WO2000037594A2 - Liquides hydrophobes confectionnes sous presentation solide pour utilisation dans des agents nettoyants et detergents de densite apparente elevee. - Google Patents

Liquides hydrophobes confectionnes sous presentation solide pour utilisation dans des agents nettoyants et detergents de densite apparente elevee. Download PDF

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Publication number
WO2000037594A2
WO2000037594A2 PCT/EP1999/009838 EP9909838W WO0037594A2 WO 2000037594 A2 WO2000037594 A2 WO 2000037594A2 EP 9909838 W EP9909838 W EP 9909838W WO 0037594 A2 WO0037594 A2 WO 0037594A2
Authority
WO
WIPO (PCT)
Prior art keywords
dextrin
weight
encapsulated
liquid
detergent
Prior art date
Application number
PCT/EP1999/009838
Other languages
German (de)
English (en)
Other versions
WO2000037594A3 (fr
Inventor
Kathleen Paatz
Wolfgang Lahn
Original Assignee
Henkel Kommanditgesellschaft Auf Aktien
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel Kommanditgesellschaft Auf Aktien filed Critical Henkel Kommanditgesellschaft Auf Aktien
Priority to EP99962252A priority Critical patent/EP1141184A2/fr
Publication of WO2000037594A2 publication Critical patent/WO2000037594A2/fr
Publication of WO2000037594A3 publication Critical patent/WO2000037594A3/fr

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules

Definitions

  • the invention relates to a process for the production of granular detergents with high bulk density, which contain hydrophobic active ingredient components which are liquid at the manufacturing temperature in encapsulated form, and correspondingly encapsulated liquid active ingredient components.
  • compositions which contain mixtures of sparingly water-soluble oil, which is located on an inorganic carrier material, with a substance which is encapsulated in a water-sensitive matrix.
  • the substance encapsulated in the water-sensitive matrix is a perfume, a flavor, a cosmetic active ingredient or an organometallic complex.
  • Starch, maltodextrin, cyclodextrin, rubber, and resins come as the material for the water-sensitive matrix.
  • the encapsulation in the water-sensitive matrix is carried out essentially for reasons of stability.
  • Granular detergents with a high bulk density can be prepared according to the process of European patent EP 0 486 592. This involves the strand-shaped pressing of a homogeneous premix of detergent ingredients, which can optionally be carried out with the addition of a plasticizer, via hole shapes, which preferably have an opening width of 0.5 mm to 5 mm, subsequent comminution of the extrudate by means of a cutting device and subsequent treatment in a rounding machine, which results in largely uniform spherical products.
  • hydrophobic ingredients which are liquid at the processing temperatures of the abovementioned production process can be incorporated into extruded detergents with a high bulk density, in particular, without disadvantageous changes in solubility, if the hydrophobic ingredient is encapsulated in optionally hydrophobicized dextrin before the extrusion step.
  • the use of hydrophobic liquids encapsulated in dextrin leads to an improvement in the dissolving behavior of such detergents and cleaning agents.
  • a first subject of the invention is therefore a non-ionic surfactant encapsulated in dextrin.
  • a particulate encapsulation product preferably has a nonionic surfactant content in the range from 10% by weight to 60% by weight, in particular 15% by weight to 50% by weight. It preferably contains 40% by weight to 90% by weight, in particular 50% by weight to 85% by weight of dextrin or a mixture of dextrin and inorganic salts in which the content of inorganic salt is up to 50% by weight. %, in particular 5 wt .-% to 30 wt .-% of the mixture of dextrin and inorganic salt.
  • the encapsulation product can contain small amounts, preferably not more than 5% by weight, contain in particular 1% by weight to 3% by weight of water. It preferably has an average particle diameter in the range from 0.05 mm to 1 mm, in particular 0.2 mm to 0.8 mm.
  • Such an encapsulation product is preferably produced by a spray drying process.
  • the procedure is such that the dextrin or the combination of dextrin and inorganic salt is slurried or dispersed in water, then the nonionic surfactant to be encapsulated is added and it is dispersed into very fine drops by intensive mixing. Average drop sizes in the range from 1 ⁇ m to 2 ⁇ m and a maximum drop size of 10 ⁇ m are preferred.
  • the viscous liquid thus obtained is then spray-dried using a device which can be used for this purpose, a so-called spray tower.
  • the spray product obtained in this way can then be dried further using, for example, a fluidized-bed dryer, or a combination of the two drying methods, as has become known under the name “MSD process” (RA Youngs, ..spray drying encapsulation) - today's view ", Food, January 1986).
  • MSD process RA Youngs, ..spray drying encapsulation
  • the inorganic salt is not incorporated into the encapsulation product or not in its entirety via the aqueous dispersion to be sprayed, but instead is encapsulated by simultaneous powdering in addition to the spray.
  • Such a spray drying process can also be used for encapsulating any other hydrophobic liquids, wherein hydrophobic liquids are to be understood as those whose solubility in water at 20 ° C. is less than 5 vol. -% (less than 5 ml in 95 ml of water).
  • Such other hydrophobic liquids can be, for example, perfume oils and / or concentrated enzyme solutions, which can also be used in a mixture with the nonionic surfactants mentioned above.
  • the enzymes used here are the enzymatic active ingredients usually provided for use in detergents or cleaning agents, in particular lipase, Protease, amylase and / or cellulase. They usually have a molecular weight of at least 10,000 g / mol.
  • Another object of the invention is therefore a process for the production of granular detergents or cleaning agents with a high bulk density by strand-shaped pressing through hole shapes and subsequent comminution of the extrudate by means of a cutting device, which is characterized in that a hydrophobic liquid is encapsulated in dextrin, this encapsulation intermediate mixed with at least one solid and / or solid detergent constituent, extruded through a perforated plate and the extrudate optionally rounded and / or powdered.
  • Another object of the invention is therefore the use of hydrophobic liquids encapsulated in dextrin to improve the washing-in behavior and / or to increase the dissolution rate of detergents with a high bulk density.
  • the encapsulated liquid is mixed with the other solid and / or solid detergent ingredients in the course of the preparation of the agents.
  • the encapsulation product can also be subjected, together with further detergent or cleaning agent components, to a granulation step which is known in principle, and so detergents or cleaning agents with an increased bulk density can be obtained, with preference being given to this. use an anhydrous granulation liquid.
  • dextrins are to be understood as meaning oligomers or polymers of carbohydrates which are accessible by partial hydrolysis of starch.
  • the hydrolysis can be carried out by customary, for example acid or enzyme-catalyzed, processes. They are preferably hydrolysis products with average molecular weights in the range from 440 to 500,000.
  • the dextrin used in the process according to the invention or in encapsulation products according to the invention is preferably a polysaccharide with a dextrose equivalent (DE) in the range from 0. 5 to 40, in particular from 2 to 30, DE being a common measure of the reducing effect of a polysaccharide compared to dextrose, which has a DE of 100.
  • DE dextrose equivalent
  • Both dry glucose syrups (DE 20 to 37) and so-called yellow dextrins and white dextrins with higher average molecular weights in the range from about 2,000 to 30,000 can be used, so-called maltodextrins (DE 3 to 20) being preferred according to the invention.
  • the dextrins can also have been modified to be hydrophobic in a known manner. Another advantage of the invention in this context is that when the dextrins are used, active ingredients are introduced into the finished detergent or cleaning agent, which contribute to the washing result, since dextrins, as known from international patent application WO 97/20905, have a Have a cobuilder effect.
  • agents with a high bulk density should be understood to mean those with bulk densities of at least 550 g / 1, in particular from 600 g / 1 to 950 g / 1 and preferably from 700 g / 1 to 850 g / 1.
  • Nonionic surfactants which are contained in the encapsulation product according to the invention include, in particular, the alkoxylates, preferably the ethoxylates and / or propoxylates of alcohols, alkylamines, vicinal diols and / or carboxylic acid amides, which have alkyl groups with 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms.
  • the average degree of alkoxylation of these compounds is generally from 1 to 25, preferably 3 to 18 and particularly preferably 6 to 10. They can be prepared in a known manner by reaction with the corresponding alkylene oxides.
  • Products which can be prepared by alkoxylation of fatty acid alkyl esters with 1 to 4 carbon atoms in the ester part by the process of international patent application WO 90/13533 are also suitable.
  • Preferred among the carboxamide derivatives are the ethanolamide derivatives of alkanoic acids with 8 to 22 carbon atoms, preferably 12 to 16 carbon atoms.
  • the alcohol alkoxylates in question include the ethoxylates and / or propoxylates of linear or branched-chain alcohols having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms.
  • Derivatives of fatty alcohols are particularly suitable, although their branched-chain isomers can also be used to prepare usable alkoxylates.
  • the ethoxylates of primary alcohols with linear dodecyl, tetradecyl, hexadecyl or octadecyl radicals and mixtures thereof are particularly useful. It is also possible to use corresponding alkoxylates of mono- or polyunsaturated fatty alcohols, which include, for example, oleyl alcohol, elaidyl alcohol, linoleyl alcohol, linolenyl alcohol, gadoleyl alcohol and erucalcohol.
  • Nonionic surfactants to be encapsulated according to the invention are liquid, preferably at temperatures not above room temperature.
  • solid individual raw materials such as powdered polycarboxylate cobuilders, for example alkali citrate, solid inorganic builder materials such as zeolite-A, the solid and / or solid-form detergent or detergent constituents with which the encapsulation product is mixed prior to strand-like molding include solid individual raw materials.
  • solid or solid-form detergent ingredients can also, as an alternative to their processing via the premix to be extruded, be mixed with the extrudate in order to obtain a finished detergent or cleaning agent, as long as care is taken to ensure that at least one solid or Detergent ingredient prepared in solid form has found its way into the premix to be extruded together with the encapsulation product.
  • a premix is preferably made from 20% by weight to 70% by weight of a builder and surfactant-containing detergent product produced by spray drying, 3% by weight to 20% by weight of anionic surfactant compound according to WO 93/04162 with a content of more than 80 wt .-%, in particular over 90 wt .-% of alkyl sulfate with alkyl chain lengths in the range of C 12 to C lg , balance essentially inorganic salts and water, 2 wt .-% to 10 wt .-% powdered, separately added alkali carbonate .
  • polycarboxylate cobuilder for example alkali citrate
  • peroxobleaching agent for example sodium perborate monohydrate
  • the extrusion is carried out under conditions which are known in principle, preferably using an extruder, into which one contains the encapsulation product homogeneous premix and fed under a pressure in the range of preferably 30 bar to 180 bar, in particular 40 bar to 80 bar, through a perforated plate with a hole diameter of preferably 1.2 mm to 2.0 mm, in particular 1.4 mm to 1, 7 mm strand ve ⁇ resst and crushed to a length that does not differ significantly from the thickness, that is, the hole diameter.
  • the extrudate if desired with application of powdery solids as described in particular in international patent application WO 94/01526, can then be rounded and deburred in a conventional rounding device, for example a Spheronizer®.
  • a hydrophobized, oxidation-stable dextrin (Narlex® ST2, manufacturer National Starch) was dispersed in water (mixing ratio 1: 1) with stirring. After the dispersion had been heated to approximately 80-90 ° C., the dextrin swelled, and a viscosity of above 20,000 mPa.s was established. The solution was cooled to about 40 ° C. A 7-fold ethoxylated C 12/18 fatty alcohol (Dehydol® LT7, manufacturer Henkel KGaA) was added and finely dispersed in the aqueous starch solution using a Supraton® mixer.
  • the composition of the slurry to be sprayed was 42.4% by weight of dextrin, 42.4% by weight of water and 15.2% by weight of nonionic surfactant. It was spray-dried via a two-fluid nozzle with a liquid outlet diameter of 2 mm in a drying tower (manufacturer Niro Atomizer) according to the fountain principle, the throughput of the aqueous slurry being 14 kg / h and the drying gas at a temperature of 150 ° C. from above into the tower entered and left the tower at a temperature of 90 ° C.
  • the encapsulation product obtained had a water content of 2.6% by weight and a nonionic surfactant content of 27% by weight. It was a free-flowing, non-sticky powder with a bulk density of 280 g / 1.
  • Example 1 The procedure was as in Example 1, using a perfume oil instead of the nonionic surfactant.
  • the resulting product had the same properties as the product in Example 1.

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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)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé de fabrication d'agents nettoyants et détergents granulaires, de densité apparente élevée, par compression sous forme de produit extrudé sur des moules à perforations, et fragmentation subséquente de l'extrudat au moyen d'un dispositif de coupe, procédé dans lequel on vise à améliorer l'incorporation de composants liquides hydrophobes. Ce but est atteint en effectuant l'encapsulation du liquide hydrophobe dans de la dextrine.
PCT/EP1999/009838 1998-12-21 1999-12-11 Liquides hydrophobes confectionnes sous presentation solide pour utilisation dans des agents nettoyants et detergents de densite apparente elevee. WO2000037594A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP99962252A EP1141184A2 (fr) 1998-12-21 1999-12-11 Liquides hydrophobes confectionnes sous presentation solide pour utilisation dans des agents nettoyants et detergents de densite apparente elevee.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19858807.0 1998-12-21
DE1998158807 DE19858807A1 (de) 1998-12-21 1998-12-21 In fester Form konfektionierte hydrophobe Flüssigkeiten für den Einsatz in Wasch- und Reinigungsmitteln mit hohem Schüttgewicht

Publications (2)

Publication Number Publication Date
WO2000037594A2 true WO2000037594A2 (fr) 2000-06-29
WO2000037594A3 WO2000037594A3 (fr) 2000-12-07

Family

ID=7891797

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1999/009838 WO2000037594A2 (fr) 1998-12-21 1999-12-11 Liquides hydrophobes confectionnes sous presentation solide pour utilisation dans des agents nettoyants et detergents de densite apparente elevee.

Country Status (3)

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EP (1) EP1141184A2 (fr)
DE (1) DE19858807A1 (fr)
WO (1) WO2000037594A2 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004042933A1 (de) * 2004-09-02 2006-03-23 Henkel Kgaa In fester Form konfektionierte Flüssigkeiten für den Einsatz in teilchenförmigen Wasch- und Reinigungsmitteln

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1207777A (en) * 1968-03-29 1970-10-07 Unilever Ltd Detergents
DE2416219A1 (de) * 1973-04-13 1974-11-14 American Cyanamid Co Shampoo-cremespuelungs-mittel
WO1994019449A1 (fr) * 1993-02-22 1994-09-01 Quest International B.V. Composition resistante a l'humidite
EP0684301A2 (fr) * 1994-04-28 1995-11-29 The Procter & Gamble Company Composition détergente granulaire
US5498378A (en) * 1993-11-12 1996-03-12 Lever Brothers Company, Division Of Conopco, Inc. Process for preparing capsules with structuring agents
DE19545725A1 (de) * 1995-12-07 1997-06-12 Henkel Kgaa Verfahren zur Herstellung von wasch- oder reinigungsaktiven Extrudaten
GB2335434A (en) * 1998-03-19 1999-09-22 Mcbride Robert Ltd Encapsulated liquid incorporation in tableted compositions
WO1999054431A1 (fr) * 1998-04-22 1999-10-28 Henkel Kommanditgesellschaft Auf Aktien Constituants detersifs enrobes

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0684984B2 (fr) * 1993-02-22 2001-02-21 Quest International B.V. Composition resistante a l'humidite

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1207777A (en) * 1968-03-29 1970-10-07 Unilever Ltd Detergents
DE2416219A1 (de) * 1973-04-13 1974-11-14 American Cyanamid Co Shampoo-cremespuelungs-mittel
WO1994019449A1 (fr) * 1993-02-22 1994-09-01 Quest International B.V. Composition resistante a l'humidite
US5498378A (en) * 1993-11-12 1996-03-12 Lever Brothers Company, Division Of Conopco, Inc. Process for preparing capsules with structuring agents
EP0684301A2 (fr) * 1994-04-28 1995-11-29 The Procter & Gamble Company Composition détergente granulaire
DE19545725A1 (de) * 1995-12-07 1997-06-12 Henkel Kgaa Verfahren zur Herstellung von wasch- oder reinigungsaktiven Extrudaten
GB2335434A (en) * 1998-03-19 1999-09-22 Mcbride Robert Ltd Encapsulated liquid incorporation in tableted compositions
WO1999054431A1 (fr) * 1998-04-22 1999-10-28 Henkel Kommanditgesellschaft Auf Aktien Constituants detersifs enrobes

Also Published As

Publication number Publication date
DE19858807A1 (de) 2000-06-29
WO2000037594A3 (fr) 2000-12-07
EP1141184A2 (fr) 2001-10-10

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