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US4968500A Expired / Lapsed US ⏱️ 0.0 years remaining

Continuous method for preparation of granulated sodium perborate

Assignee: Evonik Operations GmbH
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Filing: 1989-05-17
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Granted: 1990-11-06
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Expires: 2009-05-17
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Abstract

Abstract The spray drying of a solution containing hydrogen peroxide and sodium metaborate to obtain primary particles which are immediately conveyed after leaving the drying zone to a granulating device and are then granulated in the presence of free and/or perborate water of crystallization. The granulated materials are dried, if necessary. The generally amorphous primary particles are converted into granulated materials with at least partially crystalline structure and significantly improved shelf life. The work is performed with advantage in a spray dryer with integrated fluid bed or in a compressing granulating device. The method is suitable for preparing perborate granulated materials with over 10% by wt., especially perborate monohydrate granular materials with 14-16% by wt. active oxygen.

Inventors

  • 👤 Birgit Bertsch-Frank
  • 👤 Klaus Mueller
  • 👤 Thomas Lieser

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 13:22
CPC Classifications
C; C01; C01B; C01B15/00; C01B15/055; C01B15/12; B; B01; B01J; B01J2/00; C01B15/126

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 138 words
A continuous method for the preparation of granulated perborate with an Oa-content of 14 to 16% by weight comprising the steps of: spraying an aqueous solution comprising hydrogen peroxide and sodium metaborate in a molar ratio of 0.9 to 1.1 into a drying zone to form droplets, wherein no nuclei of perborate are introduced into said drying zone, drying said droplets by means of a heated gas in said drying zone to thereby form powdery, essentially amorphous sodium perborate, conveying said powdery perborate after leaving said drying zone to a separate granulating zone, separated from said drying zone, adding water in sprayed form, vapor form, in the form of perborate containing water of crystallization or in the form of sodium perborate tetrahydrate to said powdery perborate and granulating by intimately bringing into contact said water and powdery perborate.
Claim 2
Dependent Claim 138 words
A continuous method for the preparation of granulated perborate with an Oa-content of 14 to 16% by weight comprising the steps of: spraying an aqueous solution comprising hydrogen peroxide and sodium metaborate in a molar ratio of 0.9 to 1.1 into a drying zone to form droplets, wherein no nuclei of perborate are introduced into said drying zone, drying said droplets by means of a heated gas in said drying zone to thereby form powdery, essentially amorphous sodium perborate, conveying said powdery perborate after leaving said drying zone to a separate granulating zone, separated from said drying zone, adding water in sprayed form, vapor form, in the form of perborate containing water of crystallization or in the form of sodium perborate tetrahydrate to said powdery perborate and granulating by intimately bringing into contact said water and powdery perborate.
Claim 3
Dependent Claim 25 words
The method of claim 1 wherein sodium perborate tetrahydrate is used as auxiliary granulating agent and the granulation is performed at 60° to 75° C.
Claim 4
Dependent Claim 16 words
The method according to claim 1 wherein the granulation is performed by compression of the perborate.
Claim 5
Dependent Claim 29 words
The method according to claim 3 wherein granulation in a fluidized bed is used to obtain a product with bulk density in the range of 0.3 to 0.6 g/ml.
Claim 6
Dependent Claim 26 words
The method according to claim 3 wherein granulation of sufficient compression is used to obtain a product with a bulk density of 0.4 to 1.0 g/ml.
Claim 7
Dependent Claim 15 words
The method according to claim 1 wherein the water is introduced into said granulating zone.
Claim 8
Dependent Claim 20 words
The method according to claim 1 wherein the water is introduced to said perborate immediately after leaving the drying zone.
Claim 9
Dependent Claim 20 words
The method according to claim 1 wherein an auxiliary granulating agent is present in the water used in sprayed form.
Claim 10
Dependent Claim 25 words
The method according to claim 1 wherein the water further contains an active oxygen stabilizer or surface active agent, or bleaching activator or mixture thereof.
Claim 11
Dependent Claim 18 words
The method according to claim 1, wherein the droplets and the heated gas are in a concurrent flow.
Claim 12
Dependent Claim 113 words
A continuous method for the preparation of granulated perborate with an Oa-content of 14 to 16% by weight, comprising the steps of: spraying an aqueous solution comprising hydrogen peroxide and sodium metaborate in a molar ratio of 0.9 to 1.1 into a drying zone to form droplets, wherein no nuclei of perborate are introduced into said drying zone, drying said droplets by means of a heated gas in said drying zone to thereby form powdery, essentially amorphous sodium perborate, conveying said powdery perborate after leaving said drying zone to a granulating zone, adding water in sprayed from to said powdery perborate and granulating by intimately bringing into contact said water and powdery perborate.
Claim 13
Dependent Claim 113 words
A continuous method for the preparation of granulated perborate with an Oa-content of 14 to 16% by weight, comprising the steps of: spraying an aqueous solution comprising hydrogen peroxide and sodium metaborate in a molar ratio of 0.9 to 1.1 into a drying zone to form droplets, wherein no nuclei of perborate are introduced into said drying zone, drying said droplets by means of a heated gas in said drying zone to thereby form powdery, essentially amorphous sodium perborate, conveying said powdery perborate after leaving said drying zone to a granulating zone, adding water in sprayed from to said powdery perborate and granulating by intimately bringing into contact said water and powdery perborate.
Claim 14
Dependent Claim 29 words
The method according to claim 11 wherein granulation in a fluidized bed is used to obtain a product with bulk density in the range of 0.3 to 0.6 g/ml.
Claim 15
Dependent Claim 26 words
The method according to claim 11 wherein granulation of sufficient compression is used to obtain a product with a bulk density of 0.4 to 1.0 g/ml.
Claim 16
Dependent Claim 15 words
The method according to claim 11 wherein the water is introduced into said granulating zone.
Claim 17
Dependent Claim 20 words
The method according to claim 11 wherein the water is introduced to said perborate immediately after leaving the drying zone.

References Cited (Backward Citations)

US3555696A Cited
US4002434A Cited
US4115519A Cited
US4185960A Cited
US4215097A Cited
US4681748A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-11-05 1994-05-07 1994-11-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-11-05 1998-05-07 1998-11-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-11-05 2002-05-07 2002-11-06 $7700.00 Window Closed / Lapsed

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