EP3722404B1 - Composition solide contenant du parfum - Google Patents

Composition solide contenant du parfum Download PDF

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Publication number
EP3722404B1
EP3722404B1 EP19168924.9A EP19168924A EP3722404B1 EP 3722404 B1 EP3722404 B1 EP 3722404B1 EP 19168924 A EP19168924 A EP 19168924A EP 3722404 B1 EP3722404 B1 EP 3722404B1
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EP
European Patent Office
Prior art keywords
composition
formula
water
oil
weight
Prior art date
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EP19168924.9A
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German (de)
English (en)
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EP3722404A1 (fr
Inventor
Tobias Segler
Thomas Holderbaum
Michael Voelker
Hans-Joachim Schmidt
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Priority to EP19168924.9A priority Critical patent/EP3722404B1/fr
Priority to US16/846,486 priority patent/US11274269B2/en
Publication of EP3722404A1 publication Critical patent/EP3722404A1/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
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50Perfumes
    • C11D3/502Protected perfumes
    • C11D3/505Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay
    • 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
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2086Hydroxy carboxylic acids-salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2093Esters; Carbonates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/227Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin with nitrogen-containing groups

Definitions

  • the present invention relates to a solid, particulate composition
  • a solid, particulate composition comprising at least one water-soluble carrier material, at least one rheology modifier and at least one fragrance
  • the carrier material being a water-containing salt (hydrate) whose water vapor partial pressure at a specific temperature is in the range from 30 to 100°C corresponds to the H 2 O partial pressure of the saturated solution of this salt, so that the salt melts in its own crystal water at this temperature.
  • the invention relates to methods for producing the solid composition and to a washing or cleaning agent that contains the solid composition.
  • the present invention also relates to the use of such a washing or cleaning agent for cleaning textiles or hard surfaces and corresponding methods for cleaning textiles or hard surfaces using such a washing or cleaning agent.
  • the DE19953503 A1 describes scented pearls containing derivatives of polysaccharides as carrier material.
  • DE102016219292 A1 discloses perfume-containing fusible bodies containing polyethylene glycol as carrier material.
  • the consumer When using detergents and cleaning agents, the consumer not only aims to wash, clean or care for the objects to be treated, but he also wants the treated objects, such as textiles, after treatment, for example after the laundry, smell pleasant. For this reason in particular, most commercially available detergents and cleaning agents contain fragrances.
  • Fragrances in the form of fragrance particles are often used either as an integral part of a washing or cleaning agent, or are metered into the washing drum in a separate form directly at the start of a wash cycle. In this way, the consumer can control the scent of the laundry to be washed through individual dosing.
  • the main component of such fragrance pastilles known in the prior art is typically a water-soluble or at least water-dispersible carrier polymer, such as polyethylene glycol (PEG), which serves as a vehicle for the integrated fragrances and which more or less completely dissolves in the washing liquor during the waxing process dissolves in order to release the fragrances contained and any other components in the wash liquor.
  • PEG polyethylene glycol
  • a melt is produced from the carrier polymer, which contains the other ingredients or these are then added, and the melt obtained is then fed to a shaping process during which it cools, solidifies and assumes the desired shape.
  • the known products have the disadvantage that the polymer materials used, in particular PEG, have a delayed solubility, which is particularly important for short wash cycles, low temperature or other unfavorable conditions can lead to residues on the laundry or in the washing machine.
  • an alternative composition which shows a suitable processing range and at the same time has improved water solubility in the usual temperature ranges in which work is carried out, can be provided by using a water-containing salt ( hydrate) is used, the water vapor partial pressure of which at a certain temperature in the range from 30 to 100°C corresponds to the H 2 O partial pressure of the saturated solution of this salt at the same temperature, so that the salt dissolves in its own crystal water at this temperature, a process which can be described phenomenologically as melting, but which is thermodynamically a solution process.
  • the use of sodium acetate trihydrate is particularly advantageous.
  • These specific carrier materials are preferably processed by means of a process during which the salts are prepared as melts and then dropped onto a cooling belt, for example using a nozzle, on which they solidify and assume a final geometric shape.
  • a process during which the salts are prepared as melts and then dropped onto a cooling belt, for example using a nozzle, on which they solidify and assume a final geometric shape.
  • the yield point is measured using a rotational rheometer (AR G2 from TA Instruments or a "Kinexus” from Malvern), using a plate-plate measuring system with a diameter of 40 mm and a plate spacing of 1.1 mm.
  • the yield point is determined in a step-flow procedure in which the shear stress is increased quasi-statically, i.e. while waiting for the equilibrium deformation or stationary flow, from the lowest possible value to a value above the yield point.
  • the deformation is plotted against the shear stress in a double logarithmic diagram. If there is a yield point, the curves obtained in this way show a characteristic kink. Below the kink, only elastic deformation takes place.
  • the slope of the curve in the double logarithmic representation is one. Above the kink, the slope of the curve increases abruptly and steady flow occurs. The shear stress value of the kink corresponds to the yield point. If the kink is not very sharp, the point of intersection of the tangents of the two curve sections can be used to determine the yield point. For liquids that do not have a yield point, the graph described above is usually curved to the right.
  • the at least one carrier material is used in an amount such that the resulting melted body, ie the scented pastille, contains from 30 to 95% by weight, preferably from 40 to 90% by weight, for example 45 to 90% by weight, based on the total weight of the fused body containing support material.
  • the solid, particulate composition as described herein is prepared from a solution of the carrier material in the water/crystal water contained in the composition, the term “melt” also being used here for such a solution, in contrast to the established usage, to describe the state in which the carrier material dissolves in its own water of crystallization due to the elimination of water and thus forms a liquid.
  • the term “melt”, as used herein, thus designates the liquid state of the composition, which occurs when the temperature is exceeded at which the carrier material splits off water of crystallization and then dissolves in the water contained in the composition.
  • the corresponding dispersion, which contains the (solid) substances described herein dispersed in the melt of the carrier material is therefore also a subject of the invention. So when reference is made below to the solid, particulate composition, the corresponding melt/melt dispersion from which it can be obtained is always included. Since these do not differ in composition, with the exception of the physical state, the terms are used synonymously here.
  • fused body is used herein to describe the solid particles obtainable from the liquid composition upon cooling by solidification/transformation.
  • the main component of the particulate, solid composition as described herein is at least one water-soluble carrier material.
  • the at least one carrier material is characterized in that it is selected from water-containing salts whose water vapor partial pressure at a temperature in the range from 30 to 100° C. corresponds to the H 2 O partial pressure of the saturated solution of this salt at the same temperature.
  • the corresponding water-containing salt also referred to herein as "hydrate” dissolves in its own water of crystallization when this temperature is reached or exceeded and thereby changes from a solid to a liquid state of aggregation.
  • the carrier materials according to the invention preferably show this behavior at a temperature in the range from 40 to 90.degree. C., particularly preferably between 50 and 85.degree. C., even more preferably between 55 and 80.degree.
  • the water-soluble carrier materials from the group of hydrous salts described above include, in particular, sodium acetate trihydrate (Na(CH 3 COO) 3H 2 O), Glauber's salt (Na 2 SO 4 10H 2 O), trisodium phosphate dodecahydrate (Na 3 PO 4 x 12 H 2 O) and the strontium chloride hexahydrate (SrCl 2 x 6 H 2 O).
  • sodium acetate trihydrate Na(CH 3 COO) ⁇ 3H 2 O
  • Glauber's salt Na 2 SO 4 10H 2 O
  • trisodium phosphate dodecahydrate Na 3 PO 4 x 12 H 2 O
  • strontium chloride hexahydrate strontium chloride hexahydrate
  • the sodium acetate trihydrate (Na(CH 3 COO) ⁇ 3H 2 O) is particularly preferred.
  • the particulate composition is characterized by its content of sodium acetate trihydrate
  • those compositions which contain sodium acetate trihydrate in an amount of from 30 to 95% by weight, preferably from 40 to 90% by weight are particularly advantageous with regard to their ability to be produced, processed and handled %, especially from 45 to 90% by weight based on the total weight of the composition.
  • a particularly suitable hydrate is sodium acetate trihydrate (Na(CH 3 COO).3H 2 O), since it dissolves in its own water of crystallization in the particularly preferred temperature range of 55 to 80° C., specifically at about 58° C.
  • the sodium acetate trihydrate can be used directly as such, but alternatively the use of anhydrous sodium acetate in combination with free water is also possible, the trihydrate then being formed in situ .
  • the water is used in less than or more than the stoichiometric amount based on the amount necessary to convert all of the sodium acetate to sodium acetate trihydrate, preferably in an amount of at least 60% by weight, preferably at least 70% by weight %, more preferably at least 80%, most preferably 90%, 100% or more by weight of the amount theoretically required to convert all the sodium acetate to sodium acetate trihydrate (Na(CH 3 COO) ⁇ 3H 2 O).
  • the more than stoichiometric use of water is particularly preferred.
  • the particulate composition is characterized by its sodium acetate content
  • those compositions which contain sodium acetate in an amount of from 18 to 57% by weight, preferably from 24 to 48% by weight, are particularly advantageous with regard to their ability to be produced, processed and handled. in particular from 27 to 45% by weight based on the total weight of the composition.
  • the solid particulate compositions contain a fragrance b) as a second essential component.
  • the percentage by weight of the perfume in the total weight of the composition is preferably from 1 to 15% by weight, more preferably from 3 to 12% by weight.
  • a fragrance is a chemical substance that stimulates the sense of smell.
  • the chemical substance should be at least partially airborne, i.e. the fragrance should be at least slightly volatile at 25°C. If the fragrance is now very volatile, the odor intensity then quickly fades away. With a lower volatility, however, the odor impression is more lasting, i.e. it does not disappear as quickly.
  • the fragrance therefore has a melting point in the range from -100°C to 100°C, preferably from -80°C to 80°C, more preferably from -20°C to 50°C, in particular from - 30°C to 20°C.
  • the fragrance has a boiling point which is in the range from 25° C. to 400° C., preferably from 50° C. to 380° C., more preferably from 75° C. to 350° C., in particular from 100° C. to 330°C.
  • the fragrance has a molecular mass of 40 to 700 g/mol, more preferably 60 to 400 g/mol.
  • fragrance The smell of a fragrance is perceived as pleasant by most people and often corresponds to the smell of, for example, blossoms, fruits, spices, bark, resin, leaves, grass, moss and roots. Fragrances can also be used to mask unpleasant odors or to provide a non-smelling substance with a desired smell.
  • Individual fragrance compounds for example synthetic products of the ester, ether, aldehyde, ketone, alcohol and hydrocarbon type, can be used as fragrances.
  • Perfume compounds of the aldehyde type are, for example, adoxal (2,6,10-trimethyl-9-undecenal), anisaldehyde (4-methoxybenzaldehyde), cymal (3-(4-isopropyl-phenyl)-2-methylpropanal), ethylvanillin, florhydral ( 3-(3-isopropylphenyl)butanal), Helional (3-(3,4-methylenedioxyphenyl)-2-methylpropanal), Heliotropin, Hydroxycitronellal, Lauraldehyde, Lyral (3- and 4-(4-Hydroxy-4-methylpentyl)- 3-cyclohexene-1-carboxaldehyde), methyl nonylacetaldehyde, Lilial (3-(4-tert-butylphenyl)-2-methylpropanal), phenylacetaldehyde, undecylene aldehyde, vanillin
  • Perfume compounds of the ketone type are, for example, methyl beta-naphthyl ketone, musk indanone (1,2,3,5,6,7-hexahydro-1,1,2,3,3-pentamethyl-4H-inden-4-one), Tonalide (6-acetyl-1,1,2,4,4,7-hexamethyltetralin), alpha-damascone, beta-damascone, delta-damascone, iso-damascone, damascenone, methyldihydrojasmonate, menthone, carvone, camphor, koavone (3rd ,4,5,6,6-pentamethylhept-3-en-2-one), fenchone, alpha-lonone, beta-lonone, gamma-methyl-ionone, fleuramon (2-heptylcyclopentanone), dihydrojasmon, cis-jasmon , iso-E-
  • Perfume compounds of the alcohol type are, for example, 10-undecen-1-ol, 2,6-dimethylheptan-2-ol, 2-methylbutanol, 2-methylpentanol, 2-phenoxyethanol, 2-phenylpropanol, 2-tert-butylcyclohexanol, 3,5,5-trimethylcyclohexanol, 3-hexanol, 3-methyl-5-phenylpentanol, 3-octanol, 3-phenylpropanol, 4-heptenol, 4-isopropylcyclohexanol, 4-tert-butylcyclohexanol, 6 ,8-dimethyl-2-nona-nol, 6-nonen-1-ol, 9-decen-1-ol, ⁇ -methylbenzyl alcohol, ⁇ -terpineol, amyl salicylate, benzyl alcohol, benzyl salicylate, ⁇ -terpineol,
  • Perfume compounds of the ester type are, for example, benzyl acetate, phenoxyethyl isobutyrate, p-tert-butylcyclohexyl acetate, linalyl acetate, dimethylbenzylcarbinyl acetate (DMBCA), phenylethyl acetate, benzyl acetate, ethylmethylphenylglycinate, allylcyclohexylpropionate, styrallylpropionate, benzyl salicylate, cyclohexyl salicylate, floramat, melusate and jasmacyclate.
  • DMBCA dimethylbenzylcarbinyl acetate
  • benzyl acetate ethylmethylphenylglycinate
  • allylcyclohexylpropionate styrallylpropionate
  • benzyl salicylate cyclohexyl salicylate,
  • the ethers include, for example, benzyl ethyl ether and ambroxan.
  • the hydrocarbons mainly include terpenes such as limonene and pinene.
  • fragrance oils are preferably used, which together produce an appealing fragrance.
  • Such a mixture of fragrances can also be referred to as a perfume or perfume oil.
  • Perfume oils of this kind can also contain natural mixtures of fragrances, such as are obtainable from vegetable sources.
  • Fragrances of plant origin include essential oils such as angelica root oil, anise oil, arnica flower oil, basil oil, bay oil, champaca flower oil, citrus oil, fir oil, fir cone oil, elemi oil, eucalyptus oil, fennel oil, pine needle oil, galbanum oil, geranium oil, ginger grass oil, guaiac wood oil, gurjun balm oil, helichrysum oil, ho oil , ginger oil, iris oil, jasmine oil, cajeput oil, sweet flag oil, chamomile oil, camphor oil, kanaga oil, cardamom oil, cassia oil, pine needle oil, copaiva balm oil, coriander oil, spearmint oil, caraway oil, cumin oil, labdanum oil, lavender oil, lemongrass oil, Linden blossom oil, lime oil, tangerine oil, lemon balm oil, mint oil, musk seed oil, muscatel oil, myrrh oil, clove oil, neroli oil,
  • the active substance c in particular the fragrance.
  • at least part of the fragrance is used in encapsulated form (fragrance capsules), in particular in microcapsules.
  • the entire fragrance can also be used in encapsulated form.
  • the microcapsules can be water-soluble and/or water-insoluble microcapsules.
  • melamine-urea-formaldehyde microcapsules, melamine-formaldehyde microcapsules, urea-formaldehyde microcapsules or starch microcapsules can be used.
  • Pro-fragrance refers to compounds that only release the actual fragrance after chemical conversion/cleavage, typically upon exposure to light or other environmental conditions such as pH, temperature, etc. Such compounds are often also referred to as fragrance storage substances or “pro-fragrance”.
  • the fragrance is selected from the group of perfume oils and fragrance capsules.
  • the use of a combination of perfume oil and fragrance capsules is very particularly preferred.
  • the solid particulate composition contains a rheology modifier from the group of heteroglycans as a third essential component.
  • the proportion by weight of the rheology modifier to the total weight of the composition is preferably from 1 to 2.5% by weight, more preferably from 1.2 to 2.0% by weight.
  • Heteroglycans are polysaccharides that are made up of more than one type of monomeric simple sugar.
  • heteroglycans of bacterial origin has proven to be technically particularly advantageous.
  • Corresponding heteroglycans can be obtained, for example, by bacterial fermentation.
  • the heteroglycan is an exopolysaccharide.
  • Heteroglycans functionalized with at least one non-saccharidic group, preferably with at least one non-saccharidic group selected from acetate, pyruvate, phosphate and succinate, are preferred for reasons of manufacturability, confectionability, handling and metering of the solid, particulate composition.
  • Compounds with the INCI designation succinoglycan are very particularly preferred as rheology modifiers.
  • the optional components (d) and (e) are preferably present independently of one another in amounts of up to 20% by weight, more preferably up to 18% by weight, in particular up to 15% by weight, based on the total weight of the composition.
  • shaped bodies containing active substances include colorants, preservatives, bitter substances or buffer systems.
  • these preferably comprise at least one dye. It is preferred that the moldings at least a water-soluble dye, most preferably a water-soluble polymer dye.
  • a water-soluble dye most preferably a water-soluble polymer dye.
  • Such dyes are known in the art and are typically used in concentrations of 0.001 to 0.5% by weight, preferably 0.01 to 0.3% by weight, based on the total weight of the composition.
  • Preferred dyes should have a high storage stability and be insensitive to the other ingredients of the detergent or cleaning agent and to light and not have any pronounced substantivity to textile fibers so as not to stain them.
  • the dye is a customary dye that can be used for different detergents or cleaning agents.
  • the dye is selected from Acid Red 18 (Cl 16255), Acid Red 26, Acid Red 27, Acid Red 33, Acid Red 51, Acid Red 87, Acid Red 88, Acid Red 92, Acid Red 95, Acid Red 249 ( Cl 18134), Acid Red 52 (Cl 45100), Acid Violet 126, Acid Violet 48, Acid Violet 54, Acid Yellow 1, Acid Yellow 3 (Cl 47005), Acid Yellow 11, Acid Yellow 23 (Cl 19140), Acid Yellow 3, Direct Blue 199 (Cl 74190), Direct Yellow 28 (Cl 19555), Food Blue 2 (Cl 42090), Food Blue 5:2 (Cl 42051:2), Food Red 7(01 16255), Food Yellow 13 ( Cl 47005), Food Yellow 3 (Cl 15985), Food Yellow 4 (Cl 19140), Reactive Green 12, Solvent Green 7 (Cl 59040).
  • Particularly preferred dyes are water-soluble acid dyes, for example Food Yellow 13 (Acid Yellow 3, Cl 47005), Food Yellow 4 (Acid Yellow 23, Cl 19140), Food Red 7 (Acid Red 18, Cl 16255), Food Blue 2 (Acid Blue 9, Cl 42090), Food Blue 5 (Acid Blue 3, Cl 42051), Acid Red 249 (Cl 18134), Acid Red 52 (Cl 45100), Acid Violet 126, Acid Violet 48, Acid Blue 80(01 61585), Acid Blue 182, Acid Blue 182, Acid Green 25 (Cl 61570), Acid Green 81.
  • Food Yellow 13 Acid Yellow 3, Cl 47005
  • Food Yellow 4 Acid Yellow 23, Cl 19140
  • Food Red 7 Acid Red 18, Cl 16255
  • Food Blue 2 Acid Blue 9, Cl 42090
  • Food Blue 5 Acid Blue 3, Cl 42051
  • Acid Red 249 Cl 18134
  • Acid Red 52 Cl 45100
  • Acid Violet 126 Acid Violet 48
  • Acid Blue 80(01 61585) Acid Blue 182
  • Acid Blue 182 Acid Green 25 (C
  • Water-soluble direct dyes for example Direct Yellow 28 (CI 19555), Direct Blue 199 (CI 74190) and water-soluble reactive dyes, for example Reactive Green 12, and the dyes Food Yellow 3 (CI 15985), Acid Yellow 184 are also preferably used.
  • Aqueous dispersions of the following pigment dyes are also preferably used: Pigment Black 7 (Cl 77266), Pigment Blue 15 (Cl 74160), Pigment Blue 15:1 (Cl 74160), Pigment Blue 15:3 (Cl 74160), Pigment Green 7 (Cl 74260), Pigment Orange 5, Pigment Red 112 (Cl 12370), Pigment Red 112 (Cl 12370), Pigment Red 122 (Cl 73915), Pigment Red 179 (Cl 71130), Pigment Red 184 (Cl 12487), Pigment Red 188 (Cl 12467), Pigment Red 4 (Cl 12085), Pigment Red 5 (Cl 12490), Pigment Red 9, Pigment Violet 23 (Cl 51319), Pigment Yellow 1 (Cl 28 11680), Pigment Yellow 13 (Cl 21100 ), Pigment Yellow 154, Pigment Yellow 3 (Cl 11710), Pigment Yellow 74, Pigment Yellow 83 (Cl 21108), Pigment Yellow 97.
  • pigment dyes are used in the form of dispersions: Pigment Yellow 1 (Cl 11680), Pigment Yellow 3 (Cl 11710), Pigment Red 112 (Cl 12370), Pigment Red 5 (Cl 12490), Pigment Red 181 (Cl 73360), Pigment Violet 23 (Cl 51319), Pigment Blue 15:1 (Cl 74160), Pigment Green 7 (Cl 74260), Pigment Black 7 (Cl 77266).
  • water-soluble polymer dyes for example Liquitint, Liquitint Blue HP, Liquitint Blue MC, Liquitint Blue 65, Liquitint Cyan 15, Liquitint Patent Blue, Liquitint Violet 129, Liquitint Royal Blue, Liquitint Experimental Yellow 8949-43, Liquitint Green HMC, Liquitint Yellow LP, Liquitint Yellow II and mixtures thereof are used.
  • the group of very particularly preferred dyes includes Acid Blue 3, Acid Yellow 23, Acid Red 33, Acid Violet 126, Liquitint Yellow LP, Liquitint Cyan 15, Liquitint Blue HP and Liquitint Blue MC.
  • bitter substances primarily serves to avoid oral intake of the shaped bodies containing active substances.
  • Preferred shaped bodies contain at least one bitter substance in an amount of 0.0001 to 0.05% by weight, based on the total weight of the composition. Amounts of from 0.0005 to 0.02% by weight are particularly preferred. According to the present invention, preference is given in particular to those bitter substances which are soluble in water at 20° C. to an extent of at least 5 g/l. With regard to an undesirable interaction with the fragrance components also contained in the composition, in particular a change in the fragrance perceived by the consumer, the ionic bitter substances have proven to be superior to the non-ionic, ionic bitter substances consisting of organic(s) cation(s) and organic (n) anion(s), are therefore preferred for the composition according to the invention.
  • the at least one bitter substance is therefore an ionic bitter substance.
  • quaternary ammonium compounds which contain an aromatic group both in the cation and in the anion are outstandingly suitable.
  • the at least one bitter substance is therefore a quaternary ammonium compound.
  • a suitable quaternary ammonium compound is, for example, without limitation, benzyl diethyl ((2,6- xylylcarbamoyl )methyl)ammonium benzoate commercially available, for example, under the trademarks Bitrex® and Indigestin®. This compound is also known under the name Denatonium Benzoate.
  • the at least one bitter substance is benzyl diethyl ((2,6-xylylcarbamoyl)methyl)ammonium benzoate (Bitrex ® ). If Bitrex ® is used, proportions by weight of 0.0001 to 0.05% by weight preferred. The information is based on the active substance content and the total weight.
  • the composition also contains at least one buffer system as defined above.
  • the buffer system is preferably solid, i.e. is a solid (mixture) under standard conditions.
  • the term "buffering capacity” here refers to the amount of hydrogen chloride (HCl) in mg necessary to raise the pH of a solution of 1 g of the solid composition in 50 g of deionized water under standard conditions (20°C, 1013 mbar). to drop below 6.75.
  • the buffer systems used according to the invention are preferably characterized in that they have a pKa value of at least 5.75, preferably at least 6.25, more preferably at least 6.75, and preferably not more than 12, more preferably less than 11.5, more preferably 11 or less, most preferably 10.5 or less.
  • the buffering capacity of the resulting solution is preferably at least 2 mg HCl/g composition, preferably at least 3 mg HCl/g composition, more preferably at least 4 mg HCl/g composition.
  • Suitable buffering agents include, without limitation, sodium bicarbonate, sodium carbonate, disodium hydrogen phosphate, sodium glutamate, sodium aspartate, tris(hydroxymethyl)aminomethane (TRIS), and other organic and inorganic buffering agents known in the art that meet the above criteria, and mixtures of the foregoing. TRIS is particularly preferred.
  • the buffer substances are used in the compositions according to the invention, for example in amounts of 0.1 to 10% by weight, preferably 0.5 to 7.5% by weight, more preferably 1 to 5% by weight, in each case based on the total weight of the composition and are preferably selected from sodium bicarbonate, sodium carbonate, disodium hydrogen phosphate, sodium glutamate, sodium aspartate, tris(hydroxymethyl)aminomethane (TRIS) and combinations thereof.
  • the composition is preferably free of room temperature (25°C) solid polyethylene glycol (PEG) in the form of a coating, more preferably the composition is free of room temperature (25°C) solid PEG overall, ie the room temperature (25°) solid content PEG is less than 1% by weight of the composition.
  • PEG room temperature
  • compositions according to the invention are distinguished from the known compositions of the prior art by an improved solubility profile and an improved fragrance effect.
  • these compositions tend to vary depending on the exact manufacturing and/or storage constraints to unaesthetic "salt efflorescence" on their surface. These changes in the particle surface impair the appearance of compositions containing dyes in particular. A further task was therefore to prevent or at least reduce this efflorescence by means of formulation measures.
  • compositions according to the invention contain at least one water-miscible organic solvent as a further essential component.
  • the water-miscible organic solvents are preferably not very volatile and odorless. Suitable water-miscible organic solvents are, for example, monohydric and polyhydric alcohols, alkyl ethers, di- or low molecular weight polyalkylene ethers which are liquid at room temperature.
  • the solvents are preferably selected from ethanol, n-propanol, i-propanol, butanols, glycol, propanediol, butanediol, methylpropanediol, diglycol, butyl diglycol, hexylene glycol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol propyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol methyl ether, diethylene glycol ethyl ether, propylene glycol methyl ether, Propylene glycol ethyl ether, propylene glycol propyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, methoxytriglycol, ethoxytriglycol, butoxytriglycol, 1-butoxyethoxy-2-propanol, 3-methyl-3-methoxybutanol, prop
  • Dipropylene glycol, 1,2-propylene glycol and glycerol are particularly preferred, since these are particularly miscible with water and do not otherwise enter into any adverse reactions with the other components of the composition.
  • Dipropylene glycol is particularly preferred.
  • the proportion by weight of the water-miscible organic solvent in the total weight of the composition is preferably 0.1 to 20% by weight, preferably 0.1 to 10% by weight, particularly preferably 0.5 to 8% by weight and in particular 1 to 6% by weight %.
  • the composition may also contain free water.
  • free water refers to water which is not bound as water of crystallization in any of the salts contained in the composition.
  • the solid, particulate composition can have any shape. However, for reasons of manufacturability, fabrication, handling and dosability, preference is given to spherical, figured, scaly, cuboid, cylindrical, conical, spherical cap or lenticular, hemispherical, disk or needle shaped particles. Exemplary particles may have a gummy bear-like figural configuration. Due to their packaging properties and their performance profile, hemispherical particles are particularly preferred.
  • the composition consists of at least 20% by weight, preferably at least 40% by weight, particularly preferably at least 60% by weight and particularly preferably at least 80% by weight, of particles which in each have a spatial extent of between 0.5 to 10 mm, in particular 0.8 to 7 mm and particularly preferably 1 to 5 mm, in any spatial direction.
  • the composition consists of at least 20% by weight, preferably at least 40% by weight, particularly preferably at least 60% by weight and particularly preferably at least 80% by weight, of particles in which the Ratio of the longest particle diameter determined in any spatial direction to the shortest diameter determined in any spatial direction between 3:1 and 1:1, preferably between 2.5:1 and 1.2:1 and in particular between 2.2:1 and 1, is 4:1.
  • the weight of the solid particles in the composition can also vary within wide limits. With regard to the producibility and dosing properties, however, such compositions have proven to be advantageous which contain at least 20% by weight, preferably at least 40% by weight, particularly preferably at least 60% by weight and particularly preferably at least 80% by weight.
  • -% consists of particles which have a particle weight between 2 and 150 mg, preferably between 8 and 120 mg and in particular between 20 and 100 mg.
  • the composition is primarily suitable for scenting textiles.
  • the use of the solid composition as a textile care product for scenting textile fabrics is therefore a further aspect of this application.
  • the solid particulate composition can be marketed or used alone or in combination with another preparation.
  • the solid particulate composition is part of a washing or cleaning agent.
  • a composition as described herein can be used, for example, in the wash cycle of a laundry cleaning process and thus transport the perfume to the laundry right at the start of the washing process. Furthermore, the composition is simpler and easier to handle than liquid compositions, since no droplets remain on the edge of the bottle, which lead to edges on the substrate or to unsightly deposits in the area of the closure when the bottle is subsequently stored. The same applies in the event accidental spillage of composition during dosing. The spilled amount can also be cleaned up more easily and cleanly.
  • a method for treating textiles, in the course of which a composition according to the invention or a detergent or cleaning agent which comprises such a composition, is metered into the wash liquor of a textile washing machine is a further subject of this application.
  • composition of some preferred compositions can be found in the tables below (data in % by weight based on the total weight of the agent, unless stated otherwise).
  • the composition according to the present invention is a solid, particulate composition.
  • the individual particles of the composition can be referred to as melted bodies which are solid at room temperature and temperatures of up to 30.degree. C., preferably up to 40.degree.
  • the melting bodies according to the invention are coated.
  • Tablet coatings known from the pharmaceutical literature, for example, are suitable as coating agents.
  • the lozenges can also be waxed, i.e. coated with a wax, or powdered with a powdery material, for example a release agent, to prevent caking (agglomeration). It is preferred that the coating does not consist of PEG or that it comprises a significant amount (>10% by weight, based on the coating).
  • the melt dispersion produced in step a) is discharged from the first container by means of a pipeline and fed to the droplet former. It is furthermore preferred that the fragrance is introduced continuously into the outflow stream of the first container by means of a further pipeline from a corresponding storage container.
  • a liquid preparation of the fragrance for example in the form of a fragrance, is particularly suitable for this purpose a solution.
  • the temperature of the fragrance or the liquid preparation of the fragrance before it is introduced into the outflow stream of the first container is preferably at least 10° C., preferably at least 20° C. and in particular at least 30° C. below the temperature of the melt dispersion forming the outflow stream.
  • the mixing preferably takes place by means of a static mixer which is located in the pipeline in the direction of flow of the melt dispersion after the point of entry of the fragrance and before the point of entry of the mixture into the droplet former.
  • the length of the static mixer fitted in the pipeline in the direction of flow of the melt dispersion is preferably at least 10 times, preferably at least 20 times and in particular at least 50 times the diameter of the pipeline.
  • the distance between the end of the static mixer and the entry point of the pipeline into the drop former is less than 500 times, preferably less than 200 times and in particular less than 100 times the diameter of the pipeline.
  • the diameter of the pipeline is its inner diameter without taking the wall thickness into account.
  • the mixture of melt dispersion and fragrance enters the droplet former with a rotating, perforated outer drum from the pipeline.
  • the section of tubing that is inside the drum of the gob former is referred to below as the feed duct to distinguish it from the previous tubing.
  • the feed channel preferably extends over at least 80%, particularly preferably over at least 90% and in particular over 100% of the length of the drum of the gob former.
  • the mixture introduced into the feed channel exits the feed channel preferably through bores located on the underside of the feed channel from the feed channel onto a distributor or nozzle bar, which in turn bears against the inside of the rotating, perforated outer drum.
  • the mixture runs through the distributor or nozzle bar and is then discharged from the holes in the rotating outer drum onto a steel belt below these holes.
  • the distance between the outside of the rotating, perforated outer drum and the surface of the steel strip is preferably between 5 and 20 mm.
  • a further mixer can be arranged in the feed channel.
  • This is preferably a dynamic mixer, for example a spiral arranged rotatably within the feed channel.
  • the dwell time of the mixture of melt dispersion and fragrance in the pipeline until it emerges from the rotating, perforated outer drum of the drop former is preferably less than 20 seconds, particularly preferably less than 10 seconds and in particular between 0.5 and 5 seconds.
  • the viscosity (Texas Instruments AR-G2 rheometer; plate/plate, 4 cm diameter, 1100 ⁇ m gap; shear rate 10/1 sec) of the mixture when it emerges from the rotating, perforated external drum is preferably between 1000 and 10000 mPas.
  • the droplets of the mixture discharged from the droplet former are solidified on the steel belt to form solid melted bodies.
  • the time between the dropping of the mixture onto the steel strip and the complete solidification of the mixture is preferably between 5 and 60 seconds, particularly preferably between 10 and 50 seconds and in particular between 20 and 40 seconds.
  • the solidification of the mixture is preferably supported and accelerated by cooling.
  • the droplets applied to the steel strip can be cooled directly or indirectly. Cooling by means of cold air, for example, can be used as direct cooling. However, indirect cooling of the droplets by cooling the underside of the steel strip with cold water is preferred.
  • compositions E1 E2 E3 Sodium Acetate (anhydrous) 53.0 53.0 53.0 water 34.8 34.8 34.8 succinoglycan 1.5 1.5 1.5 dipropylene glycol 1.7 1.7 1.7 Tris(hydroxymethyl)aminomethane (TRIS) 1.9 1.9 1.9 Perfume 6.96 1.86 Perfume capsule slurry (50%) 6.96 5.1 dye 0.1 0.1 0.1 bitterness 0.04 0.04 0.04
  • the sodium acetate was dissolved in water at a temperature of 70° C. with stirring. The other components were then incorporated. Pastilles were produced by dropping the liquid mixture (“melt”) onto a cooling plate maintained at room temperature (23° C.).

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Dispersion Chemistry (AREA)
  • Molecular Biology (AREA)
  • Detergent Compositions (AREA)
  • Fats And Perfumes (AREA)

Claims (10)

  1. Composition particulaire solide comprenant, par rapport au poids total de la composition,
    a) 20 à 95 % en poids d'au moins un matériau de support hydrosoluble choisi parmi les sels hydratés, dont la pression partielle de vapeur d'eau à une température déterminée dans la plage de 30 à 100 °C correspond à la pression partielle de H2O de la solution saturée dudit sel ;
    b) 0,1 à 20 % en poids d'au moins une substance odorante,
    c) 0,1 à 10 % en poids d'au moins un modificateur de rhéologie dans le groupe des hétéroglycanes, de préférence d'un type et d'une quantité tels qu'une masse fondue obtenue par chauffage de la composition à 70 °C présente une limite d'écoulement supérieure à 1 Pa, de préférence supérieure à 5 Pa et en particulier supérieure à 10 Pa ;
    d) éventuellement jusqu'à 25 % en poids d'un émulsifiant, de préférence d'un émulsifiant dans le groupe des alcools gras, des alkoxylates d'alcool gras, des éthoxylates d'alcool gras, des sulfates d'alcool gras, des éthersulfates d'alcool gras, des alkylbenzènesulfonates, des alkylpolyglycosides, des esters de sorbitane d'acide gras, des alkylamineoxydes, des alkylbétaines ou de leurs associations ;
    e) éventuellement jusqu'à 25 % en poids d'au moins une matière solide ou charge différente de (c) et (d) ; et
    f) éventuellement au moins un colorant.
  2. Composition selon la revendication 1, caractérisée en ce que le matériau de support hydrosoluble est choisi parmi les sels hydratés dont la pression partielle de vapeur d'eau à une température dans la plage de 40 à 90 °C, de préférence de 50 à 85 °C, plus préférablement de 55 à 80 °C, correspond à la pression partielle de H2O de la solution saturée dudit sel, de préférence est de l'acétate de sodium trihydraté (Na(CH3COO) · 3H2O).
  3. Composition selon l'une des revendications précédentes, caractérisée en ce que le matériau de support hydrosoluble est contenu en une quantité de 30 à 95 % en poids, de préférence de 40 à 90 % en poids, en particulier de 45 à 90 % en poids, par rapport au poids total de la composition dans laquelle il est contenu.
  4. Composition selon l'une des revendications précédentes, caractérisée en ce que l'au moins une substance odorante est contenue dans la composition en une quantité de 1 à 20 % en poids, de préférence de 1 à 15 % en poids, plus préférablement de 3 à 12 % en poids.
  5. Composition selon l'une des revendications précédentes, caractérisée en ce que la composition, par rapport à son poids total, contient un modificateur de rhéologie dans le groupe des hétéroglycanes en une quantité de 1 à 2,5 % en poids, plus préférablement de 1,2 à 2,0 % en poids.
  6. Composition selon l'une des revendications précédentes, caractérisée en ce que la composition contient un hétéroglycane d'origine bactérienne en tant que modificateur de rhéologie.
  7. Composition selon l'une des revendications précédentes, caractérisée en ce que la composition contient un exopolysaccharide en tant que modificateur de rhéologie.
  8. Composition selon l'une des revendications précédentes, caractérisée en ce que la composition contient un composé de dénomination INCl « succinoglycane » en tant que modificateur de rhéologie.
  9. Utilisation de la composition solide selon l'une des revendications 1 à 8 en tant qu'agent d'entretien des textiles pour parfumer les tissus textiles.
  10. Procédé de fabrication de la composition selon l'une des revendications 1 à 8, comprenant
    a) la génération d'une masse fondue comprenant l'au moins un matériau de support hydrosoluble ;
    b) éventuellement l'addition dosée d'autres ingrédients facultatifs ;
    c) l'addition dosée de l'au moins une substance odorante, de l'au moins un modificateur de rhéologie et éventuellement d'un colorant à la masse fondue ;
    d) le mélange de la masse fondue et de l'au moins une substance odorante ; et
    e) le refroidissement et éventuellement le façonnage du mélange afin d'obtenir des corps fusibles contenant du parfum.
EP19168924.9A 2019-04-12 2019-04-12 Composition solide contenant du parfum Active EP3722404B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP19168924.9A EP3722404B1 (fr) 2019-04-12 2019-04-12 Composition solide contenant du parfum
US16/846,486 US11274269B2 (en) 2019-04-12 2020-04-13 Solid fragrance-containing composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP19168924.9A EP3722404B1 (fr) 2019-04-12 2019-04-12 Composition solide contenant du parfum

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EP3722404B1 true EP3722404B1 (fr) 2022-03-30

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Publication number Priority date Publication date Assignee Title
DE102019210894A1 (de) * 2019-07-23 2021-01-28 Henkel Ag & Co. Kgaa Parfümhaltiger Formkörper
US12077733B1 (en) 2023-05-24 2024-09-03 Tulco, L.P. Scent booster for laundry comprising a sodium bicarbonate/sodium acetate trihydrate mixture
US11834636B1 (en) * 2023-05-24 2023-12-05 Tufco, L.P. Scent booster comprising polyethylene glycol, sodium bicarbonate, and sodium acetate for laundry

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10058647A1 (de) * 2000-07-14 2002-05-29 Henkel Kgaa Kompartiment- Hohlkörper III

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Publication number Priority date Publication date Assignee Title
GB9807992D0 (en) * 1998-04-15 1998-06-17 Unilever Plc Water softening and detergent compositions
US6974789B1 (en) * 1999-01-23 2005-12-13 The Procter & Gamble Company Detergent tablet
DE19953503A1 (de) * 1999-11-06 2001-05-10 Henkel Kgaa Verfahren zur Herstellung von Duftperlen
EP1305396B1 (fr) * 2000-07-14 2005-11-02 Henkel Kommanditgesellschaft auf Aktien Corps creux compartimentes contenant une dose d'un produit de lavage, de nettoyage ou de rincage
DE10313458A1 (de) * 2003-03-25 2004-11-18 Henkel Kgaa Wasch- oder Reinigungsmittel
DE102016219292A1 (de) * 2016-09-26 2018-03-29 Henkel Ag & Co. Kgaa Schnelllösliche, parfümhaltige Schmelzkörper

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10058647A1 (de) * 2000-07-14 2002-05-29 Henkel Kgaa Kompartiment- Hohlkörper III

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US11274269B2 (en) 2022-03-15
US20200325421A1 (en) 2020-10-15

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