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US4061598A Expired / Lapsed US ⏱️ 0.0 years remaining

Catalyst for hydrogenating anthraquinones

Assignee: EIDP Inc
•
Filing: 1976-06-25
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Granted: 1977-12-06
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Expires: 1996-06-25
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Abstract

Abstract A palladium-on-alumina catalyst having high activity and long life and which gives low anthraquinone usage in the cyclic anthraquinone process for making H 2 O 2 is produced by impregnating the alumina under conditions such that the pore surfaces are rendered alkaline and the rate of diffusion of catalytic metal into the pores is controlled.

Inventors

  • 👤 Kamel Michel Makar

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 16:22
CPC Classifications
B; B01; B01J; B01J23/00; B01J23/38; B01J23/54; B01J23/56; B01J23/58; C; C01; C01B; C01B15/00; C01B15/01; C01B15/022; C01B15/023

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 223 words
A method for making catalysts which are useful for the hydrogenation of anthraquinones comprising the sequential steps of a. impregnating dry activated alumina particles with 2-20 parts by weight of alkali metal carbonate or alkaline earth metal carbonate and 0.1-10 parts by weight of a basic palladium salt, said parts by weight being based on 100 parts by weight of dry activated alumina prior to impregnation, by admixing the alumina with finely divided particles of the palladium salt and an aqueous solution of the carbonate in which the amount of water is sufficient to wet the pores, but not the outer surface of the alumina, and allowing the impregnated alumina to stand for a time sufficient to complete diffusion of the palladium within the wetted pores of the catalyst; b. reducing the palladium by dispersing the impregnated alumina in a dilute aqueous solution of reducing agent, the amount of reducing agent being sufficient to reduce substantially all the palladium to a zero valence state; c. separating the reduced catalyst from the solution of reducing agent, washing it with water and then removing substantially all the water therefrom while maintaining the catalyst at a temperature below about 100° C; and d. heating the dewatered catalyst in an oxidizing atmosphere for a period of at least about 1 hour at a temperature of 400°-650° C.
Claim 2
Independent Claim 223 words
A method for making catalysts which are useful for the hydrogenation of anthraquinones comprising the sequential steps of a. impregnating dry activated alumina particles with 2-20 parts by weight of alkali metal carbonate or alkaline earth metal carbonate and 0.1-10 parts by weight of a basic palladium salt, said parts by weight being based on 100 parts by weight of dry activated alumina prior to impregnation, by admixing the alumina with finely divided particles of the palladium salt and an aqueous solution of the carbonate in which the amount of water is sufficient to wet the pores, but not the outer surface of the alumina, and allowing the impregnated alumina to stand for a time sufficient to complete diffusion of the palladium within the wetted pores of the catalyst; b. reducing the palladium by dispersing the impregnated alumina in a dilute aqueous solution of reducing agent, the amount of reducing agent being sufficient to reduce substantially all the palladium to a zero valence state; c. separating the reduced catalyst from the solution of reducing agent, washing it with water and then removing substantially all the water therefrom while maintaining the catalyst at a temperature below about 100° C; and d. heating the dewatered catalyst in an oxidizing atmosphere for a period of at least about 1 hour at a temperature of 400°-650° C.
Claim 3
Dependent Claim 15 words
The method of claim 1 in which the basic palladium salt is sodium palladium chloride.
Claim 4
Dependent Claim 14 words
The method of claim 1 in which the alumina is impregnated with potassium bicarbonate.
Claim 5
Dependent Claim 15 words
The method of claim 1 in which the alumina is substantially free of alpha alumina.
Claim 6
Dependent Claim 16 words
The method of claim 4 in which the major crystalline structure of the alumina is gamma-alumina.
Claim 7
Dependent Claim 26 words
The method of claim 4 in which the major crystalline structure of the alumina is delta-alumina, theta-alumina or mixtures thereof substantially free of alpha-alumina and gamma-alumina.
Claim 8
Dependent Claim 18 words
The method of claim 1 in which the surface area of the alumina is 25-400 m 2 /gm.
Claim 9
Dependent Claim 19 words
The method of claim 1 in which the alumina is impregnated with 0.3-5 parts by weight basic palladium salt.
Claim 10
Dependent Claim 22 words
The method of claim 1 in which the temperature of the catalyst during the dewatering step is maintained below about 80° C.
Claim 11
Dependent Claim 12 words
The method of claim 1 in which the reducing agent is non-acidic.
Claim 12
Dependent Claim 12 words
The method of claim 10 in which the reducing agent is hydrazine.
Claim 13
Dependent Claim 28 words
The method of claim 1 in which the alumina is first impregnated with an aqueous solution of the carbonate and then admixed with the particles of palladium salt.
Claim 14
Dependent Claim 28 words
The method of claim 1 in which the alumina is first admixed with the particles of palladium salt and then inpregnated with the aqueous solution of the carbonate.

References Cited (Backward Citations)

US2657980A Cited
US3615207A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-12-05 1981-06-06 1981-12-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-12-05 1985-06-06 1985-12-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-12-05 1989-06-06 1989-12-06 $7700.00 Window Closed / Lapsed

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