US3901822A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process of regenerating a noble metal hydrogenation catalyst used in hydrogen peroxide production by the anthraquinone process
Assignee: FMC Corp
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Filing: 1973-11-14
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Granted: 1975-08-26
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Expires: 1993-11-14
Abstract
Abstract This invention describes a process for regenerating deactivated noble metal hydrogenation catalysts to restore their catalytic activity. The process involves contacting a deactivated noble metal hydrogenation catalyst with a polar organic solvent, then contacting the solvent-treated catalyst with an aqueous ammonium hydroxide solution followed by contacting the ammonium hydroxidetreated catalyst with steam and an oxygen-containing gas at temperatures from about 250*C to the transition temperature of the catalyst crystal structure whereby the catalytic activity of the catalyst is substantially improved.
Inventors
- 👤 Jhonce N Browning
- 👤 Nathan D Lee
- 👤 George H Smee
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 04:08
CPC Classifications
C; C01; C01B; C01B15/00; C01B15/01; C01B15/022; C01B15/023; B; B01; B01J; B01J23/00; B01J23/90; B01J23/96; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
149 words
PROCESS OF REGENERATING A DECATIVATED NOBLE METAL HYDROGENATION CATALYST USED IN THE PROCESS OF PRODUCING HYDROGEN PEROXIDE, WHEREIN SAID CATALYST CONTACTS AN ANTHRAQUINONE WORKING COMPOUND DISSOLVED IN A WORKING SOLUTION DURING HYDROGENATION OF SAID COMPOUND, WHICH COMPRISES CONTACTING SAID DECATIVATED CATALYST WITH A POLAR ORGANIC SOLVENT CONTAINING 1 TO 5 CARBON ATOMS FOR ABOUT 0.1 TO ABOUT 48 HOURS TO REMOVE ASSOCIATED WORKING SOLUTION AND SEPARATING THE TREATED CATALYST FROM THE SOLVENT, CONTACTING THE SOLVENT-TREATED CATALYST WITH AT LEAST A 1% AQUEOUS AMMONIUM HYDROXIDE SOLUTION FOR ABOUT 0.1 TO ABOUT 48 HOURS AT ABOUT 0* TO ABOUT 200*C AND SEPARATING THE CATALYST FROM THE AMMONIUM HYDROXIDE SOLUTION, AND CONTACTING THE AMMONIUM HYDROXXIDE-TREATED CATALYST WITH STEAM AND AN OXYGEN-CONTAINING GAS AT TEMPERATURES FROM ABOUT 250*C TO THE TRANSITION TEMPRATURE OF THE CATALYST CRYSTAL STRUCTURE FOR ABOUT 1 TO ABOUT 72 HOURS WHEREBY THE CATALYTIC ACTIVITY OF SAID CATALYST IS IMPROVED
Claim 2
Dependent Claim
149 words
PROCESS OF REGENERATING A DECATIVATED NOBLE METAL HYDROGENATION CATALYST USED IN THE PROCESS OF PRODUCING HYDROGEN PEROXIDE, WHEREIN SAID CATALYST CONTACTS AN ANTHRAQUINONE WORKING COMPOUND DISSOLVED IN A WORKING SOLUTION DURING HYDROGENATION OF SAID COMPOUND, WHICH COMPRISES CONTACTING SAID DECATIVATED CATALYST WITH A POLAR ORGANIC SOLVENT CONTAINING 1 TO 5 CARBON ATOMS FOR ABOUT 0.1 TO ABOUT 48 HOURS TO REMOVE ASSOCIATED WORKING SOLUTION AND SEPARATING THE TREATED CATALYST FROM THE SOLVENT, CONTACTING THE SOLVENT-TREATED CATALYST WITH AT LEAST A 1% AQUEOUS AMMONIUM HYDROXIDE SOLUTION FOR ABOUT 0.1 TO ABOUT 48 HOURS AT ABOUT 0* TO ABOUT 200*C AND SEPARATING THE CATALYST FROM THE AMMONIUM HYDROXIDE SOLUTION, AND CONTACTING THE AMMONIUM HYDROXXIDE-TREATED CATALYST WITH STEAM AND AN OXYGEN-CONTAINING GAS AT TEMPERATURES FROM ABOUT 250*C TO THE TRANSITION TEMPRATURE OF THE CATALYST CRYSTAL STRUCTURE FOR ABOUT 1 TO ABOUT 72 HOURS WHEREBY THE CATALYTIC ACTIVITY OF SAID CATALYST IS IMPROVED
Claim 3
Dependent Claim
26 words
The process of claim 1 in which the noble metal hydrogenation catalyst is selected from the group consisting of palladium, platinum, ruthenium, rubidium, rhodium and iridium.
Claim 4
Dependent Claim
14 words
The process of claim 1 in which the noble metal hydrogenation catalyst is palladium.
Claim 5
Dependent Claim
14 words
The process of claim 1 in which the noble metal hydrogenation catalyst is platinum.
Claim 6
Dependent Claim
47 words
The process of claim 1 in which the polar organic solvent is selected from the group consisting of methanol, ethanol, n-propanol, t-butanol, allyl alcohol, acetaldehyde, acetone, methyl ethyl ketone, formic acid, acetic acid, propionic acid, butyric acid, ethylene glycol, propylene glycol, 1,3-propanediol, meso-2, 3-butanediol, 1,4-butanediol and glycerol.
Claim 7
Dependent Claim
13 words
The process of claim 1 in which the polar organic solvent is methanol.
Claim 8
Dependent Claim
29 words
The process of claim 1 in which the solvent-treated catalyst is treated with a 1% to 30% aqueous ammonium hydroxide solution at temperatures from about 30* to about 70*C.
Claim 9
Dependent Claim
27 words
The process of claim 1 in which the solvent-treated catalyst is treated with a 15% aqueous ammonium hydroxide solution at temperatures from about 45* to about 55*C.
Claim 10
Dependent Claim
27 words
The process of claim 3 in which the ammonium hydroxide-treated catalyst is contacted with steam and an oxygen-containing gas at temperatures from about 250* to about 380*C.
Claim 11
Dependent Claim
27 words
The process of claim 4 in which the ammonium hydroxide-treated catalyst is contacted with steam and an oxygen-containing gas at temperatures from about 250* to about 590*C.
Claim 12
Dependent Claim
30 words
The process of claim 1 in which the ammonium hydroxide-treated catalyst is contacted with steam and a sufficient amount of an oxygen-containing gas to provide 1% to 5% of oxygen.
Claim 13
Dependent Claim
52 words
THE PROCESS OF CLAIM 1 IN WHICH THE AMMONIUM HYDIOXIDE-TREATED CATALYST IS CONTACTED WITH STEAM AND AN INERT GAS AT TEMPERATURES FROM ABOUT 250*C TO THE TRANSITION TEMPERATURE OF THE CATALYST CRYSTAL STRUCTURE FOR ABOUT 0.1 TO ABOUT 48 HOURS PRIOR TO CONTACTING THE CATALYST WITH SAID STEAM AND AN OXYGEN-CONTAINING GAS.
Claim 14
Dependent Claim
146 words
Process of regenerating a hydrogenation catalyst selected from the group consisting of palladium, and platinum used in the process of producing hydrogen peroxide, wherein said catalyst contacts an anthraquinone working compound dissolved in a working solution during hydrogenation of said compound, which comprises: contacting said catalyst with methanol for about 0.1 to about 48 hours and separating the treated catalyst from the methanol; contacting the methanol-treated catalyst with a 1% to 30% aqueous ammonium hydroxide solution at temperatures from about 30* to about 70*C for about 0.1 to about 48 hours and separating the catalyst from the ammonium hydroxide solution; and contacting the ammonium hydroxide-treated catalyst with steam and a sufficient amount of an oxygen-containing gas to provide 1% to 5% oxygen at temperatures from about 300* to about 350*C for about 1 to about 72 hours whereby the catalytic activity of said catalyst is improved.
Claim 15
Dependent Claim
146 words
Process of regenerating a hydrogenation catalyst selected from the group consisting of palladium, and platinum used in the process of producing hydrogen peroxide, wherein said catalyst contacts an anthraquinone working compound dissolved in a working solution during hydrogenation of said compound, which comprises: contacting said catalyst with methanol for about 0.1 to about 48 hours and separating the treated catalyst from the methanol; contacting the methanol-treated catalyst with a 1% to 30% aqueous ammonium hydroxide solution at temperatures from about 30* to about 70*C for about 0.1 to about 48 hours and separating the catalyst from the ammonium hydroxide solution; and contacting the ammonium hydroxide-treated catalyst with steam and a sufficient amount of an oxygen-containing gas to provide 1% to 5% oxygen at temperatures from about 300* to about 350*C for about 1 to about 72 hours whereby the catalytic activity of said catalyst is improved.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-08-25 | 1979-02-24 | 1979-08-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-08-25 | 1983-02-24 | 1983-08-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-08-25 | 1987-02-24 | 1987-08-26 | $7700.00 | Window Closed / Lapsed |