Patent US4272401A successfully refreshed from Google Patents.
US4272401A
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Regeneration of spent hydrodesulfurization catalyst with heteropoly acids
Assignee: ExxonMobil Technology and Engineering Co
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Filing: 1979-07-19
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Granted: 1981-06-09
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Expires: 1999-07-19
Abstract
Abstract Contacting deactivated hydrodesulfurization catalyst, such as Co-Mo supported on alumina, with a heteropoly acid, such as molybdophosphoric acid or tungstosilicic acid, in pH range of about 1 to 3 and temperature range of about 20 DEG to 80 DEG C., results, before any coke is burned off the catalyst, in selective abstraction of vanadium and nickel, removal of sulfur, increase in surface area, and increase in pore volume of the catalyst. Subsequent cobalt doping of demetallized catalyst followed by calcination promotes decoking, additional sulfur removal and additional increase in surface area and pore volume. The process results in substantially complete regeneration of catalytic activity.
Inventors
- 👤 Raam R. Mohan
- 👤 Gopal H. Singhal
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 13:55
CPC Classifications
B; B01; B01J; B01J23/00; B01J23/90; B01J23/94; C; C10; C10G; C10G45/00; C10G45/02; C10G45/04; C10G45/06; C10G45/08; Y; Y10; Y10S; Y10S502/00; Y10S502/515; Y10S502/516
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
45 words
An improved process for regenerating spent hydrofining catalysts which comprises contacting spent catalyst with an aqueous solution of a heteropoly acid to extract vanadium and nickel, impregnating with a water soluble cobalt or nickel salt and calcining at a maximum temperature of about 450° C.
Claim 2
Dependent Claim
45 words
An improved process for regenerating spent hydrofining catalysts which comprises contacting spent catalyst with an aqueous solution of a heteropoly acid to extract vanadium and nickel, impregnating with a water soluble cobalt or nickel salt and calcining at a maximum temperature of about 450° C.
Claim 3
Dependent Claim
17 words
The process of claim 1 in which the catalyst is impregnated with a water soluble cobalt salt.
Claim 4
Dependent Claim
16 words
The process of claim 1 in which the impregnation and calcination are repeated at least once.
Claim 5
Dependent Claim
16 words
The process of claim 1 in which the hydrofining catalyst comprises a cobalt-molybdenum loaded alumina support.
Claim 6
Dependent Claim
76 words
The process of claim 1 in which the heteropoly acid is represented by the general formula H x (YM 12 O 40 ), where Y is at least one element selected from the group consisting of phosphorus, silicon, titanium, germanium, arsenic, zirconium, thorium and cerium, M is at least one element selected from the group consisting of molybdenum, tungsten, niobium and tantalum and x is 3 when Y is pentavalent and 4 when Y is tetravalent.
Claim 7
Dependent Claim
26 words
The process of claim 5 in which Y is at least one of phosphorus and silicon and M is at least one of molybdenum and tungsten.
Claim 8
Dependent Claim
14 words
The process of claim 6 in which Y is phosphorus and M is molybdenum.
Claim 9
Dependent Claim
14 words
The process of claim 6 in which Y is phosphorus and M is tungsten.
Claim 10
Dependent Claim
14 words
The process of claim 6 in which Y is silicon and M is molybdenum.
Claim 11
Dependent Claim
14 words
The process of claim 6 in which Y is silicon and M is tungsten.
Claim 12
Dependent Claim
29 words
The process of claim 5 in which up to one-half of M is replaced by at least one element selected from the group consisting of nickel, cobalt and vanadium.
Claim 13
Dependent Claim
25 words
The process of claim 1 in which the spent catalyst is contacted with the heteropoly acid at a temperature between ambient and about 80° C.
Claim 14
Dependent Claim
16 words
The process of claim 12 in which the temperature ranges from about 30° to 60° C.
Claim 15
Dependent Claim
27 words
The process of claim 1 in which the heteropoly acid is dissolved in an aqueous medium in a concentration ranging from about 0.1 to 25 wt. %.
Claim 16
Dependent Claim
17 words
The process of claim 14 in which the concentration ranges from about 0.2 to 6 wt. %.
Claim 17
Dependent Claim
19 words
The process of claim 14 in which the aqueous solution has a pH ranging from about 1 to 3.
Claim 18
Dependent Claim
15 words
The process of claim 16 in which the pH ranges from about 1.5 to 2.5.
Claim 19
Dependent Claim
27 words
The process of claim 1 in which the spent catalyst is contacted with heteropoly acid for a period of time of between about 4 to 200 hours.
Claim 20
Dependent Claim
18 words
The process of claim 8 in which the period of contact ranges from about 15 to 90 hours.
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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) | 1984-06-08 | 1984-12-08 | 1985-06-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-06-08 | 1988-12-08 | 1989-06-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-06-08 | 1992-12-08 | 1993-06-09 | $7700.00 | Window Closed / Lapsed |