EP0094250B2 - Verfahren zur Herstellung von Antischaummittel auf Silikonbasis enthaltenden Granulaten - Google Patents

Verfahren zur Herstellung von Antischaummittel auf Silikonbasis enthaltenden Granulaten Download PDF

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Publication number
EP0094250B2
EP0094250B2 EP83302643A EP83302643A EP0094250B2 EP 0094250 B2 EP0094250 B2 EP 0094250B2 EP 83302643 A EP83302643 A EP 83302643A EP 83302643 A EP83302643 A EP 83302643A EP 0094250 B2 EP0094250 B2 EP 0094250B2
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Prior art keywords
silicone
mixture
weight
carbon atoms
hydrophobic material
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EP83302643A
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English (en)
French (fr)
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EP0094250B1 (de
EP0094250A1 (de
Inventor
Ho Tan Tai
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Unilever PLC
Unilever NV
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Unilever PLC
Unilever NV
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Priority to AT83302643T priority Critical patent/ATE21115T1/de
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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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0026—Low foaming or foam regulating compositions
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38—Cationic compounds
    • C11D1/52—Carboxylic amides, alkylolamides or imides or their condensation products with alkylene oxides
    • C11D1/528—Carboxylic amides (R1-CO-NR2R3), where at least one of the chains R1, R2 or R3 is interrupted by a functional group, e.g. a -NH-, -NR-, -CO-, or -CON- group
    • 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
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/22—Carbohydrates or derivatives thereof
    • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • 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
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones

Definitions

  • This invention relates to granules containing a silicone-based antifoam and to a process for manufacturing them, as well as to a detergent powder containing the granules.
  • Granules containing a silicone-based antifoam are known. Certain granules of this type are described in British patent No. 1492939 and others in French patent No. 2 462 184.
  • Foam regulators can also be formed as described in FR-A-2 194 771 by melting silicone together with a water-soluble or water-dispersible meltable vehicle.
  • Carbowax polyethylene glycol
  • Water-insoluble waxes are not suggested in this role.
  • European patent application No. 0 071 481 also relates to granules containing a silicone-based antifoam.
  • the process which is described in the specification of that application involves granulating gelatinised starch whilst spraying on a mixture of a silicone oil and a hydrophobic silica. Asolution of paraffin wax in chloroform is then sprayed onto the granules and the solvent is evaporated.
  • the present invention provides a process for the manufacture of granules containing from 5 to 40% by weight of a silicone antifoam, from 5 to 30% of a water-insoluble paraffin or petroleum wax having a melting point within the range of from 35 to 70°C, from 20 to 80% by weight of a granular absorbent and optionally up to 10% by weight of a nonionic surfactant, the process being characterised by the steps of:
  • the silicone comprises a mixture of a liquid or liquifiable polysiloxane with particles of a hydrophobic material
  • the hydrophobic material is preferably a hydrophobed silica, a water-insoluble salt of an alkyl phosphoric acid, or a compound of one of the following general formulae: or where R 1 and R 3 represent aliphatic hydrocarbon residues containing 14-22 carbon atoms, R 2 and R 4 represent hydrogen atoms or aliphatic hydrocarbon residues containing 1-22 carbon atoms, and R represents an aliphatic residue containing 1-9 carbon atoms.
  • alkylene-bis-amides and in particular ethylene and methylene-bis-stearimide are the preferred compounds, that is to say compounds of the general formula: where x is an integer from 5 to 25 and n is 1 or 2 and in particular compounds of the formula.
  • Waxes of mineral origin include microcrystalline and oxidised microcrystalline petroleum waxes. Whatever wax is used, its melting point is between 35° and 70°C so that it is readily liquifiable.
  • the apparatus in which the liquifiable mixture of silicone and wax is sprayed onto the absorbent can be any of the apparatus conventionally used for granulation or agglomeration. Examples are the Eirich (registered Trade Mark) pan, the Schugi (registered Trade Mark) mixer, or any one of the numerous fluidised bed apparatus which are available, such as the Anhydro (registered Trade Mark) fluidised bed.
  • a typical composition of the granules formed in the process of the invention is:
  • the absorbent is present in amounts of from 20-80%, the silicone compound in amounts of from 5-40%, the paraffin wax in amounts of from 5-30% and the nonionic surfactant in amounts up to 10%, the percentages being expressed by weight.
  • the granules may be incorporated into spray-dried (powdered) detergent compositions or into liquid ones.
  • powdered detergent compositions they will be dosed into the powder after spray-drying, along with other materials which are conventionally post-dosed such as sodium perborate and fillers.
  • liquids which are structured sometimes called false-body liquids
  • the granules can be added to the liquid in the final step of the manufacturing process.
  • structured liquids There are two basic types of structured liquids, one in which the structure is imparted by interaction between surfactants and electrolytes, and the other in which it is imparted by means of a colloid such as a clay. Both types are capable of suspending the granules of the invention.
  • composition in powdered or in liquid form it will normally contain both an anionic and a nonionic surfactant but may also contain either alone or a soap as the major detergent-active species.
  • the powdered compositions will contain a detergency builder and the liquid ones will normally do so, but need not necessarily.
  • Other components which will normally be present are corrosion inhibitors, anti-redeposition agents, fluorescers, stabilisers and substantial proportions of water.
  • Typical anionic surfactants which may be present in amounts of from about 2 to 35% by weight of the finished compositions are sodium alkylbenzene sulphonates, preferably the C 10 -C l4 alkyl compounds, sodium primary and secondary alkyl sulphates, preferably the C 10 -C 22 alkyl sulphates, sodium olefine sulphonates, preferably the C 10 -C 18 sulphonates and sodium alkane sulphonates.
  • Soaps of fatty acids may also be present, preferably the sodium and potassium salts of C, O -C 22 fatty acids, both saturated and unsaturated.
  • soap is the sole anionic surfactant it may be present in an amount up to about 65% by weight of the finished composition, down to about 1 / 2 % by weight when other anionic surfactants are present.
  • Typical soaps which can be used are those formed from coconut oil, tallow and natural oils containing high proportions of oleic acid such as sunflower oil.
  • Typical nonionic surfactants are ethoxylated pri mary and secondary alcohols offrom 8 to 25 carbon atoms containing from 3 to 25 moles of ethylene oxide per mole of alcohol. These materials may generally be present in an amount of from 1 to 15% by weight, based on the weight of the finished composition.
  • Typical detergency builders which can be used are the water-soluble phosphates, carbonates, percarbonates and aluminosilicates, particularly the sodium and potassium salts of these compounds.
  • Organic builders may also be used, examples being sodium carboxymethyloxysuccinate, sodium citrate, sodium polyacrylates and sodium nitrilotriacetate. Any of these compounds, or any other builder compound, in any suitable mixture, may be used in amounts of from 5 to 50% by weight of the finished composition.
  • gelatinised starch (Amigel 30076 registered Trade Mark, manufactured and sold by Societe des Produits du Mais, of Clarmart, France) was placed in the pan of an Eirich (registered Trade Mark) pan granulator.
  • the resultant liquid was then sprayed onto the gelatinised starch in the pan granulator then, 4.8 parts of nonionic surfactant (C 13 - 18 primary alcohol 8EO) where sprayed onto the granules.
  • the following detergent composition was prepared by conventional spray-drying and dry-dosing techniques, the granules of Example 1 being added in the dry-dosing step.
  • the powder obtained was divided into two batches. The first batch was immediately subjected to the foam assessment test described below. The other batch was stored in unlaminated, sealed cartons at 37°C and 60% relative humidity. The stored batches were then subjected to test after 2 weeks and 4 weeks of storage.
  • the suds assessment test is performed by washing a standard load of clean washing in a Brandt 433 (registered Trade Mark) washing machine.
  • the washing machine was specially modified to provide a window and the window had an arbitrary scale on it from which suds height could be read.
  • the reservoir holding the wash liquor is fitted with a thermometer.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (4)

1. Verfahren zur Herstellung von Granulaten, die ein Antischaummittel auf Silikonbasis in einer Menge von 5 bis 40 Gew.-%, ein wasserunlösliches Paraffin- oder Erdölwachs mit einem Schmelzpunkt im Bereich von 35 bis 70°C in einer Menge von 5 bis 30 Gew.-%, ein granuliertes Absorbens in einer Menge von 20 bis 80 Gew.-% und fakultativ eine nichtionische, oberflächenaktive Substanz in einer Menge bis zu 10 Gew.-% enthalten, wobei das Verfahren durch folgende Schritte gekennzeichnet ist:
(a) Bilden einer verflüssigten Mischung des Antischaummittels auf Silikonbasis, des Paraffin- oder Erdölwachses und derfakultativen, nichtionischen, oberflächenaktiven Substanz, wobei die Mischung frei von organischem Solvens ist,
(b) Aufsprühen der solvensfreien, verflüssigten Mischung auf eine in Bewegung gehaltene Aufschüttung des granulierten Absorbens,
wobei das granulierte Absorbens gelatinisierte Stärke ist.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daßdas Silikon eine Mischung eines flüssigen oder verflüssigbaren Polysiloxans mit Partikeln einer hydrophoben Substanz enthält.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die hydrophobe Substanz eine hydrophobierte Silica, ein wasserunlösliches Salz einer Alkylphosphorsäure oder eine Verbindung mit der allgemeinen Formel umfaßt:
Figure imgb0015
Figure imgb0016
Figure imgb0017
oder
Figure imgb0018
worin R1 und R3 für aliphatische Kohlenwasserstoffreste mit 14-22 Kohlenstoffatomen steht, R2 und R4 für Wasserstoffatome oder aliphatische Kohlenwasserstoffreste mit 1-22 Kohlenstoffatomen steht und R für einen aliphatischen Rest mit 1-9 Kohlenstoffatomen steht.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß die hydrophobe Substanz eine Verbindung mit der allgemeinen Formel
Figure imgb0019
umfaßt, worin x eine ganze Zahl von 5 bis 25 ist und n 1 oder 2 ist.
EP83302643A 1982-05-11 1983-05-10 Verfahren zur Herstellung von Antischaummittel auf Silikonbasis enthaltenden Granulaten Expired - Lifetime EP0094250B2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83302643T ATE21115T1 (de) 1982-05-11 1983-05-10 Granulate enthaltend antischaummittel auf silikonbasis und verfahren zu ihrer herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB8213576 1982-05-11
GB8213576 1982-05-11

Publications (3)

Publication Number Publication Date
EP0094250A1 EP0094250A1 (de) 1983-11-16
EP0094250B1 EP0094250B1 (de) 1986-07-30
EP0094250B2 true EP0094250B2 (de) 1994-06-15

Family

ID=10530279

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83302643A Expired - Lifetime EP0094250B2 (de) 1982-05-11 1983-05-10 Verfahren zur Herstellung von Antischaummittel auf Silikonbasis enthaltenden Granulaten

Country Status (4)

Country Link
EP (1) EP0094250B2 (de)
AT (1) ATE21115T1 (de)
DE (1) DE3364903D1 (de)
ZA (1) ZA833292B (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7316995B2 (en) 2003-02-10 2008-01-08 Henkel Kommanditgesellschaft Auf Aktien Detergents or cleaning agents comprising a water-soluble building block system and a cellulose derivative with dirt dissolving properties
US7375072B2 (en) 2003-02-10 2008-05-20 Henkel Kommanditgesellschaft Auf Aktien Bleach-containing laundry detergents or cleaning compositions comprising water-soluble builder system and soil release-capable cellulose derivative

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4652392A (en) * 1985-07-30 1987-03-24 The Procter & Gamble Company Controlled sudsing detergent compositions
GB8521956D0 (en) * 1985-09-04 1985-10-09 Unilever Plc Antifoam ingredient
GB8627181D0 (en) * 1986-11-13 1986-12-10 Procter & Gamble Softening detergent compositions
DE3732947A1 (de) * 1987-09-30 1989-04-13 Henkel Kgaa Zur verwendung in wasch- und reinigungsmitteln geeignetes schaumregulierungsmittel
EP0705324A1 (de) * 1993-07-12 1996-04-10 The Procter & Gamble Company Granulare waschmittelzusammensetzung enthaltend ein tensid und einen entschaeumungsinhibitor
GB9410677D0 (en) 1994-05-27 1994-07-13 Unilever Plc Detergent compositions
DE19636206A1 (de) * 1996-09-06 1998-03-12 Henkel Kgaa Verfahren zur Herstellung von paraffinhaltigen Schaumregulatoren
US6200498B1 (en) 1997-08-29 2001-03-13 Henkel Kommanditgesellschaft Auf Aktien Process for producing paraffin-containing foam regulators
DE19837195A1 (de) * 1998-08-17 2000-02-24 Cognis Deutschland Gmbh Herstellung von Entschäumergranulaten im Fließbettverfahren
DE19953796A1 (de) * 1999-11-09 2001-05-17 Cognis Deutschland Gmbh Feste Wasch-, Spül- und Reinigungsmittel
DE19953797A1 (de) * 1999-11-09 2001-05-17 Cognis Deutschland Gmbh Entschäumergranulate
DE19953794A1 (de) * 1999-11-09 2001-05-17 Cognis Deutschland Gmbh Formkörper mit verbesserter Wasserlöslichkeit
DE10108573A1 (de) * 2001-02-22 2002-09-12 Cognis Deutschland Gmbh Feste Waschmittelzusatzstoffe, deren Herstellung und Verwendung
US6656975B1 (en) 2002-05-21 2003-12-02 Dow Corning Corporation Silicone dispersions
WO2004069981A2 (en) * 2003-02-03 2004-08-19 Ciba Specialty Chemicals Holding Inc. Washing agent and fabric softener formulations
GB0518059D0 (en) 2005-09-06 2005-10-12 Dow Corning Delivery system for releasing active ingredients
EP2649172A1 (de) 2010-12-10 2013-10-16 Dow Corning Corporation Schaumregulierende zusammensetzung in granulatform

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1407997A (en) * 1972-08-01 1975-10-01 Procter & Gamble Controlled sudsing detergent compositions
GB1492939A (en) * 1974-03-11 1977-11-23 Procter & Gamble Ltd Controlled-sudsing detergent compositions
EP0008829A1 (de) * 1978-09-09 1980-03-19 THE PROCTER & GAMBLE COMPANY Reinigungsmittelzusammensetzungen mit geregeltem Schaumverhalten
FR2462184A1 (fr) * 1979-07-31 1981-02-13 Eurand France Nouvelles compositions antimousses sous forme de granules utilisables notamment dans les lessives en poudre
NZ199235A (en) * 1980-12-17 1985-02-28 Unilever Plc Controlled-sudsing detergent compositions
DE3271649D1 (en) * 1981-07-31 1986-07-17 Unilever Plc Suds control agents and detergent compositions containing them

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7316995B2 (en) 2003-02-10 2008-01-08 Henkel Kommanditgesellschaft Auf Aktien Detergents or cleaning agents comprising a water-soluble building block system and a cellulose derivative with dirt dissolving properties
US7375072B2 (en) 2003-02-10 2008-05-20 Henkel Kommanditgesellschaft Auf Aktien Bleach-containing laundry detergents or cleaning compositions comprising water-soluble builder system and soil release-capable cellulose derivative

Also Published As

Publication number Publication date
DE3364903D1 (en) 1986-09-04
ZA833292B (en) 1984-12-24
EP0094250B1 (de) 1986-07-30
EP0094250A1 (de) 1983-11-16
ATE21115T1 (de) 1986-08-15

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