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US4599321A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the manufacture of spherical bodies by selective agglomeration

Assignee: Chevron USA Inc
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Filing: 1985-01-15
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Granted: 1986-07-08
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Expires: 2005-01-15
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Abstract

Abstract This invention relates to the preparation of small substantially spherical solid catalysts. More particularly, the process produces strong solid substantially spherical agglomerates comprising inorganic materials, which process comprises: (a) mixing at high speed a portion of an inorganic material in the form of hydrophilic micron-sized particles in a water-immiscible liquid thereby forming a dispersion; (b) gradually adding to the dispersion an aqueous phase while containing the high speed mixing until substantially spherical microagglomerates form within the water-immiscible liquid; (c) subjecting the microagglomerates to agitation in a vessel having a hydrophobic inner surface at a speed low enough to achieve substantially uniformly sized spherical agglomerates; (d) drying the agglomerates to produce hardened substantially spherical uniformly sized agglomerates; and (e) optionally further separating the agglomerates by size. Optionally, the aqueous phase in step (b) may include the soluble salts of catalytic metals, acids and bases and/or colloidal-sized inorganic particles. These spherical particles have diameters generally between 1 to 5 millimeters and are useful as catalysts, or catalyst supports, where the catalytic components are subsequently deposited on the support.

Inventors

  • 👤 Andrew Rainis

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 21:12
CPC Classifications
B; B01; B01J; B01J37/00; B01J37/0009

Claims Analysis

Total Claims: 26
Claim 1
Independent Claim 125 words
A process for producing solid substantially spherical agglomerates of substantially inorganic material, which process comprises: (a) mixing at high speed a portion of an inorganic material in the form of hydrophilic micron-sized particles in a water-immiscible liquid thereby forming a dispersion; (b) gradually adding to said dispersion an aqueous phase while continuing said high speed mixing until substantially spherical hydrous micro-agglomerates form within said water immiscible liquid; (c) subjecting said micro-agglomerates in a vessel having a hydrophobic inner surface to agitation at a speed low enough to achieve uniformly sized substantially spherical agglomerates; (d) separating said agglomerates obtained from said water-immiscible liquid; and (e) drying said agglomerates to produce hardened uniformly sized substantially spherical agglomerates having a diameter of between about 1 and 5 mm.
Claim 2
Dependent Claim 125 words
A process for producing solid substantially spherical agglomerates of substantially inorganic material, which process comprises: (a) mixing at high speed a portion of an inorganic material in the form of hydrophilic micron-sized particles in a water-immiscible liquid thereby forming a dispersion; (b) gradually adding to said dispersion an aqueous phase while continuing said high speed mixing until substantially spherical hydrous micro-agglomerates form within said water immiscible liquid; (c) subjecting said micro-agglomerates in a vessel having a hydrophobic inner surface to agitation at a speed low enough to achieve uniformly sized substantially spherical agglomerates; (d) separating said agglomerates obtained from said water-immiscible liquid; and (e) drying said agglomerates to produce hardened uniformly sized substantially spherical agglomerates having a diameter of between about 1 and 5 mm.
Claim 3
Dependent Claim 23 words
The process of claim 1 wherein in step (b) said aqueous phase contains about 0.1 to 70% by weight of soluble metal salt.
Claim 4
Dependent Claim 21 words
The process of claim 1 wherein in step (e) the size of said agglomerates is beween about 2 to 4 millimeters.
Claim 5
Dependent Claim 11 words
The process of claim 1 wherein the inorganic particles comprise zeolite.
Claim 6
Dependent Claim 11 words
The process of claim 1 wherein the inorganic particles comprise silica.
Claim 7
Dependent Claim 11 words
The process of claim 1 wherein the inorganic particles comprise alumina.
Claim 8
Dependent Claim 24 words
The process of claim 1 wherein the high speed mixing in steps (a) and (b) is between about 2500 and 4000 revolutions per minute.
Claim 9
Dependent Claim 22 words
The process of claim 1 wherein the low speed mixing in step (c) is between about 200 to 400 revolutions per minute.
Claim 10
Dependent Claim 12 words
The process of claim 1 wherein said water-immiscible liquid is a fluorocarbon.
Claim 11
Dependent Claim 10 words
The process of claim 9 wherein said fluorocarbon is 1,1,2-trichloro-1,2,2-trifluoroethane.
Claim 12
Dependent Claim 116 words
A process for producing substantially spherical agglomerates, which process comprises: (a) agitating at high speed a liquid reaction mixture which comprises a water immiscible liquid and hydrophilic micron-sized inorganic particles to form a dispersion; (b) continuing to agitate at high speed said reaction mixture while adding slowly dropwise an aqueous phase containing colloidal-sized inorganic particles; (c) then subjecting the product of step (b) in a vessel having a hydrophobic inner surface to low speed mixing to produce substantially spherical uniformly sized agglomerates; (d) isolating said agglomerates of step (c) from the liquid phase; and (e) drying said agglomerates to produce hardened substantially spherical uniformly sized agglomerates having a diameter of between about 1 and 5 mm.
Claim 13
Dependent Claim 116 words
A process for producing substantially spherical agglomerates, which process comprises: (a) agitating at high speed a liquid reaction mixture which comprises a water immiscible liquid and hydrophilic micron-sized inorganic particles to form a dispersion; (b) continuing to agitate at high speed said reaction mixture while adding slowly dropwise an aqueous phase containing colloidal-sized inorganic particles; (c) then subjecting the product of step (b) in a vessel having a hydrophobic inner surface to low speed mixing to produce substantially spherical uniformly sized agglomerates; (d) isolating said agglomerates of step (c) from the liquid phase; and (e) drying said agglomerates to produce hardened substantially spherical uniformly sized agglomerates having a diameter of between about 1 and 5 mm.
Claim 14
Dependent Claim 24 words
The process of claim 11 wherein in step (b) said aqueous phase contains about 0.1 to 70% by weight of a soluble metal salt.
Claim 15
Dependent Claim 22 words
The process of claim 11 wherein in step (e) the diameter of the hardened agglomerates is between about 2 to 4 mm.
Claim 16
Dependent Claim 17 words
The process of claim 13 wherein the mircon-sized particles are zeolite and the colloidal particles are silica.
Claim 17
Dependent Claim 19 words
The process of claim 14 wherein the weight ratio of zeolite to silica is between about 40:60 and 60:40.
Claim 18
Dependent Claim 17 words
The process of claim 13 wherein the micron-sized particles are zeolite and the colloidal particles are alumina.
Claim 19
Dependent Claim 18 words
The process of claim 16 wherein the weight ratio of zeolite to alumina is about 40:60 to 60:40.
Claim 20
Dependent Claim 19 words
The process of claim 11 wherein the high speed mixing is between about 2500 and 4000 revolutions per minute.
Claim 21
Dependent Claim 19 words
The process of claim 11 wherein the low speed mixing is between about 200 and 400 revolutions per minute.
Claim 22
Dependent Claim 12 words
The process of claim 11 wherein said water-immiscible liquid is a fluorocarbon.
Claim 23
Dependent Claim 10 words
The process of claim 20 wherein said fluorocarbon is 1,2-dibromo-1,1,2,2-tetrafluoroethane.
Claim 24
Dependent Claim 16 words
The process of claim 21 which further includes: (f) separating said agglomerates of step (e) size.
Claim 25
Dependent Claim 104 words
A continuous sequential process for producing substantially spherical agglomerates, which process comprises: (a) agitating at high speed in a continuous mixer, a reaction mixture which itself comprises: (i) a water-immiscible liquid; (ii) hydrophilic micron-sized inorganic particles; and (iii) an aqueous phase containing colloidal-sized inorganic particles; (b) subjecting the product of step (a) in a different vessel having a hydrophobic inner surface to low speed mixing to produce substantially spherical uniformly sized agglomerates; (c) separating the agglomerates of step (b) from the liquid; and (d) drying said agglomerates to produce hardened substantially spherical sized agglomerates having a diameter of between about 1 and 5 mm.
Claim 26
Dependent Claim 104 words
A continuous sequential process for producing substantially spherical agglomerates, which process comprises: (a) agitating at high speed in a continuous mixer, a reaction mixture which itself comprises: (i) a water-immiscible liquid; (ii) hydrophilic micron-sized inorganic particles; and (iii) an aqueous phase containing colloidal-sized inorganic particles; (b) subjecting the product of step (a) in a different vessel having a hydrophobic inner surface to low speed mixing to produce substantially spherical uniformly sized agglomerates; (c) separating the agglomerates of step (b) from the liquid; and (d) drying said agglomerates to produce hardened substantially spherical sized agglomerates having a diameter of between about 1 and 5 mm.

References Cited (Backward Citations)

US2474911A Cited
US3296151A Cited
US3515684A Cited
US4507396A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1989-07-07 1990-01-06 1990-07-08 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1993-07-07 1994-01-06 1994-07-08 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1997-07-07 1998-01-06 1998-07-08 $7700.00 Window Closed / Lapsed

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