.
Claim 11
Dependent Claim
23 words
A process as recited in claims 1, 3 or 4 wherein reduction of said vanadium is effected by heating the vanadium-containing liquid medium.
Claim 12
Dependent Claim
17 words
A process as recited in claims 1, 3 or 4 wherein said vanadium-containing compound is vanadium pentoxide.
Claim 13
Dependent Claim
23 words
A process as recited in claims 1, 3 or 4 wherein said phosphorus component additionally contains triphosphoric acid up to 10% by weight.
Claim 14
Dependent Claim
60 words
A process as recited in claim 1, 3 or 4 wherein said oxidation catalyst is represented by the empirical formula: V.sub.1 P.sub.a Y.sub.b O.sub.x wherein Y=U, Co, Mo, Fe, Zn, Hf, Zr and mixtures thereof; and a=0.5 to 3.0, b=0 to about 0.5, and x is the number of oxygens required to satisfy the valence requirements of the other elements.
Claim 15
Dependent Claim
28 words
A process as recited in claims 1, 3 or 4 wherein said oxidation catalyst is represented by the empirical formula V 1 P 1 .16 O x .
Claim 16
Dependent Claim
74 words
An oxidation catalyst comprising the mixed oxides of vanadium and phosphorus, wherein the average valence state of said vanadium is in the range of +3.5 to +4.6 and the ratio of phosphorus to vanadium is in the range of about 0.5:1 to 3:1, wherein said catalyst is prepared by contacting a vanadium compound with a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid in a liquid medium.
Claim 17
Dependent Claim
74 words
An oxidation catalyst comprising the mixed oxides of vanadium and phosphorus, wherein the average valence state of said vanadium is in the range of +3.5 to +4.6 and the ratio of phosphorus to vanadium is in the range of about 0.5:1 to 3:1, wherein said catalyst is prepared by contacting a vanadium compound with a mixed phosphorus component comprising 45-90% by weight orthophosphoric acid and 10-50% by weight pyrophosphoric acid in a liquid medium.
Claim 18
Dependent Claim
22 words
An oxidation catalyst as recited in claim 13 wherein said mixed phosphorus component additionally comprises up to 10% triphosphoric acid by weight.
Claim 19
Dependent Claim
17 words
An oxidation catalyst as recited in claim 13 wherein said liquid medium comprises an organic liquid medium.
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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) | 1985-11-29 | 1986-05-31 | 1986-11-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-11-29 | 1990-05-31 | 1990-11-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-11-29 | 1994-05-31 | 1994-11-30 | $7700.00 | Window Closed / Lapsed |