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EP1174493A1 - Pain de savon comprenant du talc, un ou plusieurs acides gras d'alkali et un ou plusieurs émollients en absence d'oligoglycosides d'alkyl - Google Patents

Pain de savon comprenant du talc, un ou plusieurs acides gras d'alkali et un ou plusieurs émollients en absence d'oligoglycosides d'alkyl Download PDF

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Publication number
EP1174493A1
EP1174493A1 EP01115784A EP01115784A EP1174493A1 EP 1174493 A1 EP1174493 A1 EP 1174493A1 EP 01115784 A EP01115784 A EP 01115784A EP 01115784 A EP01115784 A EP 01115784A EP 1174493 A1 EP1174493 A1 EP 1174493A1
Authority
EP
European Patent Office
Prior art keywords
fatty acids
soap
alcohols
weight
fatty
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
EP01115784A
Other languages
German (de)
English (en)
Other versions
EP1174493B1 (fr
Inventor
Andreas Lenuck
Jens Dr. Treu
Erich Karcher
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beiersdorf AG
Original Assignee
Beiersdorf AG
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
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Application filed by Beiersdorf AG filed Critical Beiersdorf AG
Publication of EP1174493A1 publication Critical patent/EP1174493A1/fr
Application granted granted Critical
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Anticipated expiration legal-status Critical
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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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/48—Superfatting agents
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/06—Inorganic compounds
    • C11D9/18—Water-insoluble compounds
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/24—Hydrocarbons
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/26—Organic compounds, e.g. vitamins containing oxygen

Definitions

  • Shaped soap product containing talc, one or more fatty acids in the form of their Alkaline soaps and one or more lipid-replenishing substances while absent of alkyl (oligo) glycosides
  • the present invention relates to cosmetic cleaning agents in the form of shaped soap products. Such means are known per se. It is essentially about surface-active substances or mixtures of substances that the consumer in different Preparations are offered.
  • the invention particularly relates to bar soaps with improved Smoothness and increased lime soap dispersing capacity due to the content of talc and one or more lipid-replenishing substances in the absence of alkyl (oligo) glycosides.
  • Surfactants best known are the alkali salts of higher fatty acids, i.e. the classic "soaps" - are amphiphilic substances, the organic non-polar substances in water can emulsify.
  • a simple water bath without the addition of surfactants is the first step swelling of the horny layer of the skin, the degree of this swelling being, for example, from depends on the duration of the bath and its temperature. At the same time, they become water-soluble Fabrics, e.g. water-soluble dirt components, but also the skin's own substances that are used for Water binding capacity of the horny layer are responsible, washed off or washed out.
  • water-soluble Fabrics e.g. water-soluble dirt components
  • the syndet soap, so-called “Syndetbars” which are free of fatty acid salts except for impurities and contain only synthetic surfactants.
  • the main components are the alkali salts of the fatty acids of natural oils and. Fat, preferably of chain lengths C 12 -C 18 . Since lauric acid soaps foam particularly well, the lauric acid-rich coconut and palm kernel oils are preferred raw materials for fine soap production.
  • the sodium salts of the fatty acid mixtures are solid, the potassium salts are soft-pasty.
  • the dilute sodium or potassium hydroxide solution is added to the fat raw materials in a stoichiometric ratio in such a way that an excess of lye of at most 0.05% is present in the finished soap. In many cases, soaps are no longer produced directly from fats, but rather from the fatty acids obtained by fat splitting.
  • Usual soap additives are fatty acids, fatty alcohols, lanolin, lecithin, vegetable oils, partial glycerides and other fat-like substances for regreasing the cleansed skin, antioxidants such as ascorbyl palmitate or tocopherol to prevent the autoxidation of the Soap (rancidity), complexing agents such as nitrilotriacetate to bind traces of heavy metals, which could catalyze autoxidative spoilage, perfume oils to achieve the desired fragrance notes, dyes for coloring the soap bars and if desired special additives.
  • Surfactants are amphiphilic substances that can dissolve organic, non-polar substances in water. Due to their specific molecular structure, they provide at least one hydrophilic and a hydrophobic part of the molecule, for a reduction of the surface tension of water, wetting the skin, facilitating dirt removal and solution, easy rinsing and - if desired - for foam regulation.
  • the object of the invention was therefore to provide bar soaps, that are free from the disadvantages described. It was also important to take into account that new bar soap compositions must also be able to be produced on an industrial scale, d. H. that the compositions are, for example, sufficient but not too have high ductility and do not tend to crack when dried.
  • the invention therefore relates to a shaped soap product containing talc, a or more fatty acids with 12-22 carbon atoms in the form of their alkali soaps and one or more lipid-replenishing substances in the absence of alkyl (oligo) glycosides, which overcomes the disadvantages of the prior art.
  • the shaped soap products according to the invention also have mechanical properties Deformation a particularly smooth surface. When used they generate a creamy, stable foam. The lime soap deposit formed in hard water remains dispersed in the water and does not lead to the gray, greasy deposits on the surface of sanitary objects.
  • Talc is a hydrated magnesium silicate of the formula 3MgO 4SiO 2 ⁇ H 2 O and Mg 3 ⁇ (Si 4 O 10) ⁇ (OH) 2 or Mg 6 (OH) 4 [Si 8 O 20] or Mg 12 [Si 16 O 40 ], which may however contain proportions of hydrated magnesium aluminum silicate of up to 12% by weight Al 2 O 3 , based on the entire product.
  • Talc is a white, mostly very fine, practically odorless to earthy-smelling powder that feels greasy when rubbed without being fat. It is insoluble in water, cold acids or alkalis. Depending on the country of origin, the chemical purity of the talcum (based on the content of anhydrous magnesium silicate) should be 93-98%.
  • Talc is used for the production of pharmaceutical powders, but above all for the production of cosmetic powders that are used for personal hygiene, but is also suitable for the production of tablets as a lubricant or flow agent.
  • the equivalent spherical diameter of the talc should be in the range of 0.5-50 ⁇ m. In general, such talc qualities have proven themselves that are not more than 5% by weight of particles below 1 ⁇ m and not more than 5% by weight of particles above 50 ⁇ m in size included. Preferably, the proportion of particles larger than 40 microns in Diameters are (sieve residue), at most 2% by weight.
  • the average particle diameter (D 50) is preferably 5-15 ⁇ m.
  • the content of accompanying substances should not exceed 1.6% by weight of Fe 2 O 3 , 1% by weight of CaO and 1% by weight of unbound water (loss of drying at 1050 ° C.).
  • the hydrated magnesium aluminum silicate content can be up to 60% by weight, calculated as Al 2 O 3 , up to 12% by weight.
  • the shaped soap products contain 1 to 20% by weight talc.
  • the shaped soap products may also advantageously be present 1 - 99% by weight of a basic soap, for example one whose soap components are composed of sodium tallowate, sodium cocoat and sodium palm kernel fatty acid salt.
  • the shaped soap products according to the invention also advantageously contain water in an amount of 5-35% by weight.
  • the water content is due to the one hand Manufacturing process, on the other hand, it has a beneficial effect on the properties of use Soap out.
  • the linear fatty acids with 12 to 22 carbon atoms e.g. B. the lauric, myristic, palmitic, stearic, arachic and behenic acid, but also the unsaturated fatty acids, for. B. the palmitoleic, oleic, linoleic, linolenic, arachidonic and erucic acid used.
  • Technical mixtures such as those obtained from vegetable and animal fats and oils, are preferably used, for. B. coconut oil fatty acid and tallow fatty acid. Mixtures of coconut and tallow fatty acid cuts are particularly preferred, in particular a mixture of 50-80% by weight of C 16 -C 18 tallow fatty acid and 20-50% by weight of C 12 -C 14 coconut fatty acid.
  • the fatty acids are used in the form of their alkali soap, usually as sodium soaps.
  • the soaps can also be obtained from the fats and oils directly by saponification (hydrolysis) be generated with sodium hydroxide solution and separation of the glycerol.
  • These can be identical to the fatty acids of the basic soap and by an appropriate alkali deficit in the saponification in the Basic soap can be introduced.
  • the free fatty acids are preferred after saponification and added after concentration, before drying.
  • R 1 is a primary C 12 -C 16 - Alkyl group
  • the alkyl (oligo) glycosides can be derived from aldoses or ketoses with 5 or 6 carbons.
  • alkyl- (oligo) -glucosides derived from glucose are produced on an industrial scale.
  • the absence of these substances means that they may at most be present as impurities in the mass on which the combibar according to the invention is based, and in any case must be less than 1% by weight.
  • the content of other surface-active surfactants in addition to keeping the invention as small as possible, advantageously below 5% by weight, based on the total weight of the shaped soap products according to the invention. It is preferred to completely dispense with such surfactants.
  • the soap bars according to the invention can, as further auxiliaries and additives, oil bodies, Emulsifiers, superfatting agents, fats, waxes, stabilizers, cationic polymers, silicone compounds, Pigments, biogenic agents, preservatives, colors and fragrances contain.
  • Further refatting agents are, for example, oil bodies such as Guerbet alcohols based on fatty alcohols having 6 to 18, preferably 8 to 10 carbon atoms, esters of linear C 6 -C 20 fatty acids with linear C 6 -C 20 fatty alcohols, esters of branched C 6 - C 13 carboxylic acids with linear C 6 -C 20 fatty alcohols, esters of linear C 6 -C 18 fatty acids with branched alcohols, in particular 2-ethylhexanol, esters of linear and / or branched fatty acids with polyhydric alcohols (e.g.
  • oil bodies such as Guerbet alcohols based on fatty alcohols having 6 to 18, preferably 8 to 10 carbon atoms, esters of linear C 6 -C 20 fatty acids with linear C 6 -C 20 fatty alcohols, esters of branched C 6 - C 13 carboxylic acids with linear C 6 -C 20 fatty alcohols, esters of linear C 6 -C 18 fatty
  • Non-ionic, ampholytic and / or zwitterionic can be used as emulsifiers or co-emulsifiers surface-active compounds are used, which are characterized by a lipophilic, preferably linear, alkyl or alkenyl group and at least one hydrophilic group.
  • This hydrophilic group can be both an ionic and a non-ionic Be a group.
  • Non-ionic emulsifiers contain as a hydrophilic group z.
  • B a polyol group, a polyalkylene glycol ether group or a combination of polyol and polyglycol ether group.
  • Preferred agents are those which contain nonionic surfactants from at least one of the following groups as O / W emulsifiers: (a1) addition products of 2 to 30 mol of ethylene oxide and / or 0 to 5 mol of propylene oxide onto linear fatty alcohols having 8 to 22 carbon atoms , on fatty acids with 12 to 22 C atoms and on alkylphenols with 8 to 15 C atoms in the alkyl group; (a2) C 12/18 fatty acid monoesters and diesters of adducts of 1 to 30 moles of ethylene oxide with glycerol; (a3) glycerol monoesters and diesters and sorbitan monoesters and diesters of saturated and unsaturated fatty acids having 6 to 22 carbon
  • B polyglycerol polyricinoleate or polyglycerol poly-12-hydroxystearate. Mixtures of compounds from several of these classes of substances are also suitable.
  • the adducts of ethylene oxide and / or of propylene oxide with fatty alcohols, fatty acids, alkylphenols, glycerol mono- and diesters and sorbitan mono- and diesters of fatty acids or with castor oil are known, commercially available products. These are mixtures of homologs, the middle of which Degree of alkoxylation corresponds to the ratio of the amounts of ethylene oxide and / or propylene oxide and substrate with which the addition reaction is carried out.
  • C 12/14 fatty acid monoesters and diesters of adducts of ethylene oxide with glycerol are known from DE-20 24 051 as refatting agents for cosmetic preparations.
  • Possible W / O emulsifiers are: (b1) addition products of 2 to 15 mol of ethylene oxide onto castor oil and / or hardened castor oil; (b2) partial esters based on linear, branched, unsaturated or saturated C 12/22 fatty acids, ricinoleic acid and 12-hydroxystearic acid and glycerol, polyglycerol, pentaerythritol, dipentaerythritol, sugar alcohols (e.g. sorbitol) and polyglucosides (e.g.
  • Suitable cationic polymers are, for example, cationic cellulose derivatives, cationic Strong, copolymers of diallyl ammonium salts and acrylamides, quaternized vinyl pyrrolidone / Vinylimidazole polymers such as B.
  • Luviquat TM BASF AG
  • condensation products of polyglycols and amines condensation products of polyglycols and amines, quaternized collagen polypeptides such as "Lauryldimonium-hydroxypropyl-hydrolyzed-collagen” (Lamequat TM L, Grünau GmbH) or "Lauryldimmonium-hydroxypropyl-hydroxylayed-wheat-protein” (Gluadin TM WQ, Grünau GmbH), polyethyleneimine, cationic silicone polymers such as B.
  • Amidomethicone or Dow Coming, Dow Coming Co./US copolymers of adipic acid and dimethylaminohydroxypropyl-diethylenetriamine (Cartaretine TM, Sandoz / CH), polyaminopolyamides such as e.g. B. described in FR 22 52 840-A and their crosslinked water-soluble polymers, cationic Chitin derivatives such as quaternized chitosan, optionally microcrystalline distributed, cationic guar gum such as B.
  • Jaguar TM CBS, Jaguar TM C-17, Jaguar TM C-16 (Celanese) or Cosmedia Guar TM C 261 (Henkel KGaA) quaternized ammonium salt polymers such as B.
  • As stabilizers can metal salts of fatty acids such. B. magnesium, aluminum and / or zinc stearate be used. Titanium dioxide is an example of a pigment.
  • biogenic Active ingredients are understood as plant extracts and vitamin complexes z, for example.
  • Preservatives are suitable, for example, phenoxyethanol, formaldehyde solution, parabens, Pentanediol or sorbic acid.
  • the dyes can be used for cosmetic purposes Suitable and approved substances are used, such as in the Publication "Cosmetic Dyes” by the Dye Commission of the German Research Foundation, Verlag Chemie, Weinheim, 1984, pp. 81-106 are compiled. This Dye are usually in concentrations of 0.001 to 0.1 wt .-%, based on the entire mixture.
  • the total proportion of auxiliaries and additives can range from 1 to 50, preferably 5 to 40 wt .-% - based on the means - amount.
  • the production of the shaped soap products according to the invention can be carried out for soaps usual way.
  • a fatty acid mixture and sodium hydroxide solution become one Basic soap with a solids content of 25-50 wt .-% and a solids content concentrated from 50-70 wt .-%.
  • 60% basic soap can already talc, optionally also free fatty acid, an anionic surfactant and a complexing agent to be mixed in.
  • the basic soap is used for.
  • B. in a vacuum expansion dryer further dewatered at 120 ° C to 130 ° C. The soap cools during expansion spontaneously decreases to temperatures below 60 ° C and becomes solid. Soap noodles fall with you Solids content of 73-85 wt .-%.
  • this basic soap is then made up into fine soap. It takes place in a soap mixer in which a slurry of the alkyl (oligo) glucoside and the other auxiliaries and additives are mixed into the soap noodles.
  • Shaped soap products in the sense of the invention can also be used as noodles, needles, Granules, extrudates, flakes and in any other shape customary for soap products available.
  • the talc can only be used in the packaging can be worked into the 73-85% basic soap.
  • the talcum powder via suitable dosing devices, e.g. B. belt scale and shaker with simultaneously added to the soap mixer with the slurry of fragrances and additives.
  • the soap products according to the invention are notable for a particularly smooth surface from what is particularly noticeable when processed into bar soap makes. A lot of fine-bubble, creamy foam forms when in use. In hard water Although lime soap precipitates also form, these remain dispersed in the solution and do not appear as greasy gray spots or cheesy on hard surfaces Edge, but at best as a light, finely divided veil.
  • the basic soap noodles are dosed with the color slurry and the other components into a conventional soap mixer (screw mixer with perforated sieve), homogenized by repeated mixing, discharged via an extruder, cut and processed into pieces in the usual way.
  • a conventional soap mixer screw mixer with perforated sieve
  • Example 2 Wt .-% color slurry 3.00 basic soaps 85,00 paraffin 1.00 talc 7.00 Perfume 1.00 Na 2 S 2 O 3 0.40 octyldodecanol 0.50 water ad 100.00
  • the basic soap noodles are dosed with the color slurry and the other components into a conventional soap mixer (screw mixer with perforated sieve), homogenized by repeated mixing, discharged via an extruder, cut and processed into pieces in the usual way.
  • a conventional soap mixer screw mixer with perforated sieve
  • Example 3 Wt .-% color slurry 3.00 basic soaps 81.80 paraffin 1.00 talc 9.00 Perfume 1.00 Na 2 S 2 O 3 0.40 octyldodecanol 0.50 water ad 100.00
  • the basic soap noodles are dosed with the color slurry and the other components into a conventional soap mixer (screw mixer with perforated sieve), homogenized by repeated mixing, discharged via an extruder, cut and processed into pieces in the usual way.
  • a conventional soap mixer screw mixer with perforated sieve
  • Example 4 Wt .-% color slurry 3.00 basic soaps 78,90 paraffin 1.00 talc 12,00 Perfume 1.00 Na 2 S 2 O 3 0.40 octyldodecanol 0.50 water ad 100.00
  • the basic soap noodles are combined with the color slurry and the other components usual soap mixer (screw mixer with perforated sieve) dosed, by repeated mixing homogenized, discharged via an extruder, cut and in the usual way Processed into pieces.
  • usual soap mixer screw mixer with perforated sieve

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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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)
EP01115784A 2000-07-20 2001-07-11 Pain de savon comprenant du talc, un ou plusieurs acides gras d'alkali et un ou plusieurs émollients en absence d'oligoglycosides d'alkyl Revoked EP1174493B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10035213A DE10035213A1 (de) 2000-07-20 2000-07-20 Geformtes Seifenprodukt, enthaltend Talkum, eine oder mehrere Fettsäuren in Form ihrer Alkaliseifen und eine oder mehrere rückfettend wirkende Substanzen bei gleichzeitiger Abwesenheit von Alkyl-(oligo)-glycosiden
DE10035213 2000-07-20

Publications (2)

Publication Number Publication Date
EP1174493A1 true EP1174493A1 (fr) 2002-01-23
EP1174493B1 EP1174493B1 (fr) 2005-01-26

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ID=7649527

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Application Number Title Priority Date Filing Date
EP01115784A Revoked EP1174493B1 (fr) 2000-07-20 2001-07-11 Pain de savon comprenant du talc, un ou plusieurs acides gras d'alkali et un ou plusieurs émollients en absence d'oligoglycosides d'alkyl

Country Status (6)

Country Link
US (1) US6589923B2 (fr)
EP (1) EP1174493B1 (fr)
JP (1) JP2002097496A (fr)
AT (1) ATE287943T1 (fr)
DE (2) DE10035213A1 (fr)
ES (1) ES2234736T3 (fr)

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JP2010528627A (ja) * 2007-06-01 2010-08-26 ソラザイム、インク 微生物による油の生産
EP2265724A4 (fr) * 2008-04-09 2013-01-23 Solazyme Inc Modification chimique directe de biomasse microbienne et d'huiles microbiennes
ES2583639T3 (es) * 2008-11-28 2016-09-21 Terravia Holdings, Inc. Producción de aceites específicos en microorganismos heterótrofos
CN102933700B (zh) 2009-12-23 2016-05-04 高露洁-棕榄公司 清洁皂条
SG10201504197SA (en) 2010-05-28 2015-06-29 Solazyme Inc Food Compositions Comprising Tailored Oils
RU2593784C2 (ru) 2010-12-09 2016-08-10 Колгейт-Палмолив Компани Очищающая композиция
EP2817403B1 (fr) 2012-02-24 2017-04-05 Colgate-Palmolive Company Pain de savon
EP3500658B1 (fr) * 2016-08-17 2021-12-15 Zobele Holding S.P.A. Pastille soluble dans l'eau et procédé de fabrication de ladite pastille soluble dans l'eau
EP4569066A1 (fr) * 2022-08-12 2025-06-18 The Procter & Gamble Company Compositions à faible teneur en eau
MX2024006097A (es) * 2022-08-12 2024-05-30 Procter & Gamble Composiciones solidas disolubles.
EP4569071A1 (fr) * 2022-08-12 2025-06-18 The Procter & Gamble Company Compositions solubles solides
CA3235845A1 (fr) * 2022-08-12 2024-02-15 The Procter & Gamble Company Compositions a faible teneur en eau
WO2024036116A1 (fr) * 2022-08-12 2024-02-15 The Procter & Gamble Company Compositions solides solubles
MX2024006600A (es) * 2022-08-12 2024-06-12 Procter & Gamble Composiciones de bajo contenido de agua.
WO2024036124A1 (fr) * 2022-08-12 2024-02-15 The Procter & Gamble Company Compositions solides solubles
JP2024543587A (ja) * 2022-08-12 2024-11-21 ザ プロクター アンド ギャンブル カンパニー 低水分組成物
US20240060016A1 (en) * 2022-08-12 2024-02-22 The Procter & Gamble Company Low-Water Compositions

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JP2002097496A (ja) 2002-04-02
DE10035213A1 (de) 2002-01-31
ATE287943T1 (de) 2005-02-15
US6589923B2 (en) 2003-07-08
US20020045555A1 (en) 2002-04-18
EP1174493B1 (fr) 2005-01-26
ES2234736T3 (es) 2005-07-01

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