EP0336635A1 - Verfahren zur Herstellung von einem granulierten gefärbten Alkalisilikat - Google Patents

Verfahren zur Herstellung von einem granulierten gefärbten Alkalisilikat Download PDF

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Publication number
EP0336635A1
EP0336635A1 EP19890303091 EP89303091A EP0336635A1 EP 0336635 A1 EP0336635 A1 EP 0336635A1 EP 19890303091 EP19890303091 EP 19890303091 EP 89303091 A EP89303091 A EP 89303091A EP 0336635 A1 EP0336635 A1 EP 0336635A1
Authority
EP
European Patent Office
Prior art keywords
granules
coloured
alkali metal
silicate
granular material
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.)
Granted
Application number
EP19890303091
Other languages
English (en)
French (fr)
Other versions
EP0336635B1 (de
Inventor
Theo Jan Osinga
Joseph Pierre Hubert Theunissen
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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=8199773&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0336635(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Priority to AT89303091T priority Critical patent/ATE102647T1/de
Publication of EP0336635A1 publication Critical patent/EP0336635A1/de
Application granted granted Critical
Publication of EP0336635B1 publication Critical patent/EP0336635B1/de
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/08Silicates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/40Dyes ; Pigments

Definitions

  • the invention relates to coloured granules which can be used as speckles in detergent powders and to a process for manufacturing speckles.
  • Coloured granules in detergent compositions are well-known in the art, especially in phosphate containing detergent compositions and the detergent speckles therefore are usually mainly based on soluble inorganic salts like phosphates, especially sodium triphosphate, sodium sulphate or mixtures therefrom, which granules have been coated/impregnated with a solution or dispersion of a colourant i.e. a dye or pigment.
  • a colourant i.e. a dye or pigment.
  • the speckles are green or blue. Speckles give the detergent composition a more attractive consumer appeal, moreover it is possible to incorporate special purpose ingredients via the speckles in the detergent composition.
  • the amount of colourant in the granular material is so low as not to interfere with the washing process, moreover the speckles should be bright coloured and if possible the detergent speckle base material should serve a useful and practical purpose in the detergent composition.
  • the detergent speckle base material should serve a useful and practical purpose in the detergent composition.
  • the present invention provides coloured detergent speckles satisfying most of the above requirements in the form of granular alkali metal silicate which has been coated with a colourant i.e. a pigment or dye.
  • the alkali metal silicate is sodium silicate, more preferably metasilicate and/or disilicate.
  • Silicates have the functions of improving the washing effect and of corrosion inhibitor in detergent composition and consequently are a functional additive.
  • silicate hydrates as the base material for the speckles according to the present invention and sodium silicate penta- and/or hexahydrate give optimal results.
  • sodium silicate penta- and/or hexahydrate give optimal results.
  • the base material for the speckles consists substantially of sodium silicate it is, however, also possible to use as the base material for the speckles a mixture of materials in which at least 50% of the dry weight consists ot alkali metal silicate, the remainder being other inorganic materials like eg. zeolite, sodium sulfate or sodium phosphate if the latter can be tolerated in the eventual detergent composition.
  • the coloured silicate granules according to the present invention usually have an average particle size of 0.2 - 2mm, preferably from 0.8 to 1.6 mm, diameter. Granules with an spherical shape have advantages and then the diameter is taken to determine the size. Of course the actual size of the speckles desired depends on that of the detergent powder in which the speckles are incorporated.
  • the colourant i.e. dye or pigment, which forms a coating on the alkali metal silicate granules is normally present in an amount of 0.1 to 2.0% (w.w.) of the granules.
  • the colourant usually is a commercially available dye and compounds like Monastral Blue and Monastral Green + Unidispers Blue (ex CIBA-Geigy) are preferred. (Monastral dyes are ex ICI, England.)
  • the coloured detergent speckles are usually incorporated in detergent powders in a level between 0.1 - 5%, preferably between 0.2 and 2.0%, by weight of the total detergent composition.
  • the invention extends particularly to the use of sodium silicate having Na2O:SiO2 ratios from 1:1.2 to 1:3.3, preferably 1:1.5 to 1:3.0.
  • the higher ratios are generally less preferred because of slower solution.
  • the granules of alkali metal silicate can be prepared by a number of suitable procedures, for example metasilicate (Na2O:Silica ratio 1:1) can be granulated in a rotary barrel as described in GB 1149859 (Baker-Holloway).
  • silicates in compacted form is particularly valuable for speckles intended for the higher density detergent powder compositions, that is having a bulk density above 700 g/l, preferably above 800 g/l.
  • Sodium disilicate can be prepared with a bulk density between 700 and 900 g/l by compaction between rollers.
  • Sodium metasilicate can be prepared with a bulk density between 880 and 1,000 g/l using granulation in a rotary barrel.
  • a binder eg. silicate solution
  • detergent speckles are manufactured by a number of methods.
  • One method involved the spray-drying of a special coloured slurry but the obvious disadvantage is that thorough cleaning is required before normal detergent powder can be produced again.
  • Another method involved spraying a coloured solution onto a spray-dried detergent powder, but this requires, as the previous method, a large amount of coloured solution.
  • a solution of a colourant that also comprises a hydratable salt, preferably a warm and concentrated solution, to facilitate subsequent crystallisation.
  • zeolite containing detergent compositions this method was found not quite practical because a high percentage of colourant was required.
  • the coloured detergent speckles according to the present invention which are based on alkali metal silicate, can be prepared by spraying under suitable conditions a solution of a colourant on granular alkali metal silicate, which is kept in constant motion so as to avoid caking. This can be done e.g. by carrying out the operation in a fluidized bed, or in a mixer, followed by drying while keeping the granules in constant motion.
  • Suitable equipment for this technique comprises fluidized beds, nozzles for the coloured liquid, for hot and cool air, Tellschig*-type mixers consisting of rotating drums and fitted with a spray-nozzle, Loedige-type mixers consisting of fixed drums with an internal scraper fitted with a spray-nozzle, Nauta*-mixers of a type consisting of a conical vessel with a rotating scraper fitted with a spray-nozzle etc. (*stands for tradename).
  • the amount of dye solution or pigment suspension sprayed on the alkali metal silicate granules normally lies between 0.1 and 5.0% by weight, preferably between 0.5 - 2.0%, calculated on the alkali metal silicate.
  • the particle size distribution of the starting granules determines the size of the coloured speckles and most alkali metal silicate granules are available in various, often uniform or narrow particle size ranges which can be chosen dependent on the size desired in the detergent composition.
  • the solution which is sprayed onto the granular alkali metal silicate materiai usually contains from 0.05 to 50% of colourant preferably completely dissolved.
  • solubility of e.g. the dye in the solvent to be observed. Water is preferred as the solvent but it is sometimes advantageous to use (aqueous) methanol to increase the solubility of the dye.
  • the quantity of liquid sprayed onto the granules is normally between 0.1 and 5%, preferably between 0.5 and 2%, by weight calculated on the silicate and spraying normally is completed within a few minutes to half an hour, 2 to 10 minutes is typical.
  • the detergent speckles so obtained are distinctive, of uniform colour, resistant to attrition and have virtually the same particle size distribution as the alkali metal silicate starting granules have.
  • alkali metal silicates as a core for speckles is particularly efficient because, for one or more of the reasons,
  • 1.5 kg sodium metasilicate pentahydrate granules with a particle size between 0.2 and 1.2 mm was placed in a Loedige mixer of 5 litres. The mixer was switched on and the contents were pre-heated to 35 - 45°C by blowing in hot air with a temperature of 50°C. An aqueous solution containing 25% by weight of Monastral Blue was sprayed onto the granules for 5 minutes. The amount of solution sprayed onto the granules was 1% by weight calculated on the metasilicate. Consequently only 0.25% of dye was used relative to the metasilicate. Drying was also carried out at a temperature of 35-45°C for a period of 20 minutes.
  • the water content of the metasilicate was monitored during the drying and kept at around 43% by weight.
  • the detergent speckles were then cooled to 20°C by blowing in cool air.
  • the detergent speckles thus obtained showed excellent brightness, a deep hue, were uniformly coloured, colour-stable and the original particle size distribution had substantially been retained. Whe mixed in a detergent powder at a level of 1% by weight they imparted an excellent consumer appeal to the product.
  • Sodium disilicate Na2O:SiO2 ratio of 1:2 was spray dried to provide granules.

Landscapes

  • 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)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
EP89303091A 1988-03-30 1989-03-29 Verfahren zur Herstellung von einem granulierten gefärbten Alkalisilikat Revoked EP0336635B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT89303091T ATE102647T1 (de) 1988-03-30 1989-03-29 Verfahren zur herstellung von einem granulierten gefaerbten alkalisilikat.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP88200604 1988-03-30
EP88200604 1988-03-30

Publications (2)

Publication Number Publication Date
EP0336635A1 true EP0336635A1 (de) 1989-10-11
EP0336635B1 EP0336635B1 (de) 1994-03-09

Family

ID=8199773

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89303091A Revoked EP0336635B1 (de) 1988-03-30 1989-03-29 Verfahren zur Herstellung von einem granulierten gefärbten Alkalisilikat

Country Status (5)

Country Link
EP (1) EP0336635B1 (de)
JP (1) JPH01299898A (de)
AU (1) AU3223389A (de)
DE (1) DE68913575T2 (de)
ZA (1) ZA892357B (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0737739A2 (de) * 1995-04-13 1996-10-16 The Procter & Gamble Company Verfahren zur Herstellung eines Waschmittelteilchens
WO1997033965A1 (de) * 1996-03-14 1997-09-18 Henkel Kommanditgesellschaft Auf Aktien Verfahren und vorrichtung zur herstellung von farbgesprenkeltem pulverförmigem schuttgut
WO2000027980A1 (en) * 1998-11-06 2000-05-18 The Procter & Gamble Company Speckle particles and compositions containing the speckle particles
EP1113068A2 (de) * 1999-12-16 2001-07-04 Clariant GmbH Granulares Alkalischichtsilicat-Compound
US6545147B1 (en) 1999-09-10 2003-04-08 Clariant Gmbh Bleaching-active metal complexes
WO2007096052A1 (en) * 2006-02-25 2007-08-30 Unilever Plc Shading dye granule its use in a detergent formulation and process to make it
US20150105312A1 (en) * 2010-05-28 2015-04-16 Milliken & Company Colored Speckles For Use In Granular Detergents

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2771792A (en) * 1992-03-31 1993-11-08 Kyowa Hakko Kogyo Co. Ltd. Novel cosmetic

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3679610A (en) * 1968-07-30 1972-07-25 Philadelphia Quartz Co Tinted granules
DE2632367A1 (de) * 1975-07-23 1977-02-17 Procter & Gamble Granulierte gefaerbte partikel
DE2626383A1 (de) * 1976-06-12 1977-12-22 Baerle & Co Chem Fab Van Verfahren zur herstellung von modifizierten natriumsilikathydraten und danach hergestellte modifizierte natriumsilikathydrate sowie deren verwendung
EP0060728A1 (de) * 1981-03-18 1982-09-22 Unilever Plc Verfahren zur Herstellung von gefärbten Detergensteilchen

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE549160A (de) * 1956-04-23
BE791891A (en) * 1971-11-26 1973-05-24 Procter & Gamble Washing and cleaning compsns, to give bluing action - whasing and cleaning compsns, to give bluing action
DE2744753C2 (de) * 1977-10-05 1986-08-28 Joh. A. Benckiser Gmbh, 6700 Ludwigshafen Verfahren zur Herstellung von Granulaten

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3679610A (en) * 1968-07-30 1972-07-25 Philadelphia Quartz Co Tinted granules
DE1938756B2 (de) * 1968-07-30 1978-09-14 Philadelphia Quartz Co., Philadelphia, Pa. (V.St.A.) Poröses rasch lösliches Produkt auf Basis von hydratisiertem, kristallinem Natriumsilikat
DE2632367A1 (de) * 1975-07-23 1977-02-17 Procter & Gamble Granulierte gefaerbte partikel
DE2626383A1 (de) * 1976-06-12 1977-12-22 Baerle & Co Chem Fab Van Verfahren zur herstellung von modifizierten natriumsilikathydraten und danach hergestellte modifizierte natriumsilikathydrate sowie deren verwendung
EP0060728A1 (de) * 1981-03-18 1982-09-22 Unilever Plc Verfahren zur Herstellung von gefärbten Detergensteilchen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0737739A2 (de) * 1995-04-13 1996-10-16 The Procter & Gamble Company Verfahren zur Herstellung eines Waschmittelteilchens
EP0737739A3 (de) * 1995-04-13 1998-08-26 The Procter & Gamble Company Verfahren zur Herstellung eines Waschmittelteilchens
WO1997033965A1 (de) * 1996-03-14 1997-09-18 Henkel Kommanditgesellschaft Auf Aktien Verfahren und vorrichtung zur herstellung von farbgesprenkeltem pulverförmigem schuttgut
WO2000027980A1 (en) * 1998-11-06 2000-05-18 The Procter & Gamble Company Speckle particles and compositions containing the speckle particles
US6545147B1 (en) 1999-09-10 2003-04-08 Clariant Gmbh Bleaching-active metal complexes
EP1113068A2 (de) * 1999-12-16 2001-07-04 Clariant GmbH Granulares Alkalischichtsilicat-Compound
EP1113068A3 (de) * 1999-12-16 2001-12-19 Clariant GmbH Granulares Alkalischichtsilicat-Compound
WO2007096052A1 (en) * 2006-02-25 2007-08-30 Unilever Plc Shading dye granule its use in a detergent formulation and process to make it
US20150105312A1 (en) * 2010-05-28 2015-04-16 Milliken & Company Colored Speckles For Use In Granular Detergents
US11649417B2 (en) 2010-05-28 2023-05-16 Milliken & Company Colored speckles for use in granular detergents

Also Published As

Publication number Publication date
DE68913575D1 (de) 1994-04-14
JPH01299898A (ja) 1989-12-04
AU3223389A (en) 1989-10-05
ZA892357B (en) 1990-12-28
EP0336635B1 (de) 1994-03-09
DE68913575T2 (de) 1994-06-16

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