US4268415A
Expired / Lapsed
US
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Regeneration of spent hydrodesulfurization catalysts with heteropoly acids and hydrogen peroxide
Assignee: ExxonMobil Technology and Engineering Co
•
Filing: 1979-07-19
•
Granted: 1981-05-19
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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, to which dilute hydrogen peroxide is added, results in a significant enhancement in the rate and extent of carbon and metals removal. Forms of deposited vanadium intractable by other treatments are also removed. The process results in substantially complete regeneration of catalytic activity.
Inventors
- 👤 Raam R. Mohan
- 👤 Bernard G. Silbernagel
- 👤 Gopal H. Singhal
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 19:09
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
54 words
An improved process for regenerating spent hydrofining catalysts which comprises contacting spent catalyst with an aqueous solution of a heteropoly acid containing about 1 to 50 wt.% hydrogen peroxide, based on the amount of heteropolyacid, impregnating with a water soluble cobalt or nickel salt and calcining at a maximum temperature of about 450° C.
Claim 2
Dependent Claim
54 words
An improved process for regenerating spent hydrofining catalysts which comprises contacting spent catalyst with an aqueous solution of a heteropoly acid containing about 1 to 50 wt.% hydrogen peroxide, based on the amount of heteropolyacid, impregnating with a water soluble cobalt or nickel salt and calcining at a maximum temperature of about 450° C.
Claim 3
Dependent Claim
15 words
The process of claim 1 in which spent catalyst is pre-cleaned with an organic solvent.
Claim 4
Dependent Claim
17 words
The process of claim 1 in which the catalyst is impregnated with a water soluble cobalt salt.
Claim 5
Dependent Claim
16 words
The process of claim 1 in which the impregnation and calcination are repeated at least once.
Claim 6
Dependent Claim
16 words
The process of claim 1 in which the hydrofining catalyst comprises a cobalt-molybdenum loaded alumina support.
Claim 7
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 8
Dependent Claim
26 words
The process of claim 6 in which Y is at least one of phosphorus and silicon and M is at least one of molybdenum and tungsten.
Claim 9
Dependent Claim
14 words
The process of claim 7 in which Y is phosphorus and M is molybdenum.
Claim 10
Dependent Claim
29 words
The process of claim 6 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 11
Dependent Claim
27 words
The process of claim 1 in which the spent catalyst is contacted with the heteropoly acid/hydrogen peroxide solution at a temperature between ambient and about 80° C.
Claim 12
Dependent Claim
16 words
The process of claim 10 in which the temperature ranges from about 30° to 60° C.
Claim 13
Dependent Claim
20 words
The process of claim 1 in which the heteropoly acid in solution ranges from about 0.1 to 25 wt. %.
Claim 14
Dependent Claim
17 words
The process of claim 12 in which the concentration ranges from about 0.2 to 6 wt. %.
Claim 15
Dependent Claim
18 words
The process of claim 12 in which the solution has a pH ranging from about 1 to 3.
Claim 16
Dependent Claim
15 words
The process of claim 13 in which the pH ranges from about 1.5 to 2.5.
Claim 17
Dependent Claim
20 words
The process of claim 1 in which the concentration of hydrogen peroxide ranges from about 3 to 15 wt. %.
Claim 18
Dependent Claim
17 words
The process of claim 16 in which the concentration of hydrogen peroxide is about 15 wt. %.
Claim 19
Dependent Claim
30 words
The process of claim 1 in which the spent catalyst is contacted by the heteropoly acid/hydrogen peroxide solution for a period of time of between about 4 and 200 hours.
Claim 20
Dependent Claim
18 words
The process of claim 18 in which the period of contact ranges from about 10 to 50 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) | 1984-05-18 | 1984-11-17 | 1985-05-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-05-18 | 1988-11-17 | 1989-05-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-05-18 | 1992-11-17 | 1993-05-19 | $7700.00 | Window Closed / Lapsed |