EP1165743B1 - Aqueous multiphase surfactant preparations - Google Patents

Aqueous multiphase surfactant preparations Download PDF

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Publication number
EP1165743B1
EP1165743B1 EP00920627A EP00920627A EP1165743B1 EP 1165743 B1 EP1165743 B1 EP 1165743B1 EP 00920627 A EP00920627 A EP 00920627A EP 00920627 A EP00920627 A EP 00920627A EP 1165743 B1 EP1165743 B1 EP 1165743B1
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EP
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Prior art keywords
preparations
aqueous preparations
aqueous
contain
water
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EP00920627A
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German (de)
French (fr)
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EP1165743A1 (en
Inventor
Thomas Förster
Barbara Heide
Wolfhard Scholz
Soraya Heinen
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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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
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2006—Monohydric alcohols
    • C11D3/201—Monohydric alcohols linear
    • 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
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/0017—Multi-phase liquid 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
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • 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
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2006—Monohydric alcohols
    • C11D3/2017—Monohydric alcohols branched

Definitions

  • the invention relates to aqueous surfactant preparations which are in the state of rest in the form of two or more segregated, liquid, aqueous phases present by movement temporarily are dispersible in each other.
  • EP 0116 442 A1 describes a shampoo which consists of two separate aqueous Phases and whose specific heavier, lower phase has a content of at least 6 Wt .-% dissolved sodium hexametaphosphate has. Such a high content of condensed However, phosphates are neither advantageous in terms of application technology nor ecologically desirable.
  • JP 62 263 297 A1 cosmetic cleaners were known, the two denmischte, have liquid, aqueous phases and by a content of surfactants and water-soluble polymers are characterized.
  • the cleaning agents described there however, they take a relatively long time (several hours) until they mix in the mix Disconnect the idle state again.
  • the invention therefore aqueous, at rest in the form of two or more demixed aqueous, with intermittent intermittently dispersible phases present preparations with at least one dissolved surface-active compound and at least one dissolved polymer compound used to accelerate the phase separation at rest, at least one water-soluble, mono- or polyhydric alcohol with 2-9 C atoms, they are defined in the claims
  • dissolved surface-active Compounds can be ionogenic or nonionic compounds, it is crucial that they are a preferably linear lipid group having 8-22 C atoms and at least one water-solubilizing polyol or polyether group or a water-solubilizing salt-forming group, e.g. a carboxyl, sulfonate or sulfate ester group or both or an optionally quaternary ammonium group or ampholytic aminocarboxylate or Aminosulfonatrios or a betaine moiety, preferably at one end of the linear Contain lipid group.
  • water-solubilizing polyol or polyether group or a water-solubilizing salt-forming group e.g. a carboxyl, sulfonate or sulfate ester group or both or an optionally quaternary ammonium group or ampholytic aminocarboxylate or Aminosulfonatrios or a betaine moiety, preferably at one end of the
  • Suitable cosmetic cleaners are preferably those preparations which contain as surface-active compounds high-foaming anionic surfactants, preferably those with anionic sulfonate or sulfate ester groups in the form of their alkali metal, magnesium or ammonium salts.
  • Such preferably suitable surfactants are, above all, the alkylpolyglycol ether sulfate salts or the alkylpolyglycol ether sulfosuccinate salts which, for example, fulfill the general formula I or II as sodium salts: R 1 -O- (C 2 H 4 O) n -SO 3 Na
  • R 1 and R 2 is a preferably linear alkyl group having 8-22, preferably having 12-18 C atoms and n is a number from 1 to 6, preferably from 2-4.
  • Preferred preparations contain as surface-active compounds an alkylpolyglycol ether sulfate salt or an alkylpolyglycol ether-sulfosuccinate salt having an alkyl group with 12-18 C atoms and 1-6 glycol ether groups or a mixture thereof in a total amount of 5-20% by weight of the preparation, preferably from 8-12% by weight of the preparation.
  • anionic surfactants are, for example, soaps, N-acylamino acid salts, alkyl phosphate salts, alkylpolyglycate-carboxylate salts, alkyl sulfate-alkanolamine salts, alkylsulfonate salts, ⁇ -olefinsulfonate salts, acylisethionate salts and acyltaurine salts.
  • amphoteric and / or zwitterionic surfactants for example cocoamphoglycinate or cocoamidopropyl-dimethyl-ammonio-glycinate and betaine surfactants may also be present.
  • Nonionic surfactants for example the adducts of 6-30 moles of ethylene oxide with fatty acids, fatty alcohols, fatty acid monoglycerides, fatty acid alkanolamides, fatty acid sorbitan esters, alkylphenols, methylglucoside fatty acid esters and other polar lipids and alkylglucosides and their ethylene oxide adducts can also be present as surface-active substances.
  • the total amount of surfactants may be 5-40 wt .-%, but an amount of 5-20 wt .-% is preferred because otherwise the rapid separation of the phases is no longer guaranteed.
  • dissolved polymer compounds are all suitable in water or aqueous surfactant solutions at 20 ° C in amounts of at least 1% by weight soluble natural or synthetic high-molecular substances with recurring structural elements
  • natural polymers are water-soluble proteins or water-soluble polysaccharides or the water-soluble derivatives of water-insoluble proteins or polysaccharides understood.
  • Suitable natural polymers are e.g. Albumins, gelatin, glycosaminoglycans (Hyaluronic acid), chitosans, starch, guar, cellulose ethers, e.g. Methylcelluloses or Hydroxyethylcelluloses, carboxymethylcelluloses and cationic cellulose derivatives, e.g.
  • the with epoxypropyl-trimethylammoinum chloride modified starch, guar or Cellulose ethers are suitable polymer compounds.
  • Suitable synthetic polymer compounds are e.g. polyvinyl alcohols, Polyvinylpyrrolidone, polyacrylamides and polyalkylene glycols having molecular weights of more than 1000 D. Also water-soluble copolymers of acrylic acid, acrylamide, the Vinylpyrrolidons and other water-soluble monomers with non-water-soluble Comonomers are suitable as polymer compounds in the context of the present invention.
  • Polymer compounds selected from polypropylene glycols having molecular weights of more than 1000 D, hydroxyethylcelluloses, xanthan gum, dextran, sodium hyaluronate and cationic cellulose ethers.
  • the quantities required for separation Polymer compounds are of the type and molecular weight of the polymer compound dependent, it is general that the higher the quantities required, the lower the required quantities is the molecular weight of the polymer compound.
  • the very high molecular weight salts of Hyaluronic acid or xanthan gum are therefore amounts of 0.1 - 1 wt .-%, of Cellulose ethers such.
  • the upper limit of salary Polymer compounds should be chosen so that the preparation does not gel and the Demixing is not hindered by the toughness of the phases.
  • the dissolved surface-active compounds and polymer compounds can be individually or as combinations of two or more such surfactants or polymers in the Preparations should be included. It has been shown that it is for the segregation of Composition is advantageous if at least two different surface-active Compounds or at least two different polymer compounds in the Contain compositions of the invention.
  • the polymer compounds has this is a combination of a particularly high molecular weight polymer with a low molecular weight polymer compound proved to be particularly suitable. So, for example Combinations of sodium hyaluronate with cellulose derivatives or of Polypropylene glycols having average molecular weights of 2000 D and more with such of 1000 D and less particularly well proven.
  • Suitable water-soluble mono- or polyhydric alcohols are all aliphatic alcohols, Diols or polyols, preferably those having 2-9 carbon atoms, in quantities of at least 1 wt .-% in water at 20 ° C are clearly soluble.
  • Such mono- or polyvalent ones Alcohols are in an amount of 1-40 wt .-% in the inventive preparations contain.
  • Suitable alcohols are e.g. Ethanol, 1-propanol, 2-propanol (isopropanol), n-butanol, Isobutanol, methoxyethanol or 2-ethoxyethanol.
  • Suitable diols are e.g.
  • Ethylene glycol 1,2-propylene glycol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, Diethylene glycol, triethylene glycol, dipropylene glycol, glycerol monomethyl ether or Cyclohexanediol.
  • Suitable polyols are glycerol, erythritol, diglycerol, triglycerol, sorbitol, Methyl glucoside, butyl glucoside, pentaerythritol or trimethyl propane.
  • the multiphase preparations of the present invention of the present invention separate particularly easy if, as alcohol, ethanol or isopropanol in an amount of 2 - 20 Wt .-% is included. It could be obtained in this way preparations that after intensive mixing of the phases at rest in less than 10 minutes to separate completely and be in the form of separate, clear phases.
  • Suitable electrolyte salts are especially water-soluble inorganic salts, e.g. Alkali halides such as sodium chloride (sodium chloride), calcium or Magnesium chloride, the sulphates of the alkali metals or of magnesium, sodium bicarbonate, Sodium hydrogen phosphate and sodium pyrophosphate but are also suitable salts of organic, low molecular weight acids, e.g.
  • Sodium acetate, sodium citrate, sodium lactate, Sodium toluenesulfonate, sodium xylenesulfonate or sodium benzoate are preferred water-soluble, inorganic electrolyte salts in an amount of 1-6 wt .-%.
  • the multiphase preparations according to the invention can also other advantageous for the application or the appearance Contain components, as they are common in cosmetic cleaning and care products.
  • these are e.g. Dyes, fragrances, preservatives and pH-adjusting agents (buffer salts), Complexing agents, antioxidants and cosmetic or dermatological active substances, the give the skin a pleasant feel or give the hair a good finish or the cause specific dermatological effects on the skin.
  • dyes preferably from those which have a different solubility in the segregated, aqueous phases and in this way the preparations have a particularly appealing appearance to lend.
  • yellow dyes e.g. Quinoline yellow varnish (Food color E 104)
  • red dyes such as Cochenillerot lacquer (food color E 124) or blue dyes (Sudan blue)
  • blue dyes Sud blue
  • the surfactant preparations of the invention may e.g. as shampoos for shampooing, as Shower preparations, bath products, liquid soaps - but also as liquid cleaning agents in the Household or used as a mild detergent. That segregated two- or multi-phase appearance can be used to give the consumer the Make composition of cleansing and nourishing components vivid and to motivate him to homogenize the product before use by shaking to remove from to use all components in the same way.
  • the percentages given in the table refer to% by weight of anhydrous active substance.
  • the following raw materials were used: LES-Na Sodium C 12 / C 14 alkylpoly (2) glycol ether sulphate (Texapon®NSO, Henkel KGaA) SBE-Na Sulfosuccinic acid - alkyl (C 12/14 -poly (3) glycol ether monoester di-sodium salt (Texapon® SB3, Henkel KGaA) HEC Hydroxyethylcellulose, viscosity 25 ° C (1% by weight): 350 m Pa s Degree of substitution 2.5 Natrasol® 250 HR (Hercules) Xanthan gum Keltrol® SF (Kelco) IR 400 Polyquaternium-1 O (Polymer IR 400, Amerchol) dextran Fa. Sigma, MG: 2-82000 PPG 600 Polypropylene glycol, molecular weight about 6000

Abstract

The invention relates to aqueous preparations in the form of two or more separated, aqueous phases in the idle state, whereby said phases are dispersible together. The preparations have at least one surface-active compound and at least one solved polymer compound and are provided with an accelerated phase separation in the idle state when said preparations contain at least one water-soluble, monovalent or multivalent alcohol with 2-9 C-atoms. In a preferred embodiment, 2-20 wt. % of an ether sulfate or ether sulfosuccinate are contained as a surface-active substance and 2-20 wt. % of ethyl alcohol or isopropyl alcohol are contained as an alcohol. The polymer compound is preferably chosen from polypropylene glycol with molecular weights of more than 1,000 D, hydroxyethylcellulose, xanthan gum, dextrane, sodium hyaluronate or cationic cellulose ethers.

Description

Die Erfindung betrifft wässrige Tensidzubereitungen, die im Ruhezustand in Form von zwei oder mehr entmischten, flüssigen, wässrigen Phasen vorliegen, die durch Bewegung zeitweise ineinander dispergiebar sind.The invention relates to aqueous surfactant preparations which are in the state of rest in the form of two or more segregated, liquid, aqueous phases present by movement temporarily are dispersible in each other.

Die Verbraucher erwarten bei einem kosmetischen Reinigungs- oder Pflegemittel in der Regel nicht nur eine bestimmte, für den Körper, die Haut, Haare und Zähne nützliche Wirkung, sondern in gleicher Weise auch ein attraktives Aussehen und eine die Wirkung unterstreichende galenische Zubereitung.Consumers usually expect a cosmetic cleanser or conditioner not just a specific effect that is beneficial to the body, skin, hair and teeth, but in the same way also an attractive appearance and an effect underlining galenic preparation.

So wird z.B. in DE 1617208 A1 ein flüssiges Reinigungsmittel beschrieben, das aus einer nichtwässrigen, öligen Phase und einer wässrigen Phase besteht, die durch Schütteln in eine instabile Öl-in-Wasser-Emulsion überführt werden können. Solche Zubereitungen sind aber nur mit einem hohen Anteil an Ölkomponenten zu realisieren und für viele kosmetische Reinigungszwecke wegen dieses hohen Ölgehalts ungeeignet.For example, in DE 1617208 A1 describes a liquid detergent, which consists of a non-aqueous, oily phase and an aqueous phase, which by shaking in a unstable oil-in-water emulsion can be transferred. But such preparations are Only with a high proportion of oil components to realize and for many cosmetic Cleaning purposes because of this high oil content unsuitable.

In EP 0116 442 A1 wird ein Shampoo beschrieben, das aus zwei entmischten wässrigen Phasen besteht und dessen spezifisch schwerere, untere Phase einen Gehalt von wenigstens 6 Gew.-% gelöstem Natriumhexametaphosphat aufweist. Ein so hoher Gehalt an kondensierten Phosphaten ist aber weder anwendungstechnisch vorteilhaft noch ökologisch erwünscht.EP 0116 442 A1 describes a shampoo which consists of two separate aqueous Phases and whose specific heavier, lower phase has a content of at least 6 Wt .-% dissolved sodium hexametaphosphate has. Such a high content of condensed However, phosphates are neither advantageous in terms of application technology nor ecologically desirable.

Schließlich waren aus JP 62 263 297 A1 kosmetische Reinigungsmittel bekannt, die zwei entmischte, flüssige, wässrige Phasen aufweisen und die durch einen Gehalt an Tensiden und wasserlöslichen Polymeren gekennzeichnet sind. Die dort beschriebenen Reinigungsmittel benötigen jedoch relativ lang (mehrere Stunden) bis sie sich nach dem Vermischen im Ruhezustand wieder entmischen.Finally, from JP 62 263 297 A1 cosmetic cleaners were known, the two denmischte, have liquid, aqueous phases and by a content of surfactants and water-soluble polymers are characterized. The cleaning agents described there However, they take a relatively long time (several hours) until they mix in the mix Disconnect the idle state again.

Es wurde daher nach Möglichkeiten gesucht, um eine raschere Entmischung der beiden wässrigen Phasen solcher Reinigungsmittel zu erreichen, damit der Verbraucher auch bei häufigerer Verwendung solche Produkte jedesmal im entmischten Zustand vorfindet. It was therefore looking for ways to a faster separation of the two to achieve aqueous phases of such detergents, so that the consumer also at more frequent use such products every time segregated state finds.

Als Lösung dieser Aufgabe wurde gefunden, daß eine Beschleunigung der Entmischung im Ruhezustand durch einen Gehalt an wasserlöslichen, ein- oder mehrwertigen Alkoholen erreicht werden kann.As a solution to this problem has been found that an acceleration of segregation in Resting state by a content of water-soluble, monohydric or polyhydric alcohols can be achieved.

Gegenstand der Erfindung sind daher wässrige, im Ruhezustand in Form von zwei oder mehr entmischten wässrigen, unter Bewegung zeitweise ineinander dispergierbaren Phasen vorliegende Zubereitungen mit wenigstens einer gelösten oberflächenaktiven Verbindung und wenigstens einer gelösten Polymerverbindung, die zur Beschleunigung der Phasentrennung im Ruhezustand wenigstens einen wasserlöslichen, ein- oder mehrwertigen Alkohol mit 2 - 9 C-Atomen enthalten, eine sie in den Ansprüchen definiert sindThe invention therefore aqueous, at rest in the form of two or more demixed aqueous, with intermittent intermittently dispersible phases present preparations with at least one dissolved surface-active compound and at least one dissolved polymer compound used to accelerate the phase separation at rest, at least one water-soluble, mono- or polyhydric alcohol with 2-9 C atoms, they are defined in the claims

Die in der erfindungsgemäßen Zubereitung zusätzlich enthaltenen, gelösten oberflächenaktiven Verbindungen können ionogene oder nichtionische Verbindungen sein, entscheidend ist, daß sie eine bevorzugt lineare Lipidgruppe mit 8-22 C-Atomen und wenigstens eine wasserlöslich machende Polyol- oder Polyethergruppe oder eine wasserlöslich machende salzbildende Gruppe, z.B. eine Carboxyl-, Sulfonat- oder Sulfatestergruppe oder beides oder eine ggf. quartäre Ammoniumgruppe oder ampholytische Aminocarboxylat- oder Aminosulfonatgruppe oder eine Betaingruppierung, bevorzugt an einem Ende der linearen Lipidgruppe enthalten.The additionally contained in the preparation according to the invention, dissolved surface-active Compounds can be ionogenic or nonionic compounds, it is crucial that they are a preferably linear lipid group having 8-22 C atoms and at least one water-solubilizing polyol or polyether group or a water-solubilizing salt-forming group, e.g. a carboxyl, sulfonate or sulfate ester group or both or an optionally quaternary ammonium group or ampholytic aminocarboxylate or Aminosulfonatgruppe or a betaine moiety, preferably at one end of the linear Contain lipid group.

Als kosmetische Reinigungsmittel eignen sich bevorzugt solche Zubereitungen, die als oberflächenaktive Verbindungen schaumstarke anionische Tenside, bevorzugt also solche mit anionischen Sulfonat- oder Sulfatestergruppen in Form ihrer Alkali-, Magnesium- oder Ammoniumsalze enthalten. Solche bevorzugt geeigneten Tenside sind vor allem die Alkylpolyglycolether-sulfat-Salze oder die Alkylpolyglycolether-sulfosuccinat-Salze, die z.B. als Natriumsalze die allgemeine Formel I bzw. II erfüllen: R1-O-(C2H4O)n-SO3 Na

Figure 00020001
Suitable cosmetic cleaners are preferably those preparations which contain as surface-active compounds high-foaming anionic surfactants, preferably those with anionic sulfonate or sulfate ester groups in the form of their alkali metal, magnesium or ammonium salts. Such preferably suitable surfactants are, above all, the alkylpolyglycol ether sulfate salts or the alkylpolyglycol ether sulfosuccinate salts which, for example, fulfill the general formula I or II as sodium salts: R 1 -O- (C 2 H 4 O) n -SO 3 Na
Figure 00020001

In diesen Formeln ist R1 und R2 eine bevorzugt lineare Alkylgruppe mit 8 - 22, bevorzugt mit 12-18 C-Atomen und n eine Zahl von 1 - 6, bevorzugt von 2-4.
Bevorzugt geeignete Zubereitungen enthalten als oberflächenaktive Verbindungen ein Alkylpolyglycolethersulfatsalz oder ein Alkylpolyglycolether-sulfosuccinatsalz mit einer Alkylgruppe mit 12-18 C-Atomen und 1- 6 Glycolethergruppen oder ein Gemisch davon in einer Menge von insgesamt 5-20 Gew.-% der Zubereitung, bevorzugt von 8-12 Gew.-% der Zubereitung.
Weitere geeignete anionische Tenside sind z.B. Seifen, N-Acylaminosäure-Salze, Alkylphosphat-Salze, Alkylpolyglycotether-carboxylat-Salze, Alkylsulfat-Alkanolamin-Salze, Alkylsulfonat-Salze, α-Olefinsulfonat-Salze, Acylisethionat-Salze und Acyltaurin-Salze.In these formulas, R 1 and R 2 is a preferably linear alkyl group having 8-22, preferably having 12-18 C atoms and n is a number from 1 to 6, preferably from 2-4.
Preferred preparations contain as surface-active compounds an alkylpolyglycol ether sulfate salt or an alkylpolyglycol ether-sulfosuccinate salt having an alkyl group with 12-18 C atoms and 1-6 glycol ether groups or a mixture thereof in a total amount of 5-20% by weight of the preparation, preferably from 8-12% by weight of the preparation.
Further suitable anionic surfactants are, for example, soaps, N-acylamino acid salts, alkyl phosphate salts, alkylpolyglycate-carboxylate salts, alkyl sulfate-alkanolamine salts, alkylsulfonate salts, α-olefinsulfonate salts, acylisethionate salts and acyltaurine salts.

Daneben können auch amphotere und/oder zwitterionische Tenside, z.B. Cocoamphoglycinat oder Cocoamidopropyl-dimethyl-ammonio-glycinat und Betaintenside enthalten sein.
Auch nichtionische Tenside, z.B. die Anlagerungsprodukte von 6-30 Mol Ethylenoxid an Fettsäuren, Fettalkohole, Fettsäuremonoglyceride, Fettsäurealkanolamide, Fettsäure-sorbitanester, Alkylphenole, Methylglucosid-Fettsäureester und andere polare Lipide sowie Alkylglucoside und deren Ethylenoxidaddukte können als oberflächenaktive Stoffe enthalten sein.
Die Gesamtmenge an oberflächenaktiven Stoffen kann 5-40 Gew.-% betragen, eine Menge von 5-20 Gew.-% ist aber bevorzugt, da sonst die rasche Entmischung der Phasen nicht mehr gewährleistet ist.In addition, amphoteric and / or zwitterionic surfactants, for example cocoamphoglycinate or cocoamidopropyl-dimethyl-ammonio-glycinate and betaine surfactants may also be present.
Nonionic surfactants, for example the adducts of 6-30 moles of ethylene oxide with fatty acids, fatty alcohols, fatty acid monoglycerides, fatty acid alkanolamides, fatty acid sorbitan esters, alkylphenols, methylglucoside fatty acid esters and other polar lipids and alkylglucosides and their ethylene oxide adducts can also be present as surface-active substances.
The total amount of surfactants may be 5-40 wt .-%, but an amount of 5-20 wt .-% is preferred because otherwise the rapid separation of the phases is no longer guaranteed.

Als gelöste Polymerverbindungen eignen sich alle in Wasser oder wässrigen Tensidlösungen bei 20° C in Mengen von wenigstens 1 Gew.-% löslichen natürlichen oder synthetischen hochmolekularen Stoffe mit wiederkehrenden Strukturelementen Als natürliche Polymere werden dabei wasserlösliche Proteine oder wasserlösliche Polysaccharide oder die wasserlöslichen Derivate von wasserunlöslichen Proteinen oder Polysacchariden verstanden. Geeignete natürliche Polymere sind z.B. Albumine, Gelatine, Glycosaminoglycane (Hyaluronsäure), Chitosane, Stärke, Guar, Celluloseether, z.B. Methylcellulosen oder Hydroxyethylcellulosen, Carboxymethylcellulosen und kationische Cellulosederivate, z.B. die mit Epoxypropyl-trimethylammoinumchlorid modifizierten Stärke-, Guar- oder Celluloseether. Auch die wasserlöslichen Biopolymeren wie z.B. Xanthan-Gum oder die Dextrane und Pullulan sind geeignete Polymerverbindungen. As dissolved polymer compounds are all suitable in water or aqueous surfactant solutions at 20 ° C in amounts of at least 1% by weight soluble natural or synthetic high-molecular substances with recurring structural elements As natural polymers are water-soluble proteins or water-soluble polysaccharides or the water-soluble derivatives of water-insoluble proteins or polysaccharides understood. Suitable natural polymers are e.g. Albumins, gelatin, glycosaminoglycans (Hyaluronic acid), chitosans, starch, guar, cellulose ethers, e.g. Methylcelluloses or Hydroxyethylcelluloses, carboxymethylcelluloses and cationic cellulose derivatives, e.g. the with epoxypropyl-trimethylammoinum chloride modified starch, guar or Cellulose ethers. Also, the water-soluble biopolymers such as e.g. Xanthan gum or the Dextrans and pullulan are suitable polymer compounds.

Geeignete synthetische Polymerverbindungen sind z.B. Polyvinylalkohole, Polyvinylpyrrolidon, Polyacrylamide und Polyalkylenglykole mit Molekulargewichten von mehr als 1000 D. Auch wasserlösliche Copolymerisate der Acrylsäure, des Acrylamids, des Vinylpyrrolidons und anderer wasserlöslicher Monomeren mit nicht-wasserlöslichen Comonomeren sind als Polymerverbindungen im Sinne der vorliegenden Erfindung geeignet.Suitable synthetic polymer compounds are e.g. polyvinyl alcohols, Polyvinylpyrrolidone, polyacrylamides and polyalkylene glycols having molecular weights of more than 1000 D. Also water-soluble copolymers of acrylic acid, acrylamide, the Vinylpyrrolidons and other water-soluble monomers with non-water-soluble Comonomers are suitable as polymer compounds in the context of the present invention.

Bevorzugt geeignet zur Herstellung der erfindungsgemäßen Zubereitungen sind Polymerverbindungen ausgewählt aus Polypropylenglycolen mit Molekulargewichten von mehr als 1000 D, Hydroxyethylcellulosen, Xanthan-Gum, Dextran, Natrium-Hyaluronat und kationischen Celluloseethem. Die zur Entmischung erforderlichen Mengen an Polymerverbindungen sind von der Art und dem Molekulargewicht der Polymerverbindung abhängig, dabei gilt allgemein, daß die erforderlichen Mengen um so niedriger sind, je höher das Molekulargewicht der Polymerverbindung ist. Von den sehr hochmolekularen Salzen der Hyaluronsäure oder von Xanthan-Gum sind daher Mengen von 0,1 - 1 Gew.-%, von Celluloseethern wie z.B. Hydroxyethylcellulose oder den kationischen Celluloseethern sind Mengen von 0,5 - 6 Gew.-% ausreichend, während z.B. Polypropylenglycole oder abgebaute Dextrane in Mengen von 2- 20 Gew.-% enthalten sein sollen. Die Obergrenze des Gehalts an Polymerverbindungen ist so zu wählen, daß die Zubereitung nicht geliert und die Entmischung durch die Zähigkeit der Phasen nicht behindert wird.They are preferably suitable for the preparation of the preparations according to the invention Polymer compounds selected from polypropylene glycols having molecular weights of more than 1000 D, hydroxyethylcelluloses, xanthan gum, dextran, sodium hyaluronate and cationic cellulose ethers. The quantities required for separation Polymer compounds are of the type and molecular weight of the polymer compound dependent, it is general that the higher the quantities required, the lower the required quantities is the molecular weight of the polymer compound. Of the very high molecular weight salts of Hyaluronic acid or xanthan gum are therefore amounts of 0.1 - 1 wt .-%, of Cellulose ethers such. Hydroxyethylcellulose or the cationic cellulose ethers Amounts of 0.5-6 wt.%, While e.g. Polypropylene glycols or degraded Dextrans in amounts of 2- 20 wt .-% should be included. The upper limit of salary Polymer compounds should be chosen so that the preparation does not gel and the Demixing is not hindered by the toughness of the phases.

Die gelösten oberflächenaktiven Verbindungen und Polymerverbindungen können einzeln oder als Kombinationen von zwei oder mehr solcher Tenside oder Polymeren in den Zubereitungen enthalten sein. Dabei hat sich gezeigt, daß es für die Entmischung der Zusammensetzung vorteilhaft ist, wenn wenigstens zwei unterschiedliche oberflächenaktive Verbindungen oder wenigstens zwei unterschiedliche Polymerverbindungen in den erfindungsgemäßen Zusammensetzungen enthalten sind. Bei den Polymerverbindungen hat sich dabei eine Kombination eines besonders hochmolekularen Polymerisats mit einer niedrigmolekularen Polymerverbindung als besonders geeignet erwiesen. So haben sich z.B Kombinationen von Natrium-Hyaluronat mit Cellulosederivaten oder von Polypropylenglycolen mit mittlerem Molekulargewichten von 2000 D und mehr mit solchen von 1000 D und weniger besonders gut bewährt.The dissolved surface-active compounds and polymer compounds can be individually or as combinations of two or more such surfactants or polymers in the Preparations should be included. It has been shown that it is for the segregation of Composition is advantageous if at least two different surface-active Compounds or at least two different polymer compounds in the Contain compositions of the invention. For the polymer compounds has this is a combination of a particularly high molecular weight polymer with a low molecular weight polymer compound proved to be particularly suitable. So, for example Combinations of sodium hyaluronate with cellulose derivatives or of Polypropylene glycols having average molecular weights of 2000 D and more with such of 1000 D and less particularly well proven.

Als wasserlösliche ein- oder mehrwertige Alkohole eignen sich alle aliphatischen Alkohole, Diole oder Polyole, bevorzugt solche mit 2-9 Kohlenstoffatomen, die in Mengen von wenigstens 1 Gew.-% in Wasser bei 20°C klar löslich sind. Solche ein- oder mehrwertigen Alkohole sind in einer Menge von 1- 40 Gew.-% in den erfindungsgemäßen Zubereitungen enthalten. Geeignete Alkohole sind z.B. Ethanol, 1-Propanol, 2-Propanol (Isopropanol), n-Butanol, Isobutanol, Methoxyethanol oder 2-Ethoxyethanol. Geeignete Diole sind z.B. Ethylenglycol, 1,2-Propylenglycol, 1,4-Butandiol, 1,5-Pentandiol, 1,6-Hexandiol, Diethylenglycol, Triethylenglycol, Dipropylenglycol, Glycerinmonomethylether oder Cyclohexandiol. Geeignete Polyole sind Glycerin, Erythrit, Diglycerin, Triglycerin, Sorbit, Methylglucosid, Butylglucosid, Pentaerythrit oder Trimethyl-propan.Suitable water-soluble mono- or polyhydric alcohols are all aliphatic alcohols, Diols or polyols, preferably those having 2-9 carbon atoms, in quantities of at least 1 wt .-% in water at 20 ° C are clearly soluble. Such mono- or polyvalent ones Alcohols are in an amount of 1-40 wt .-% in the inventive preparations contain. Suitable alcohols are e.g. Ethanol, 1-propanol, 2-propanol (isopropanol), n-butanol, Isobutanol, methoxyethanol or 2-ethoxyethanol. Suitable diols are e.g. Ethylene glycol, 1,2-propylene glycol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, Diethylene glycol, triethylene glycol, dipropylene glycol, glycerol monomethyl ether or Cyclohexanediol. Suitable polyols are glycerol, erythritol, diglycerol, triglycerol, sorbitol, Methyl glucoside, butyl glucoside, pentaerythritol or trimethyl propane.

Die erfindungsgemäßen Mehrphasen-Zubereitungen der vorliegenden Erfindung entmischen sich besonders leicht, wenn als Alkohol Ethanol oder Isopropanol in einer Menge von 2 - 20 Gew.-% enthalten ist. Es konnten auf diese Weise Zubereitungen erhalten werden, die nach intensiver Vermischung der Phasen im Ruhezustand innerhalb von weniger als 10 Minuten sich vollständig entmischen und in Form von getrennten, klaren Phasen vorliegen.The multiphase preparations of the present invention of the present invention separate particularly easy if, as alcohol, ethanol or isopropanol in an amount of 2 - 20 Wt .-% is included. It could be obtained in this way preparations that after intensive mixing of the phases at rest in less than 10 minutes to separate completely and be in the form of separate, clear phases.

Die Separation diskreter wässriger Phasen kann weiterhin durch einen Gehalt an gelösten Elektrolytsalzen gefördert werden. Geeignete Elektrolytsalze sind vor allem wasserlösliche anorganische Salze, z.B. Alkalihalogenide wie Kochsalz (Natriumchlorid), Calzium- oder Magnesium-chlorid, die Sulfate der Alkalimetalle oder des Magnesiums, Natriumbicarbonat, Natriumhydrogenphosphat und Natriumpyrophosphat Geeignet sind aber auch die Salze von organischen, niedermolekularen Säuren, z.B. Natriumacetat, Natriumcitrat, Natriumlactat, Natrium-toluolsulfonat, Natrium-xylolsulfonat oder Natriumbenzoat Bevorzugt sind wasserlösliche, anorganische Elektrolytsalze in eine Menge von 1-6 Gew.-% enthalten.The separation of discrete aqueous phases may further be solved by a content of dissolved Be promoted electrolyte salts. Suitable electrolyte salts are especially water-soluble inorganic salts, e.g. Alkali halides such as sodium chloride (sodium chloride), calcium or Magnesium chloride, the sulphates of the alkali metals or of magnesium, sodium bicarbonate, Sodium hydrogen phosphate and sodium pyrophosphate but are also suitable salts of organic, low molecular weight acids, e.g. Sodium acetate, sodium citrate, sodium lactate, Sodium toluenesulfonate, sodium xylenesulfonate or sodium benzoate are preferred water-soluble, inorganic electrolyte salts in an amount of 1-6 wt .-%.

Neben den genannten Komponenten können die erfindungsgemäßen Mehrphasen-Zubereitungen auch weitere, für die Anwendung oder das Aussehen vorteilhafte Komponenten enthalten, wie sie in kosmetischen Reinigungs- und Pflegemitteln üblich sind. Dies sind z.B. Farbstoffe, Duftstoffe, Konservierungsmittel und PH-Stellmittel (Pfuffersalze), Komplexbildner, Antioxidantien und kosmetische oder dermatologische Wirksubstanzen, die der Haut ein angenehmes Hautgefühl oder den Haaren eine gute Avivage verleihen oder die spezifischen dermatologischen Effekte auf der Haut bewirken.In addition to the components mentioned, the multiphase preparations according to the invention can also other advantageous for the application or the appearance Contain components, as they are common in cosmetic cleaning and care products. These are e.g. Dyes, fragrances, preservatives and pH-adjusting agents (buffer salts), Complexing agents, antioxidants and cosmetic or dermatological active substances, the give the skin a pleasant feel or give the hair a good finish or the cause specific dermatological effects on the skin.

Von besonderer Bedeutung ist der Zusatz von ein oder zwei Farbstoffen, bevorzugt von solchen, die in den entmischten, wässrigen Phasen eine unterschiedliche Löslichkeit aufweisen und auf diese Weise den Zubereitungen ein besonders ansprechendes Aussehen verleihen. So konnte z.B. durch Zusatz von gelben Farbstoffen wie z.B. Chinolingelb Lack (Lebensmittelfarbstoff E 104), roten Farbstoffen wie Cochenillerot Lack (Lebensmittelfarbstoff E 124) oder blauen Farbstoffen (Sudanblau) unterschiedlich gefärbte Phasen der erfindungsgemäßen Zusammensetzungen erzielt werden.Of particular importance is the addition of one or two dyes, preferably from those which have a different solubility in the segregated, aqueous phases and in this way the preparations have a particularly appealing appearance to lend. For example, by the addition of yellow dyes, e.g. Quinoline yellow varnish (Food color E 104), red dyes such as Cochenillerot lacquer (food color E 124) or blue dyes (Sudan blue) differently colored phases of the Compositions according to the invention can be achieved.

Die erfindungsgemäßen Tensidzubereitungen können z.B. als Shampoos zur Haarwäsche, als Duschpräparate, Badezusätze, flüssige Seifen - aber auch als flüssige Reinigungsmittel im Haushalt oder als Feinwaschmittel verwendet werden. Das entmischte zwei- oder mehrphasige Erscheinungsbild kann dazu benutzt werden, dem Verbraucher die Zusammensetzung aus reinigenden und pflegenden Komponenten anschaulich zu machen und ihn zu motivieren, das Produkt vor Gebrauch durch Schütteln zu homogenisieren, um von allen Komponenten in gleicher Weise Gebrauch zu machen.The surfactant preparations of the invention may e.g. as shampoos for shampooing, as Shower preparations, bath products, liquid soaps - but also as liquid cleaning agents in the Household or used as a mild detergent. That segregated two- or multi-phase appearance can be used to give the consumer the Make composition of cleansing and nourishing components vivid and to motivate him to homogenize the product before use by shaking to remove from to use all components in the same way.

Die folgenden Beispiele sollen den Gegenstand der Erfindung näher erläutern - ohne ihn darauf zu beschränken: The following examples are intended to explain the subject matter of the invention in more detail - without him to limit it to:

BeispieleExamples

Es wurden Zweiphasen-Zusammensetzungen durch Vermischen der in Tabelle I angegebenen Komponenten hergestellt.Two-phase compositions were prepared by mixing those listed in Table I. Components made.

Teilweise wurden auch Farbstoffe eingearbeitet.
Dabei wurde ein Teil des Tensids mit dem Farbstoff gemischt und dann zugegeben. So wurde z.B. in Beispiel 11 ein Teil des wässrigen Ethersulfats mit Sudanblau und ein anderer Teil des Ethersulfats mit Chinolingelblack gefärbt. Auf diese Weise werden - nach Separation der Phasen - eine obere blaue und eine untere gelbe Phase erhalten.Partly also dyes were incorporated.
In this case, a part of the surfactant was mixed with the dye and then added. For example, in Example 11, a portion of the aqueous ether sulfate was stained with Sudan blue and another portion of the ether sulfate was tinted with quinoline yellow. In this way - after separation of the phases - an upper blue and a lower yellow phase are obtained.

Die Phasenseparation erfolgte in einer Zeitspanne von 5-60 Minuten. Die Beispiele mit einem Gehalt an Ethanol zeigten eine raschere Phasentrennung, meist innerhalb von 10 Minuten. Beispiele Nr. 1 2 3 4 5 6 7 8 LES-Na 10 10 4,5 4,5 4,5 4,5 4,5 4,5 SBE-Na - - 4,5 4,5 4,5 4,5 4,5 4,5 PPG 6000 - - - - - - - - PPG 2000 20 10 10 - - - - - PPG 620 20 10 10 - - - - - HEC - - - 1,25 1,25 1,5 1,25 1,5 Xanthan-Gum - - 0,4 - - - - - Na-Hyaluronat - - - 0,5 0,1 - - - IR 400 - - - - - - - - Glycerin 10 10 5 - - 10 10 5 1,2-Propylenglycol - - 10 - - - - 10 Ethanol - - 5 3 - 5 - Parfumöl - - - 1 - - - 1 1 Na Cl - - 2 1 2 3 2 2 Wasser und Farbstoffe ad 100 ad 100 ad 100 ad 100 ad 100 ad 100 ad 100 ad 100 The phase separation was carried out in a period of 5-60 minutes. The examples containing ethanol showed a faster phase separation, usually within 10 minutes. Examples no. 1 2 3 4 5 6 7 8th LES-Na 10 10 4.5 4.5 4.5 4.5 4.5 4.5 SBE-Na - - 4.5 4.5 4.5 4.5 4.5 4.5 PPG 6000 - - - - - - - - PPG 2000 20 10 10 - - - - - PPG 620 20 10 10 - - - - - HEC - - - 1.25 1.25 1.5 1.25 1.5 Xanthan gum - - 0.4 - - - - - Na hyaluronate - - - 0.5 0.1 - - - IR 400 - - - - - - - - glycerin 10 10 5 - - 10 10 5 1,2-propylene glycol - - 10 - - - - 10 ethanol - - 5 3 - 5 - Perfume oil - - - 1 - - - 1 1 Na Cl - - 2 1 2 3 2 2 Water and dyes ad 100 ad 100 ad 100 ad 100 ad 100 ad 100 ad 100 ad 100

Die in der Tabelle angegebenen Prozentzahlen beziehen sich auf Gewichts% wasserfreier Aktivsubstanz.
Es wurden die folgenden Rohstoffe eingesetzt: LES-Na Natrium C12/C14-Alkylpoly (2)glycolethersulfat (Texapon®NSO, Henkel KGaA) SBE-Na Sulfobernsteinsäure - Alkyl(C12/14-poly(3)glycolethermonoester-di-Natriumsalz (Texapon®SB3, Henkel KGaA) HEC Hydroxyethylcellulose, Viskosität 25°C (1-Gew.%) : 350 m Pa s Substitutionsgrad 2,5 Natrasol® 250 HR (Hercules) Xanthan-Gum Keltrol® SF (Kelco) IR 400 Polyquatemium-1 0 (Polymer IR 400, Amerchol) Dextran Fa. Sigma, MG : 2-82000 PPG 600 Polypropylenglycol, Molgewicht ca. 6000 The percentages given in the table refer to% by weight of anhydrous active substance.
The following raw materials were used: LES-Na Sodium C 12 / C 14 alkylpoly (2) glycol ether sulphate (Texapon®NSO, Henkel KGaA) SBE-Na Sulfosuccinic acid - alkyl (C 12/14 -poly (3) glycol ether monoester di-sodium salt (Texapon® SB3, Henkel KGaA) HEC Hydroxyethylcellulose, viscosity 25 ° C (1% by weight): 350 m Pa s Degree of substitution 2.5 Natrasol® 250 HR (Hercules) Xanthan gum Keltrol® SF (Kelco) IR 400 Polyquaternium-1 O (Polymer IR 400, Amerchol) dextran Fa. Sigma, MG: 2-82000 PPG 600 Polypropylene glycol, molecular weight about 6000

Claims (7)

  1. Aqueous preparations which, at rest, are present as two or more separated aqueous phases temporarily dispersible in one another by agitation and which contain at least one dissolved surface-active compound selected from an alkyl polyglycol ether sulfate salt or an alkyl polyglycol ether sulfosuccinate salt containing an alkyl group with 12 to 18 carbon atoms and 1 to 6 glycidyl ether groups or a mixture thereof and at least one dissolved polymer compound, characterized in that at least one water-soluble, mono- or polyhydric alcohol containing 2 to 9 carbon atoms is present to accelerate phase separation in the rest state.
  2. Aqueous preparations as claimed in claim 1, characterized in that ethanol or isopropanol in a quantity of 2 to 20% by weight is present as the alcohol.
  3. Aqueous preparations as claimed in claim 1 or 2, characterized in that the surface-active compound is present in a total quantity of 5 to 20% by weight.
  4. Aqueous preparations as claimed in any of claims 1 to 3, characterized in that the polymer compound is a compound selected from polypropylene glycols with a molecular weight of more than 1,000 D, a hydroxyethyl cellulose, xanthan gum, dextran, sodium hyaluronate or cationic cellulose ethers.
  5. Aqueous preparations as claimed in any of claims 1 to 4, characterized in that they contain at least two different surface-active compounds or at least two different polymer compounds.
  6. Aqueous preparations as claimed in any of claims 1 to 5, characterized in that they contain water-soluble inorganic electrolyte salts in a quantity of 1 to 6% by weight to promote phase separation.
  7. Aqueous preparations as claimed in any of claims 1 to 6, characterized in that they contain dyes differing in their solubility in the separated aqueous phases.
EP00920627A 1999-04-08 2000-03-30 Aqueous multiphase surfactant preparations Expired - Lifetime EP1165743B1 (en)

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AU1152601A (en) * 1999-10-22 2001-05-08 Reckitt Benckiser France Compositions and their use
DE19951635A1 (en) * 1999-10-26 2001-05-17 Henkel Kgaa Aqueous multiphase detergent
US6429177B1 (en) * 2000-08-22 2002-08-06 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Separating multi-phase personal wash composition in a transparent or translucent package
DE10062045A1 (en) * 2000-12-13 2002-06-27 Henkel Kgaa Different colored aqueous multiphase cleaner
DE10206795A1 (en) * 2002-02-19 2003-08-28 Beiersdorf Ag Two-phase cosmetic or dermatological compositions useful as sunscreen, artificial tanning or insect repellent products comprise a microemulsion phase and a lipophilic phase
US6787511B2 (en) * 2002-08-14 2004-09-07 Unilever Home & Personal Care Usa Division Of Conopco, Inc. Biphasic composition induced by polydextrose
DE10341024A1 (en) * 2003-09-03 2005-03-31 Hans Schwarzkopf & Henkel Gmbh & Co. Kg Multiphase surfactant product
WO2005023975A1 (en) * 2003-09-03 2005-03-17 Henkel Kommanditgesellschaft Auf Aktien Multi-phase cosmetic agent for cleansing hair and skin
FR2859626B1 (en) * 2003-09-12 2006-01-27 Oreal BIPHASE COMPOSITION AND USES IN THE COSMETIC FIELD
FR2871373B1 (en) * 2004-06-11 2006-12-01 Oreal METHOD FOR WASHING FROZEN OR CREPUS HAIR
DE102004054278A1 (en) * 2004-11-10 2006-06-01 Wella Ag Clear, biphasic, foam-forming aerosol hair styling product
US20060140897A1 (en) * 2004-12-28 2006-06-29 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Biphasic inducing agent for aqueous cleansing compositions
DE102005051860A1 (en) * 2005-10-25 2007-04-26 Beiersdorf Ag Aqueous cosmetic preparation, useful as e.g. soaking medium for patch or cloth, comprises 1,2-hexanediol
DE102005051864A1 (en) 2005-10-25 2007-04-26 Beiersdorf Ag Cosmetic oil-in-water emulsion for, e.g. ointment, cream, or low-viscosity lotion, includes 1,2-hexanediol, and oil-in-water emulsifiers
EP1894994B1 (en) 2006-08-31 2013-10-16 Henkel AG & Co. KGaA Two or more phase face cleansing agent with improved reversible mixing and demixing solution
DE102014205475A1 (en) * 2014-03-25 2015-10-01 Beiersdorf Ag Polypropylene glycols with antimicrobial activity in cosmetic or dermatological preparations
US11459527B2 (en) 2017-11-30 2022-10-04 Colgate-Palmolive Company Cleansing compositions and use thereof

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FR1188460A (en) * 1955-09-06 1959-09-23 Colgate Palmolive Co Detergent composition in the form of a suspension
GB8421196D0 (en) * 1984-08-21 1984-09-26 Reckitt & Colmann Prod Ltd Cleansing compositions
JPS62263297A (en) * 1986-05-09 1987-11-16 ライオン株式会社 Two-phase separable liquid detergent composition
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