EP0329842A2 - Powdery antifoaming agents for detergents - Google Patents

Powdery antifoaming agents for detergents Download PDF

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Publication number
EP0329842A2
EP0329842A2 EP88120606A EP88120606A EP0329842A2 EP 0329842 A2 EP0329842 A2 EP 0329842A2 EP 88120606 A EP88120606 A EP 88120606A EP 88120606 A EP88120606 A EP 88120606A EP 0329842 A2 EP0329842 A2 EP 0329842A2
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EP
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Prior art keywords
silicone oil
weight
defoamer
detergent
zeolite
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EP88120606A
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German (de)
French (fr)
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EP0329842A3 (en
Inventor
Marc Lambermont
Manfred Dr. Diehl
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Evonik Operations GmbH
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Degussa GmbH
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    • 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
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • the invention relates to a powder detergent defoamer, the process for its preparation and its use as a defoamer in detergents.
  • EP-OS 142 910 describes a detergent defoamer which consists of a mixture of polydimethylsiloxane with a viscosity of 20 to 12,500 cs and polydimethylsiloxane with a viscosity of at least 25,000 cs and hydrophobic silicon dioxide.
  • This defoamer can additionally contain a solid, water-soluble, inorganic carrier substance such as sodium tripolyphosphate or aluminum silicate. Before being used, the defoamer is dispersed in an organic carrier system which consists of a mixture of high-melting nonionic surfactants.
  • the known defoamer has the disadvantage that its shelf life is limited because the defoamer activity decreases with increasing storage time.
  • the invention relates to a powder detergent defoamer consisting of 65 to 99.9% by weight, preferably 85 to 96% by weight of a carrier and 0.1 to 35, preferably 5 to 15% by weight of a silica-containing silicone oil defoamer.
  • the powder detergent defoamer consists of 85-96% by weight of powdered type A zeolite as carrier 3 - 9% by weight of low viscosity silicone oil 1 - 5% by weight of highly viscous silicone oil 0.5-1.5% by weight of hydrophobic precipitated silica
  • the zeolite A in the form of a zeolite compound can be used as the carrier.
  • Zeolite compounds are known. They are commercially available as a builder component for detergents.
  • Another object of the invention is a process for the preparation of the powder detergent defoamer, which is characterized in that the low-viscosity silicone oil is mixed with vigorous stirring with the hydrophobic precipitated silica and then the highly viscous silicone oil is mixed in, the mixture thus obtained with the powdered zeolite of the type A is converted into the powder form in a mixing device.
  • a powdery zeolite of type A with a particularly defined particle spectrum is used.
  • Such zeolite powder can according to DE-AS 24 47 021, DE-AS 25 17 218, DE-OS 26 52 419, DE-OS 26 51 420, DE-OS 26 51 436, DE-OS 26 51 437, DE-OS 26 51 445, DE-OS 26 51 485 are produced. They then have the particle distribution curves given there.
  • a powdery zeolite of type A can be used, which has the particle size distribution described in DE-PS 26 51 485.
  • the silicone oil is an organopolysiloxane liquid of the general formula wherein each R may be the same or different radicals which are selected from optionally substituted monovalent hydrocarbon radicals, such as aliphatic, halogenaliphatic and cyclo-aliphatic radicals, e.g. B. alkyl, alkenyl, Cycloalkyl, haloalkyl, such as methyl, ethyl, propyl, chloroethyl, trifluoropropyl, phenyl, tolyl, benzyl or OH or halogen, where a is a number sufficient to achieve the viscosity mentioned above. Dimethylpolysiloxanes are preferably used.
  • Sipernat® D10 can be used as the hydrophobic precipitated silica.
  • Sipernat® D10 is a precipitated silica that has been made hydrophobic by post-treatment with a silicone oil. Such an aftertreatment method is used e.g. B. described in DE-OS 26 28 975.
  • Sipernat D 10 is a commercially available precipitated silica that has the following physico-chemical characteristics: Sipernat® D 10 Surface according to BET 1) m2 / g 90 Average size of the primary particles nm 18th Tamped density 2) g / l 100 pH 3) 10.3 8) Sieve residue (according to Mocker 45 ⁇ m) 4)% 0.01 Loss on drying (2 h, 105 ° C) 5)% 3rd Loss on ignition (2 h, 1000 ° C) 5) 6)% 7 9) SiO2 7)% 98 Na2O 7)% 0.8 Fe2O3 7)% 0.03 SO3 7)% 0.8 1) according to DIN 66 131 2) according to DIN 53 194 (not screened), ISO 787 / XI or JIS K 5101/18 3) according to DIN 53 200 (in 5% aqueous dispersion) ISO 787 / IX, ASTM D 1208 or JIS K 5101/24 4) according to DIN 53 580
  • B. spray mixing units such. B. free fall mixer or ploughshare mixer, such as. B. Lödige mixer use.
  • the powder detergent defoamer according to the invention has the advantage that it has excellent storage stability in detergents and good flow properties.
  • Wessalith® P is a powdery zeolite A according to DE-PS 26 51 485.
  • CMC is carboxymethyl cellulose.
  • Wessalith® CS, Wessalith® CN and Wessalith® CD are Zeolite granules (compounds) that can be processed with other ingredients to form detergent mixtures.
  • the composition of the individual zeolite granules is listed in Table 1.
  • the examples show the test of the defoaming behavior of the defoamer according to the invention on the basis of Sipernat® D 10, Silicone oil mixture of two silicone oils with a viscosity of 1,000 and 60,000 cst and different carriers.
  • the silicone oils are designated with DC 200/1000 cst or DC 200/60000 cst.
  • Phosphate, sulfate, starch, CMC, soda and WESSALITH® P, -CS, -CN and -CD are used as carriers.
  • the defoaming behavior was tested after storage for 2, 4 and 8 weeks under critical conditions (35 ° C and 70% relative air humidity).
  • Figures 1 to 9 show the defoaming behavior of the respective foam inhibitor concentrates. - after production (defoamer picture top left) - after two weeks of storage in detergent (defoamer picture top right) - after four weeks of storage in detergent (defoamer picture bottom left) - after eight weeks of storage in detergent (defoamer picture bottom right)
  • the silicone oil Dow Corning® Fluid DC 200 Fluid with a viscosity at 25 ° C of 1,000 cst was used as the low-viscosity silicone oil.
  • the silicone oil Dow Corning Fluid DC 200 Fluid with a viscosity of 60,000 cst at 25 ° C was used as the highly viscous silicone oil.
  • SIPERNAT® D 10 is added to the low-viscosity silicone oil with intensive stirring (Ultra-Turrax, dispersion time 5 min at 11,000 U). Then the respective amount of highly viscous silicone oil is added.
  • a detergent of the following composition is used as the detergent: Bandwidth in particular Nonionic surfactants 2 - 5 4th Anionic surfactants 7-10 9 polymer 2 - 5 4th Zeolite A 20-30 29 Sodium silicate 4 - 9 7.5 Sodium carbonate 6-10 8.5 CMC 1 - 2.5 2nd Sodium sulfate 15-25 21st water 7-17 15 %

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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)

Abstract

The agent consists of 65 to 99.9% by weight, preferably 85 to 96% by weight, of a carrier and 0.1 to 35, preferably 5 to 15, % by weight of a silica-containing silicone oil antifoam agent. The antifoaming agent for detergents preferably has the following composition: 85 - 96% by weight of powdered zeolite of type A as carrier 3 - 9% by weight of low-viscosity silicone oil 1 - 5% by weight of high-viscosity silicone oil 0.5 - 1.5% by weight of hydrophobic precipitated silica <IMAGE>

Description

Die Erfindung betrifft einen pulverförmigen Waschmittelentschäumer, das Verfahren zu seiner Herstellung sowie seine Anwendung als Entschäumer in Waschmitteln.The invention relates to a powder detergent defoamer, the process for its preparation and its use as a defoamer in detergents.

Waschmittelentschäumer auf der Basis von Siliconöl sind bekannt. So wird in der EP-OS 142 910 ein Waschmittelentschäumer, der aus einem Gemisch von Polydimethylsiloxan mit einer Viskosität von 20 bis 12.500 cs und Polydimethylsiloxan mit einer Viskosität von mindestens 25.000 cs sowie hydrophoben Siliciumdioxid besteht, beschrieben. Dieser Entschäumer kann zusätzlich eine feste, wasserlösliche, anorganische Trägersubstanz wie Natriumtripolyphosphat oder Aluminiumsilikat enthalten. Vor seiner Anwendung wird der Entschäumer in einem organischen Trägersystem, welches aus einem Gemisch hochschmelzender nichtionischer Tenside besteht, dispergiert.Detergent defoamers based on silicone oil are known. For example, EP-OS 142 910 describes a detergent defoamer which consists of a mixture of polydimethylsiloxane with a viscosity of 20 to 12,500 cs and polydimethylsiloxane with a viscosity of at least 25,000 cs and hydrophobic silicon dioxide. This defoamer can additionally contain a solid, water-soluble, inorganic carrier substance such as sodium tripolyphosphate or aluminum silicate. Before being used, the defoamer is dispersed in an organic carrier system which consists of a mixture of high-melting nonionic surfactants.

Der bekannte Entschäumer hat den Nachteil, daß seine Lagerfähigkeit begrenzt ist, weil mit zunehmender Lagerzeit die Entschäumeraktivität nachläßt.The known defoamer has the disadvantage that its shelf life is limited because the defoamer activity decreases with increasing storage time.

Gegenstand der Erfindung ist ein pulverförmiger Waschmittelentschäumer, bestehend aus 65 bis 99,9 Gew.-%, vorzugsweise 85 bis 96 Gew.-% eines Trägers und 0,1 bis 35, vorzugsweise 5 bis 15 Gew.-% eines kieselsäurehaltigen Siliconölentschäumers.The invention relates to a powder detergent defoamer consisting of 65 to 99.9% by weight, preferably 85 to 96% by weight of a carrier and 0.1 to 35, preferably 5 to 15% by weight of a silica-containing silicone oil defoamer.

In einer bevorzugten Ausführungsform der Erfindung besteht der pulverförmige Waschmittelentschäumer aus
85 - 96 Gew.-% pulverförmigem Zeolith des Typs A als Träger
3 - 9 Gew.-% niedrigviskosem Siliconöl
1 - 5 Gew.-% hochviskosem Siliconöl
0,5 - 1,5 Gew.-% hydrophober FällungskieselsäureIn a preferred embodiment of the invention, the powder detergent defoamer consists of
85-96% by weight of powdered type A zeolite as carrier
3 - 9% by weight of low viscosity silicone oil
1 - 5% by weight of highly viscous silicone oil
0.5-1.5% by weight of hydrophobic precipitated silica

Als Träger kann in einer weiteren Ausführungsform der Erfindung der Zeolith A in Form eines Zeolith-Compounds eingesetzt werden.In a further embodiment of the invention, the zeolite A in the form of a zeolite compound can be used as the carrier.

Zeolith-Compounds sind bekannt. Sie werden als Builderbestandteil für Waschmittel im Handel angeboten.Zeolite compounds are known. They are commercially available as a builder component for detergents.

Ein weiterer Gegenstand der Erfindung ist ein Verfahren zur Herstellung des pulverförmigen Waschmittelentschäumers, welches dadurch gekennzeichnet ist, daß man das niedrig viskose Siliconöl unter intensivem Rühren mit der hydrophoben Fällungskieselsäure vermischt und anschließend das hochviskose Silikonöl hinzumischt, die so erhaltene Mischung mit dem pulverförmigen Zeolith des Typs A in einer Mischvorrichtung in die Pulverform überführt.Another object of the invention is a process for the preparation of the powder detergent defoamer, which is characterized in that the low-viscosity silicone oil is mixed with vigorous stirring with the hydrophobic precipitated silica and then the highly viscous silicone oil is mixed in, the mixture thus obtained with the powdered zeolite of the type A is converted into the powder form in a mixing device.

In einer bevorzugten Ausführungsform der Erfindung wird ein pulverförmiger Zeolith des Typs A mit besonders definiertem Teilchenspektrum eingesetzt.In a preferred embodiment of the invention, a powdery zeolite of type A with a particularly defined particle spectrum is used.

Derartige Zeolithpulver können gemäß DE-AS 24 47 021, DE-AS 25 17 218, DE-OS 26 52 419, DE-OS 26 51 420, DE-OS 26 51 436, DE-OS 26 51 437, DE-OS 26 51 445, DE-OS 26 51 485 hergestellt werden. Sie weisen dann die dort angegebenen Teilchenverteilungskurven auf.Such zeolite powder can according to DE-AS 24 47 021, DE-AS 25 17 218, DE-OS 26 52 419, DE-OS 26 51 420, DE-OS 26 51 436, DE-OS 26 51 437, DE-OS 26 51 445, DE-OS 26 51 485 are produced. They then have the particle distribution curves given there.

In einer besonders bevorzugten Ausführungsform kann ein pulverförmiger Zeolith des Typs A verwendet werden, die die in der DE-PS 26 51 485 beschriebene Teilchengrößenverteilung aufweist.In a particularly preferred embodiment, a powdery zeolite of type A can be used, which has the particle size distribution described in DE-PS 26 51 485.

In einer bevorzugten Ausführungsform der Erfindung kann das niedrigviskose Siliconöl (= Polydimethylsiloxan) mit einer Viskosität von 100 bis 5000 cst bei 25 °C, vorzugsweise 500 bis 2000, insbesondere von 1000 cst bei 25 °C, und das hochviskose Siliconöl (= Polydimethylsiloxan) mit einer Viskosität von 30.000 bis 100.000 cst bei 25 °C, vorzugsweise 60.000 cst bei 25 °C eingesetzt werden.In a preferred embodiment of the invention, the low-viscosity silicone oil (= polydimethylsiloxane) with a viscosity of 100 to 5000 cst at 25 ° C, preferably 500 to 2000, in particular 1000 cst at 25 ° C, and the highly viscous silicone oil (= polydimethylsiloxane) a viscosity of 30,000 to 100,000 cst at 25 ° C, preferably 60,000 cst at 25 ° C can be used.

Das Siliconöl ist eine Organopolysiloxanflüssigkeit der allgemeinen Formel

Figure imgb0001
worin für R jeweils gleiche oder verschiedene Reste stehen können, die ausgewählt sind aus gegebenenfalls substituierten einwertigen Kohlenwasserstoffresten, wie aliphatischen, halogenaliphatischen und cyclo-aliphatischen Resten, z. B. Alkyl, Alkenyl, Cycloalkyl, Halogenalkyl, wie Methyl, Ethyl, Propyl, Chlorethyl, Trifluorpropyl, Phenyl, Tolyl, Benzyl oder aber OH oder Halogen, wobei a für eine Zahl steht, die ausreicht, die oben erwähnte Viskosität zu erreichen. Bevorzugt werden Dimethylpolysiloxane eingesetzt.The silicone oil is an organopolysiloxane liquid of the general formula
Figure imgb0001
 wherein each R may be the same or different radicals which are selected from optionally substituted monovalent hydrocarbon radicals, such as aliphatic, halogenaliphatic and cyclo-aliphatic radicals, e.g. B. alkyl, alkenyl, Cycloalkyl, haloalkyl, such as methyl, ethyl, propyl, chloroethyl, trifluoropropyl, phenyl, tolyl, benzyl or OH or halogen, where a is a number sufficient to achieve the viscosity mentioned above. Dimethylpolysiloxanes are preferably used.

Als hydrophobe Fällungskieselsäure kann man das Handelsprodukt Sipernat® D10 einsetzen. Sipernat® D10 ist eine Fällungskieselsäure, die durch Nachbehandlung mit einem Siliconöl hydrophobiert wurde. Ein derartiges Nachbehandlungsverfahren wird z. B. in der DE-OS 26 28 975 beschrieben.The commercial product Sipernat® D10 can be used as the hydrophobic precipitated silica. Sipernat® D10 is a precipitated silica that has been made hydrophobic by post-treatment with a silicone oil. Such an aftertreatment method is used e.g. B. described in DE-OS 26 28 975.

Sipernat D 10 ist eine im Handel erhältliche Fällungskieselsäure, die die folgenden physikalisch­chemischen Kenndaten aufweist: Sipernat® D 10 Oberfläche nach BET 1) m²/g 90 Mittlere Größe der Primärteilchen nm 18 Stampfdichte 2) g/l 100 pH-Wert 3) 10,3 8) Siebrückstand (nach Mocker 45 µm) 4) % 0,01 Trocknungsverlust (2 h, 105 °C) 5) % 3 Glühverlust (2 h, 1000 °C)5) 6) % 7 9) SiO₂ 7) % 98 Na₂O 7) % 0,8 Fe₂O₃ 7) % 0,03 SO₃ 7) % 0,8 1) nach DIN 66 131 2) nach DIN 53 194 (nicht gesiebt), ISO 787/XI oder JIS K 5101/18 3) nach DIN 53 200 (in 5 %iger wäßriger Dispersion) ISO 787/IX, ASTM D 1208 oder JIS K 5101/24 4) nach DIN 53 580, ISO 787/XVIII oder JIS K 5101/20 5) nach DIN 55 921, ASTM D 1208 oder JIS K 5101/23 6) bezogen auf die 2 Stunden bei 105 °C getrocknete Substanz 7) bezogen auf die 2 Stunden bei 1000 °C geglühte Substanz 8) in Wasser : Methanol = 1 : 1 9) enthält ca. 3 % chemisch gebundenen Kohlenstoff 10) enthält ca. 2 % chemisch gebundenen Kohlenstoff Sipernat D 10 is a commercially available precipitated silica that has the following physico-chemical characteristics: Sipernat® D 10 Surface according to BET 1) m² / g 90 Average size of the primary particles nm 18th Tamped density 2) g / l 100 pH 3) 10.3 8) Sieve residue (according to Mocker 45 µm) 4)% 0.01 Loss on drying (2 h, 105 ° C) 5)% 3rd Loss on ignition (2 h, 1000 ° C) 5) 6)% 7 9) SiO₂ 7)% 98 Na₂O 7)% 0.8 Fe₂O₃ 7)% 0.03 SO₃ 7)% 0.8 1) according to DIN 66 131 2) according to DIN 53 194 (not screened), ISO 787 / XI or JIS K 5101/18 3) according to DIN 53 200 (in 5% aqueous dispersion) ISO 787 / IX, ASTM D 1208 or JIS K 5101/24 4) according to DIN 53 580, ISO 787 / XVIII or JIS K 5101/20 5) according to DIN 55 921, ASTM D 1208 or JIS K 5101/23 6) based on the substance dried at 105 ° C. for 2 hours 7) based on the substance annealed at 1000 ° C for 2 hours 8) in water: methanol = 1: 1 9) contains approx. 3% chemically bound carbon 10) contains approx. 2% chemically bound carbon

Als Mischvorrichtung kann man z. B. Sprühmischaggregate, wie z. B. Freifallmischer oder Pflugscharmischer, wie z. B. Lödige-Mischer, verwenden.As a mixing device you can e.g. B. spray mixing units such. B. free fall mixer or ploughshare mixer, such as. B. Lödige mixer use.

Der erfindungsgemäße pulverförmige Waschmittelentschäumer hat den Vorteil, daß er eine ausgezeichnete Lagerstabilität in Waschmitteln und eine gute Rieselfähigkeit aufweist.The powder detergent defoamer according to the invention has the advantage that it has excellent storage stability in detergents and good flow properties.

BeispieleExamples

Das in den Beispielen verwendete
Wessalith® P ist ein pulverförmiger Zeolith A gemäß DE-PS 26 51 485.
CMC ist Carboxymethylcellulose.
Wessalith® CS, Wessalith® CN und Wessalith® CD sind Zeolithgranulate (Compounds), die mit weiteren Bestandteilen zu Waschmittelmischungen verarbeitet werden können. Die Zusammensetzung der einzelnen Zeolithgranulate ist in der Tabelle 1 aufgeführt.

Figure imgb0002
Figure imgb0003
 The one used in the examples
Wessalith® P is a powdery zeolite A according to DE-PS 26 51 485.
CMC is carboxymethyl cellulose.
Wessalith® CS, Wessalith® CN and Wessalith® CD are Zeolite granules (compounds) that can be processed with other ingredients to form detergent mixtures. The composition of the individual zeolite granules is listed in Table 1.
Figure imgb0002
Figure imgb0003

Die Beispiele zeigen die Prüfung des Entschäumungsverhaltens des erfindungsgemäßen Entschäumers auf Basis von
Sipernat® D 10,
Siliconölgemisch zweier Siliconöle mit einer Viskosität von 1.000 und 60.000 cst und verschiedener Träger.The examples show the test of the defoaming behavior of the defoamer according to the invention on the basis of
Sipernat® D 10,
Silicone oil mixture of two silicone oils with a viscosity of 1,000 and 60,000 cst and different carriers.

Die Siliconöle werden mit DC 200/1000 cst bzw. DC 200 /60000 cst bezeichnet.The silicone oils are designated with DC 200/1000 cst or DC 200/60000 cst.

Als Träger werden Phosphat, Sulfat, Stärke, CMC, Soda, sowie WESSALITH® P, -CS, -CN und -CD verwendet. Das Entschäumungsverhalten wurde nach einer Lagerung von 2, 4 und 8 Wochen unter kritischen Bedingungen (35 °C und 70 % relative Luftfeuchte) geprüft.Phosphate, sulfate, starch, CMC, soda and WESSALITH® P, -CS, -CN and -CD are used as carriers. The defoaming behavior was tested after storage for 2, 4 and 8 weeks under critical conditions (35 ° C and 70% relative air humidity).

ErgebnisseResults

Die Figuren 1 bis 9 zeigen das Entschäumungsverhalten der jeweiligen Schauminhibitorkonzentrate.
- nach Herstellung (Entschäumerbild links oben)
- nach zweiwöchiger Lagerung in Waschmittel (Entschäumerbild rechts oben)
- nach vierwöchiger Lagerung in Waschmittel (Entschäumerbild links unten)
- nach achtwöchiger Lagerung in Waschmittel (Entschäumerbild rechts unten)Figures 1 to 9 show the defoaming behavior of the respective foam inhibitor concentrates.
- after production (defoamer picture top left)
- after two weeks of storage in detergent (defoamer picture top right)
- after four weeks of storage in detergent (defoamer picture bottom left)
- after eight weeks of storage in detergent (defoamer picture bottom right)

Es wird festgestellt, daß die Art des Trägermaterials einen Einfluß auf das Entschäumungsverhalten des im Waschmittel gelagerten Schauminhibitorkonzentrates hat. Auffällig ist hier die absolut hohe Lagerstabilität der Schauminhibitorkonzentrate auf Basis von WESSALITH® (Zeolith A) im Waschmittel.It is found that the type of carrier material has an influence on the defoaming behavior of the foam inhibitor concentrate stored in the detergent. What is striking here is the absolutely high storage stability of the foam inhibitor concentrates based on WESSALITH® (Zeolite A) in the detergent.

Versuchsdurchführung:Carrying out the experiment:

Als niedrigviskoses Siliconöl wurde das Siliconöl Dow Corning® Fluid DC 200 Fluid mit einer Viskosität bei 25 °C von 1.000 cst verwendet. Als hochviskoses Siliconöl wurde das Siliconöl Dow Corning Fluid DC 200 Fluid mit einer Viskosität von 60.000 cst bei 25 °C verwendet.The silicone oil Dow Corning® Fluid DC 200 Fluid with a viscosity at 25 ° C of 1,000 cst was used as the low-viscosity silicone oil. The silicone oil Dow Corning Fluid DC 200 Fluid with a viscosity of 60,000 cst at 25 ° C was used as the highly viscous silicone oil.

Das niedrigviskose Siliconöl wird unter intensivem Rühren (Ultra-Turrax, Dispergierzeit 5 min bei 11.000 U) mit SIPERNAT® D 10 versetzt. Anschließend wird die jeweilige Menge an hochviskosem Siliconöl zugegeben.SIPERNAT® D 10 is added to the low-viscosity silicone oil with intensive stirring (Ultra-Turrax, dispersion time 5 min at 11,000 U). Then the respective amount of highly viscous silicone oil is added.

Die anwendungstechnische Prüfung dieser Schauminhibitorkonzentrate wurde mit einer mit Schaummeßelektronik ausgerüsteten Waschmaschine mit horizontal gelagerter Trommel (Miele W 433) zwischen 30 und 90 °C (Hauptwaschprogramm) durchgeführt. Als Wäschegewebe wurden ca. 3 kg saubere Wäsche der Qualität Baumwolle, weiß, DIN 53919 der Firma EMPA, Schweiz verwendet.The application test of these foam inhibitor concentrates was carried out with a washing machine equipped with foam measuring electronics with a horizontally mounted drum (Miele W 433) between 30 and 90 ° C (main wash program). As Linen fabrics were used about 3 kg of clean laundry of the quality cotton, white, DIN 53919 from EMPA, Switzerland.

Als Waschmittel wird ein Waschmittel der folgenden Zusammensetzung verwendet: Bandbreite insbesondere Nichtionische Tenside 2 - 5 4 Anionische Tenside 7 - 10 9 Polymer 2 - 5 4 Zeolith A 20 - 30 29 Natriumsilikat 4 - 9 7,5 Natriumkarbonat 6 - 10 8,5 CMC 1 - 2,5 2 Natriumsulfat 15 - 25 21 Wasser 7 - 17 15 % A detergent of the following composition is used as the detergent: Bandwidth in particular Nonionic surfactants 2 - 5 4th Anionic surfactants 7-10 9 polymer 2 - 5 4th Zeolite A 20-30 29 Sodium silicate 4 - 9 7.5 Sodium carbonate 6-10 8.5 CMC 1 - 2.5 2nd Sodium sulfate 15-25 21st water 7-17 15 %

3,75 g des Schauminhibitorkonzentrates wird mit dem Waschmittel vermischt und vor und nach Lagerung auf Entschäumerverhalten in der Waschmaschine geprüft. Der Lagertest wurde bei 35 °C und bei einer relativen Luftfeuchte von ca. 70 % durchgeführt. Die Dauer der Lagerung betrug in unserem Versuch jeweils 2, 4 und 8 Wochen.3.75 g of the foam inhibitor concentrate is mixed with the detergent and checked for defoamer behavior in the washing machine before and after storage. The storage test was carried out at 35 ° C and a relative humidity of approx. 70%. The duration of storage in our experiment was 2, 4 and 8 weeks.

Die Schaumhöhe in Abhängigkeit von der Temperatur wird mittels einem Druckschreiber registiert. Die Erläuterung der beigefügten Kurven gemäß Figuren 1 bis 9 ist aus der Figur 10 zu entnehmen.The foam height depending on the temperature is registered using a pressure recorder. The explanation of the attached curves according to FIGS. 1 to 9 can be found in FIG. 10.

Die Druckschreiber-Ergebnisse zeigen, daß das Anschäumen bei niedriger und hoher Temperatur durch die Entschäumerkomposition auf Basis von WESSALITH®, insbesondere nach Lagerung unter den vorher genannten kritischen Bedingungen, unterdrückt wird.The results of the pressure recorders show that foaming at low and high temperatures is suppressed by the defoamer composition based on WESSALITH®, especially after storage under the critical conditions mentioned above.

Claims (4)

1. Pulverförmiger Waschmittelentschäumer, bestehend aus 65 bis 99,9 Gew.-%, vorzugsweise 85 bis 96 Gew.-% eines Trägers und 0,1 bis 35, vorzugsweise 5 bis 15 Gew.-% eines kieselsäurehaltigen Siliconölentschäumers.1. Powder detergent defoamer, consisting of 65 to 99.9 wt .-%, preferably 85 to 96 wt .-% of a carrier and 0.1 to 35, preferably 5 to 15 wt .-% of a siliceous silicone oil defoamer. 2. Pulverförmiger Waschmittelentschäumer gemäß Anspruch 1, bestehend aus
85 - 96 Gew.-% pulverförmigem Zeolith des Typs A als Träger
3 - 9 Gew.-% niedrigviskosem Siliconöl
1 - 5 Gew.-% hochviskosem Siliconöl
0,5 - 1,5 Gew.-% hydrophober Fällungskieselsäure2. Powdered detergent defoamer according to claim 1, consisting of
85-96% by weight of powdered type A zeolite as carrier
3 - 9% by weight of low viscosity silicone oil
1 - 5% by weight of highly viscous silicone oil
0.5-1.5% by weight of hydrophobic precipitated silica 3. Verfahren zur Herstellung des pulverförmigen Waschmittelentschäumers gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, daß man das niedrigviskose Siliconöl unter intensivem Rühren mit der hydrophoben Fällungskieselsäure vermischt und anschließend das höherviskose Siliconöl hinzumischt, die so erhaltene Mischung mit dem pulverförmigen Zeolith des Typs A in einer Mischvorrichtung in die Pulverform überführt.3. A process for the preparation of the powder detergent defoamer according to claim 1 or 2, characterized in that the low-viscosity silicone oil is mixed with vigorous stirring with the hydrophobic precipitated silica and then admixed with the higher-viscosity silicone oil, the mixture thus obtained with the powdered zeolite of type A in one Mixing device converted into the powder form. 4. Verwendung des pulverförmigen Waschmittelentschäumers gemäß Anspruch 1 als Entschäumer in Waschmitteln.4. Use of the powder detergent defoamer according to claim 1 as a defoamer in detergents.
EP88120606A 1988-02-24 1988-12-09 Powdery antifoaming agents for detergents Withdrawn EP0329842A3 (en)

Applications Claiming Priority (2)

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DE3805624 1988-02-24
DE19883805624 DE3805624A1 (en) 1988-02-24 1988-02-24 POWDERED DETERGENT DEFOAMER

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0427577A1 (en) * 1989-10-09 1991-05-15 Rhone-Poulenc Chimie Aqueous zeolite suspension comprising of a silicon resin
EP0517298A1 (en) * 1991-06-03 1992-12-09 The Procter & Gamble Company Foam control agents in granular form
EP0618290A1 (en) * 1993-03-30 1994-10-05 The Procter & Gamble Company Flow aids for detergent powders comprising sodium aluminosilicate and hydrophobic silica
EP0636685A2 (en) * 1993-07-29 1995-02-01 Dow Corning S.A. Particulate foam control agents and their use
EP0636684A2 (en) * 1993-07-29 1995-02-01 Dow Corning S.A. Particulate foam control agents
EP0718018A2 (en) 1994-12-24 1996-06-26 Dow Corning S.A. Particulate foam control agents and their use
EP0723795A2 (en) * 1995-01-26 1996-07-31 Dow Corning S.A. Particulate foam control agents and their use
US5589449A (en) * 1993-07-29 1996-12-31 Dow Corning S.A. Particulate foam control agents
US5691294A (en) * 1993-03-30 1997-11-25 The Procter & Gamble Company Flow aids for detergent powders comprising sodium aluminosilicate and hydrophobic silica
US6140301A (en) * 1995-04-27 2000-10-31 The Procter & Gamble Company Process for producing granular detergent components or compositions
US6165968A (en) * 1998-10-24 2000-12-26 Dow Corning S. A. Particulate foam control agents
US6521586B1 (en) 1999-08-13 2003-02-18 Dow Corning S.A. Silicone foam control agent
US6521587B1 (en) 1999-08-13 2003-02-18 Dow Corning S.A. Silicone foam control agent
EP2206765A1 (en) * 2009-01-08 2010-07-14 Unilever N.V. Detergent composition
US9023781B2 (en) 2011-06-29 2015-05-05 Nanjing Sixin Scientific-Technological Application Research Institute Co., Ltd. Particle defoamer comprising a silicone emulsion and process for preparing same
EP3240618B1 (en) 2014-12-30 2021-04-21 Kemira Oyj Defoaming compositions comprising hydroxy terminated siloxanes and methods of making and using the same

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EP0013028A1 (en) * 1979-01-02 1980-07-09 Henkel Kommanditgesellschaft auf Aktien Detergent with a polydimethyl-siloxane content possessing an anti-foaming activity, and process for its production
EP0036162A1 (en) * 1980-03-17 1981-09-23 Henkel Kommanditgesellschaft auf Aktien Low-phosphate foam regulated detergent
EP0142910A1 (en) * 1983-08-27 1985-05-29 The Procter & Gamble Company Suds suppressor compositions and their use in detergent compositions
EP0149264A1 (en) * 1983-11-09 1985-07-24 Unilever N.V. Stable, free-flowing particulate adjuncts for use in detergent compositions

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EP0013028A1 (en) * 1979-01-02 1980-07-09 Henkel Kommanditgesellschaft auf Aktien Detergent with a polydimethyl-siloxane content possessing an anti-foaming activity, and process for its production
EP0036162A1 (en) * 1980-03-17 1981-09-23 Henkel Kommanditgesellschaft auf Aktien Low-phosphate foam regulated detergent
EP0142910A1 (en) * 1983-08-27 1985-05-29 The Procter & Gamble Company Suds suppressor compositions and their use in detergent compositions
EP0149264A1 (en) * 1983-11-09 1985-07-24 Unilever N.V. Stable, free-flowing particulate adjuncts for use in detergent compositions

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0427577A1 (en) * 1989-10-09 1991-05-15 Rhone-Poulenc Chimie Aqueous zeolite suspension comprising of a silicon resin
EP0517298A1 (en) * 1991-06-03 1992-12-09 The Procter & Gamble Company Foam control agents in granular form
TR25905A (en) * 1991-06-03 1993-11-01 Procter & Gamble FOAM CONTROL MATERIALS IN GRANULAR FORM WITH SILICONE AND ALUMINOSILICATE.
EP0618290A1 (en) * 1993-03-30 1994-10-05 The Procter & Gamble Company Flow aids for detergent powders comprising sodium aluminosilicate and hydrophobic silica
US5691294A (en) * 1993-03-30 1997-11-25 The Procter & Gamble Company Flow aids for detergent powders comprising sodium aluminosilicate and hydrophobic silica
EP0636685A2 (en) * 1993-07-29 1995-02-01 Dow Corning S.A. Particulate foam control agents and their use
EP0636684A2 (en) * 1993-07-29 1995-02-01 Dow Corning S.A. Particulate foam control agents
EP0636685A3 (en) * 1993-07-29 1995-06-07 Dow Corning Sa Particulate foam control agents and their use.
EP0636684A3 (en) * 1993-07-29 1995-06-07 Dow Corning Sa Particulate foam control agents.
US5861368A (en) * 1993-07-29 1999-01-19 Dow Corning S. A. Particulate foam control agents and their use
US5589449A (en) * 1993-07-29 1996-12-31 Dow Corning S.A. Particulate foam control agents
US5668101A (en) * 1993-07-29 1997-09-16 Dow Corning S. A. Particulate foam control agents and their use
EP0718018A3 (en) * 1994-12-24 1997-01-22 Dow Corning Sa Particulate foam control agents and their use
US5767053A (en) * 1994-12-24 1998-06-16 Dow Corning S. A. Particulate foam control agents and their use
EP0718018A2 (en) 1994-12-24 1996-06-26 Dow Corning S.A. Particulate foam control agents and their use
EP0723795A3 (en) * 1995-01-26 1997-01-22 Dow Corning Sa Particulate foam control agents and their use
EP0723795A2 (en) * 1995-01-26 1996-07-31 Dow Corning S.A. Particulate foam control agents and their use
US6140301A (en) * 1995-04-27 2000-10-31 The Procter & Gamble Company Process for producing granular detergent components or compositions
US6165968A (en) * 1998-10-24 2000-12-26 Dow Corning S. A. Particulate foam control agents
US6521586B1 (en) 1999-08-13 2003-02-18 Dow Corning S.A. Silicone foam control agent
US6521587B1 (en) 1999-08-13 2003-02-18 Dow Corning S.A. Silicone foam control agent
EP2206765A1 (en) * 2009-01-08 2010-07-14 Unilever N.V. Detergent composition
US9023781B2 (en) 2011-06-29 2015-05-05 Nanjing Sixin Scientific-Technological Application Research Institute Co., Ltd. Particle defoamer comprising a silicone emulsion and process for preparing same
EP3240618B1 (en) 2014-12-30 2021-04-21 Kemira Oyj Defoaming compositions comprising hydroxy terminated siloxanes and methods of making and using the same

Also Published As

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EP0329842A3 (en) 1990-05-30
DE3805624A1 (en) 1989-08-31

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