EP0238341B2 - Granulierte Bleichaktivatorzusammensetzungen - Google Patents

Granulierte Bleichaktivatorzusammensetzungen Download PDF

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Publication number
EP0238341B2
EP0238341B2 EP87302379A EP87302379A EP0238341B2 EP 0238341 B2 EP0238341 B2 EP 0238341B2 EP 87302379 A EP87302379 A EP 87302379A EP 87302379 A EP87302379 A EP 87302379A EP 0238341 B2 EP0238341 B2 EP 0238341B2
Authority
EP
European Patent Office
Prior art keywords
activator
process according
granules
binder
disintegration aid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP87302379A
Other languages
English (en)
French (fr)
Other versions
EP0238341B1 (de
EP0238341A2 (de
EP0238341A3 (en
Inventor
John Townend
Anthony John Gradwell
John David Withenshaw
Rudolph Hirsch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Warwick International Ltd
Original Assignee
WARWICK INTERNATIONAL GROUP PLC
Warwick International Group Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=10594881&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0238341(B2) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by WARWICK INTERNATIONAL GROUP PLC, Warwick International Group Ltd filed Critical WARWICK INTERNATIONAL GROUP PLC
Priority to AT87302379T priority Critical patent/ATE68010T1/de
Publication of EP0238341A2 publication Critical patent/EP0238341A2/de
Publication of EP0238341A3 publication Critical patent/EP0238341A3/en
Publication of EP0238341B1 publication Critical patent/EP0238341B1/de
Application granted granted Critical
Publication of EP0238341B2 publication Critical patent/EP0238341B2/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives

Definitions

  • bleach activator granules are produced by mixing dry particles of the activator, which is usually tetraacetylglycolurile, with inorganic salts containing water of hydration and then moistening the blend with water or a solution of granulating aid, which is selected from inorganic salts, organic binders and detergent compounds. No mixtures of such granulating aids are specifically exemplified. The granules are then coated with water-insoluble solid coating substances such as magnesium oxide.
  • the process can produce granule compositions in which the presence of the disintegration aid causes substantial increase in the activity of the composition when dissolved in water at 20°C containing perborate and a detergent base in a simulation of a cold-fill system (PA 20).
  • the objective of the invention here is to reduce the quantity of undissolved activator collecting in the sump of the machine by effecting rapid release of the available peracid.
  • the product of the process show an increase in activity of more than 1.3 times compared to the compositions free of the granulation aid after 2 minutes of the test and an increase of more than 1.3 after 5 minutes of the test.
  • the 2 and 5 minutes activities at 20°C are measured by the following test.
  • the granulated composition (3g) is added to 1 litre of distilled water containing 100 ppm of calcium ions and 40g of a spray dried detergent base (ECE detergent base obtained from the Society of Dyers and Colourists, Bradford, W. Yorks), thermostatically controlled at 20°C.
  • EAE detergent base obtained from the Society of Dyers and Colourists, Bradford, W. Yorks
  • Sodium perborate tetrahydrate (12g) is added and the timer set to zero. Aliquots of 50 ml are taken at 2, 5 min and titrated as described above. The results are expressed as moles of peracid liberated per g of activator as a percentage of the theoretical quantity available.
  • the granule disintegration aid can be any water soluble material comprising sequestering agent that will promote rupture of the granules and exposure of the activator particles to the water. It is advantageous because the granule disintegration aid has stabilising properties upon the peracid species formed on the reaction of the bleach and the activator. By using these stabilising compounds it is possible to maintain the peracid activity over an extended period in the wash as compared to compositions free of the compounds. Thus the 30 minute activity at 40°C (as defined above) can be maintained at, or close to, the 5 minute activity at 40°C.
  • the disintegration aid comprises a sequestering agent or mixture of sequestering agents. It may comprise an amino carboxylic acid sequestering agent, for instance nitrilo triacetic acid or ethylene diamine tetra acetic acid or diethylene triamine penta acetic acid (or salts thereof) or a low molecular weight anionic polymer formed from ethylenically unsaturated monomers e.g. unsaturated carboxylic acid or sulphonic acid monomers, such as acrylic acid, but preferably the disintegration aid comprises a phosphonic acid sequestrant or stabiliser.
  • an amino carboxylic acid sequestering agent for instance nitrilo triacetic acid or ethylene diamine tetra acetic acid or diethylene triamine penta acetic acid (or salts thereof) or a low molecular weight anionic polymer formed from ethylenically unsaturated monomers e.g. unsaturated carboxylic acid or sulphonic acid
  • the disintegration aid may comprise, in addition to such sequestering agents, water-soluble inorganic salts, such as alkali metal or alkaline earth metal salts, preferably sodium, potassium calcium or magnesium salts or mixtures.
  • the salts may be the water-soluble sulphates, carbonates or halides, usually chlorides, mixtures can be used. Particularly suitable examples are sodium sulphate and magnesium sulphate.
  • the binder must be an organic polymeric binder that can be a natural or synthetic polymer and can be water swellable or water soluble.
  • Synthetic binders include polyacrylates, polymaleates and polyvinyl pyrollidones, which may be cross linked, e.g., the cross linked polyvinyl pyrollidone sold under the trade mark Gafdis.
  • the binder is a natural binder (including derivatives thereof), most preferably a starch binder, generally a starch ether, or a cellulose binder, generally a cellulose ether or ester.
  • Particularly preferred binders are carboxymethyl cellulose CMC.
  • the amount of granulating aid(s) will depend on the granulation aid(s) being used and on the binder and the amount of binder but is generally in the range 1 to 20%, preferably 2 to 15% and most preferably 3 to 10% by weight of the activator, binder and granulating aid(s).
  • the cation should contribute from 0.165% by weight of the granule, preferably 0.3 to 2.0%, most preferably 0.4 to 1.5%.
  • the product granules preferably consist substantially only of the activator, binder and disintegration aid(s)
  • other components of the final detergent may be included in the process if desired in any suitable amounts.
  • Preferably however such additions provide less than 10% and generally less than 5% by weight of the granules.
  • One component that can usefully be included in the granules is optical brightening agent since its incorporation in the granules avoids the problems associated with incorporating it in the remainder of the detergent composition. For instance it may be damaged by the spray drying to which the remainder of the composition is generally subjected.
  • Another component that can conveniently be co-granulated is an antisudsing (anti foaming) or foam stabilising agent.
  • Other components that may be cogranulated are other components of detergent compositions such as surfactants, anti redeposition acids, builders, pigments or dyes and enzymes.
  • the granules preferably have an average particle size of between 300 and 1500 »m, most preferably 500 to 1000 »m. Preferably substantially none of them have a size above 2000 »m and preferably not above 1700 »m. Preferably none of the granules have a size below 50 »m and most preferably none have a size below about 125 »m. Granules that are too fine are preferably separated from the granules and recycled for further granulation, often after crushing.
  • a particular advantage of the invention is that the large amounts of binder that can be used minimise the risk of formation of fines.
  • the resultant granules can be incorporated in conventional detergent compositions that contain a suitable bleach component that is activated by the activator.
  • the preferred bleaches are peroxy compounds, especially perborates such as sodium perborate tetrahydrate but others that can be used include sodium perborate monohydrate or sodium percarbonate.
  • the detergent may contain, in addition to surfactants, detergent builders and anti-redeposition aids, enzymes, anti-sudsing agents, foam stabilisers,optical brightening agents, pigments, dyes and perfumes, sequestrants, halide salts such as sodium bromide, manganese salts such as manganous sulphate and inert fillers such as sodium sulphate or silicate.
  • a particular advantage of the invention is that it is not necessary to include phosphates, although they may be included if desired.
  • the amount of activator, based on the total weight of the detergent may be conventional or may be less than usual, because of the increased activity. Typical amounts are 1 to 5% based on the total detergent, or 10 to 50% based on the bleach.
  • the standard composition is made by the following process:- Into a suitable mixing machine is weighed: TAED 1012g CMC 56g The dry components are mixed for 3 minutes after which Water 233g is added, whilst mixing is continued, over 2 minutes. The product is then discharged and dried for 15 minutes at 60°C using a fluid bed drier.
  • compositions made by these general techniques were sieved to separate a fraction of 1000 to 1700 »m and the granules were then tested for activity by the method described above.
  • Granules of activator were formed using a range of conventional table disintegration aids, i.e. which are water-swellable, instead of the water-soluble disintegration aids used in the present invention.
  • a process similar to that used in the reference example was used but replacing part of the binder with the disintegrant.
  • the type and amount (weight percentage based on total dry ingredients) of disintegrant and PA20 values are given in the table below:
  • Table 3 shows that conventional disintegration agents of the water-swellable type produce granules which have even worse PA20 values than the standard composition.
  • ⁇ R% in the table is the percentage difference in stain removal as measured by reflectance from a washed swatch of stained cloth, with the value of ⁇ R% for the standard composition being given the value 0.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)

Claims (11)

  1. Verfahren zur Herstellung eines granulierten Bleichmittelaktivators, worin Teilchen aus organischem Bindemittelmaterial und Teilchen aus Bleichmittelaktivator trocken vermischt, während des Mischens durch eine wäßrige Lösung angefeuchtet und getroknet werden, dadurch gekennzeichnet, daß die Lösung ein gelöstes, wasserlösliches Komplexierungsmittel umfaßendes Granulatsprenghilfsmittel umfaßt.
  2. Verfahren nach Anspruch 1, worin das Granulatsprenghilfsmittel unter Aminocarbonsäuren, Phosphonsäuren und anionischen Polymeren mit niedrigem Molekulargewicht, welche aus ethylenisch ungesättigten Monomeren gebildet werden, ausgewählt ist und vorzugsweise ein Phosphonsäurekomplexierungsmittel ist.
  3. Verfahren nach Anspruch 1 oder 2, worin das Granulatsprenghilfsmittel auch ein anorganisches Salz umfaßt.
  4. Verfahren nach einem der vorstehenden den Ansprüche, worin das Gewichtsverhältnis von Aktivator zu Bindemittel im Bereich von 98:2 bis 30:70, vorzugsweise von 89:11 bis 50:50 oder bis 55:45 reicht, und worin die Menge an Granulatsprenghilfsmittel im Bereich von 1 bis 20 Gew.-% des Gesamtgewichtes von Aktivator, Bindemittel und Granulatsprenghilfsmittel, vorzugsweise 1 bis 15 %, beträgt.
  5. Verfahren nach einem der vorstehenden Ansprüche, worin das Bindemittel unter Stärke und Cellulosebindemitteln vorzugsweise Carboxymethylcellulose, ausgewählt ist.
  6. Verfahren nach einem der vorstehenden Ansprüche, worin die Körnchen im wesentlichen nur aus dem Aktivator, dem Bindemittel, dem Sprenghilfsmittel und 0 bis 10 % von anderen Komponenten, welche wahlweise einen oder mehrere optische Aufheller und/oder Antischaummittel beinhalten, bestehen.
  7. Verfahren nach einem der vorstehenden Ansprüche, worin der Aktivator Tetraacetylethlendiamin ist.
  8. Verfahren nach einem der vorstehenden Ansprüche, worin der Aktivator am Beginn in Form von Teilchen zur Verfügung gestellt wird, weiche Größen im Bereich von 100 bis 300 »m besitzen, und die Granulate eine mittlere Teilchengröße im Bereich von 300 bis 1500 »m aufweisen, wobei im wesentlichen keines der Granulate eine Größe über 1700 »m besitzt.
  9. Verfahren nach einem der vorstehenden Ansprüche, worin die Lösung im wesentlichen von organischen Bindemittelmaterial frei ist.
  10. Verfahren nach einem der vorstehenden Ansprüche, worin im wesentlichen das gesamte wasserlösliche Granulasprenghilfsmittel in der wäßrigen Lösung gelöst ist.
  11. Granulatdetergenszusammensetzung, welche das Produkt eines Verfahrens gemäß einem der vorstehenden Ansprüche, eine Detergenskomponente und eine Bleichmittelkomponente enthält.
EP87302379A 1986-03-19 1987-03-19 Granulierte Bleichaktivatorzusammensetzungen Expired - Lifetime EP0238341B2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87302379T ATE68010T1 (de) 1986-03-19 1987-03-19 Granulierte bleichaktivatorzusammensetzungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB868606804A GB8606804D0 (en) 1986-03-19 1986-03-19 Particulate bleach activator composition
GB8606804 1986-03-19

Publications (4)

Publication Number Publication Date
EP0238341A2 EP0238341A2 (de) 1987-09-23
EP0238341A3 EP0238341A3 (en) 1988-08-17
EP0238341B1 EP0238341B1 (de) 1991-10-02
EP0238341B2 true EP0238341B2 (de) 1995-12-13

Family

ID=10594881

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87302379A Expired - Lifetime EP0238341B2 (de) 1986-03-19 1987-03-19 Granulierte Bleichaktivatorzusammensetzungen

Country Status (7)

Country Link
EP (1) EP0238341B2 (de)
JP (1) JP2528863B2 (de)
AT (1) ATE68010T1 (de)
DE (1) DE3773418D1 (de)
ES (1) ES2026180T5 (de)
GB (1) GB8606804D0 (de)
GR (1) GR3003106T3 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7138139B2 (en) 2002-10-22 2006-11-21 Rohm And Haas Company Tablet coating
US7550156B2 (en) 2001-11-23 2009-06-23 Rohm And Haas Company Optimised pellet formulations

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5112514A (en) * 1986-11-06 1992-05-12 The Clorox Company Oxidant detergent containing stable bleach activator granules
US5002691A (en) * 1986-11-06 1991-03-26 The Clorox Company Oxidant detergent containing stable bleach activator granules
DE3826092A1 (de) * 1988-08-01 1990-02-08 Henkel Kgaa Granulares, bleichaktivatoren enthaltendes bleichhilfsmittel mit verbesserten eigenschaften
US5269962A (en) * 1988-10-14 1993-12-14 The Clorox Company Oxidant composition containing stable bleach activator granules
US5055218A (en) * 1990-04-13 1991-10-08 The Procter & Gamble Company Bleach granules containing an amidoperoxyacid
GB9323634D0 (en) * 1993-11-16 1994-01-05 Warwick Int Ltd Bleach activator compositions
DE19841184A1 (de) 1998-09-09 2000-03-16 Clariant Gmbh Bleichaktivatorgranulate
GB2345701A (en) * 1999-01-12 2000-07-19 Procter & Gamble Particulate bleaching components
DE60000022T2 (de) 1999-03-05 2002-03-14 Rohm & Haas Verbesserte teilchenförmige Zusammensetzungen
GB0710559D0 (en) * 2007-06-02 2007-07-11 Reckitt Benckiser Nv Composition
US9587205B2 (en) 2012-05-18 2017-03-07 Warwick International Group Limited Activation of peroxygen bleach

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2048331A1 (de) * 1970-10-01 1972-04-06 Henkel & Cie GmbH, 4000 Dusseldorf Feste, pulverförmige bis kornige Mittel zur Herstellung von kaltwirksamen Bleich flotten, insbesondere von kaltwirksamen blei chenden Waschlaugen, und Verfahren zur Her stellung dieser Mittel
JPS5527333A (en) * 1978-08-16 1980-02-27 Kao Corp Bleaching agent composition
JPS5851999B2 (ja) * 1978-08-30 1983-11-19 花王株式会社 漂白剤組成物
GB2053998B (en) * 1979-07-06 1983-04-20 Unilever Ltd Particulate bleach composition
DE3268039D1 (en) * 1981-09-28 1986-01-30 Basf Ag Granular bleach activator
DE3247893A1 (de) * 1982-12-24 1984-06-28 Henkel KGaA, 4000 Düsseldorf Bleichmittel und bleichmittelhaltiges waschmittel
JPS59196399A (ja) * 1983-04-22 1984-11-07 花王株式会社 漂白剤組成物
DE3417820A1 (de) * 1984-05-14 1985-11-14 Henkel KGaA, 4000 Düsseldorf Verfahren zur herstellung eines waschzusatzes in tablettenform

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7550156B2 (en) 2001-11-23 2009-06-23 Rohm And Haas Company Optimised pellet formulations
US7138139B2 (en) 2002-10-22 2006-11-21 Rohm And Haas Company Tablet coating

Also Published As

Publication number Publication date
GR3003106T3 (en) 1993-02-17
EP0238341B1 (de) 1991-10-02
GB8606804D0 (en) 1986-04-23
EP0238341A2 (de) 1987-09-23
JPS62230898A (ja) 1987-10-09
ES2026180T5 (es) 1996-03-16
ES2026180T3 (es) 1992-04-16
JP2528863B2 (ja) 1996-08-28
EP0238341A3 (en) 1988-08-17
DE3773418D1 (de) 1991-11-07
ATE68010T1 (de) 1991-10-15

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