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WO2019115435A1 - Système structurant conservant une humidité élevée pour composition détergente - Google Patents

Système structurant conservant une humidité élevée pour composition détergente Download PDF

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Publication number
WO2019115435A1
WO2019115435A1 PCT/EP2018/084120 EP2018084120W WO2019115435A1 WO 2019115435 A1 WO2019115435 A1 WO 2019115435A1 EP 2018084120 W EP2018084120 W EP 2018084120W WO 2019115435 A1 WO2019115435 A1 WO 2019115435A1
Authority
WO
WIPO (PCT)
Prior art keywords
detergent
structuring system
moisture
composition
hydrated
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.)
Ceased
Application number
PCT/EP2018/084120
Other languages
English (en)
Inventor
Amalendu BANGAL
Sujitkumar Suresh Hibare
Narayanan Subrahmaniam
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.)
Unilever NV
Conopco Inc
Original Assignee
Unilever NV
Conopco Inc
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 Unilever NV, Conopco Inc filed Critical Unilever NV
Priority to CN201880080691.7A priority Critical patent/CN111511886B/zh
Publication of WO2019115435A1 publication Critical patent/WO2019115435A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0069—Laundry bars
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/1213—Oxides or hydroxides, e.g. Al2O3, TiO2, CaO or Ca(OH)2
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/10—Salts
    • C11D7/12—Carbonates bicarbonates
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/20—Water-insoluble oxides

Definitions

  • the present invention relates to a structuring system having hydrated sodium carbonate, which holds high levels of moisture.
  • the present invention also relates to detergent composition and in particular detergent bar having the structuring system without compromising on bar properties.
  • detergent bars contain detergent active components and detergent builders together with optional components for example abrasives, perfumes, alkaline salts, hardeners and bleaching agents. Structuring system and fillers are also present in such compositions in small amounts that replace some of the detergent active in the bar while retaining the desired hardness of the bar.
  • a few known fillers include starch, kaolin and talc.
  • Detergent bars in particular require an acceptable physical strength so that they retain their structural integrity during handling, transport and use.
  • the hardness of the bars, at the time of manufacture and subsequently, is an especially important property.
  • US2004/0102353 discloses dimensionally stable alkaline solid block warewashing detergent using an E-form binder, forming a solid comprising a sodium carbonate source of alkalinity, a metal corrosion protecting alkali metal silicate composition, a sequestrant, a surfactant package and other optional material.
  • the solid block is dimensionally stable and highly effective in removing soil from the surfaces of dishware in the institutional and industrial environment.
  • the E-form hydrate comprises an organic phosphonate and a hydrated carbonate.
  • WO 01/42413 relates to a detergent bar composition
  • a detergent bar composition comprising from 10 to 60 % by weight of detergent active; from 0.5 to 40 % by weight of colloidal aluminium hydroxide- phosphate and/or aluminium hydroxide-sulphate complex (Al-complex); from 0-30 % by weight of detergent builder; from 0-60 % by weight of inorganic particulate material; from 8 to 35 % by weight of water and optionally other liquid benefit agents; and the balance optionally being other minor additives.
  • Al-complex colloidal aluminium hydroxide- phosphate and/or aluminium hydroxide-sulphate complex
  • US Patent 4,427,417 discloses a non-caking, granular detergent compositions suitable for use in automatic laundry machines or in automatic dishwashing machines prepared from hydratable particulate detergent salts or such salts in admixture with other detergent ingredients such as non-hydratable detergent salts, surfactants, fillers, corrosion inhibiors, chlorine releasing agents, colorign agents, and perfumes under conditions insuring substantially complete hydration of the hydratable detergent salts and agglomeration of the hydrated particulates in the compositiuon into storage stable, dry pourable agglomerates.
  • Structuring systems like those disclosed in IN177828 A (Unilever, 1997) enables the soap/detergent bar to have satisfactory hardness with high water and low total fatty matter (TFM) content.
  • the application discloses a structuring system having a balanced combination of aluminium hydroxide and total fatty matter (TFM), which enables use of higher water content in the bar while using TFM at a lower level.
  • the patent describes a process for generating colloidal aluminium hydroxide in-situ by reacting a fatty acid with an aluminium containing alkaline material such as sodium aluminate.
  • Some of the known structuring systems use phosphates for structuring water and increasing the moisture content in the detergent bars, but incorporation of phosphates in composition adversely affect the lakes and streams by causing eutrophication and their use in detergent composition has been subject to government scrutiny and regulation.
  • Increased levels of water content for structuring the bar helps in improving the in use property of the bar without affecting its physical properties in an economical way. It is important to deliver sensory properties such as lather, cleaning, product feel and improved economy in use by reducing mush and wear without altering the
  • hydrated salts as a water structuring system is reported in GB1230427 A1 (Colgate, 1971 ) which describes a built detergent laundry bar, substantially free of pre- formed sodium bicarbonate, and having a smooth feel in use.
  • the detergent bar includes at least 22 wt.% of a binder having starch and/or cereal flour and an alkaline builder having a salt that has been hydrated in situ in the presence of the binder.
  • the disclosed hydrated salt includes sodium carbonate, pentasodium tripolyphosphate or a mixture thereof.
  • starch may not be stable in highly alkaline condition within the detergent composition and may degrade over time.
  • hydrated sodium carbonate surprisingly provides improved structuring system that retains high levels of moisture content when used in combination with a structurant selected from hydrated aluminium material, silica material or a mixture thereof.
  • the structuring system when used in a detergent bar composition is capable of retaining high levels of moisture without compromising on the physical properties and sensorial attributes.
  • the invention provides a high-moisture retaining structuring system for use in a high-moisture detergent composition, said structuring system comprising:
  • the invention provides a process for preparing a structuring system of the first aspect, said process including the steps of contacting a carbonic acid or a partially neutralised water-soluble salt of carbonic acid with a strong alkali, wherein the strong alkali is selected from alkali metal salt of aluminate or alkali metal salt of silicate.
  • the present invention provides a high-moisture detergent composition comprising the structuring system of the first aspect or a structuring system obtainable by a process of the second aspect.
  • the present invention provides a method for preparing a detergent bar composition according to the third aspect comprising the steps of: i. preparing in-situ a structuring system according to the first aspect, by mixing a strong alkali with a carbonic acid or a partially neutralised water soluble salt of carbonic acid;
  • step (ii) adding either a preformed detergent active to the structuring system of step (i) or preparing in-situ a detergent active to form an extrudable dough; and, iii. extruding the dough of step (ii) into a detergent bar.
  • the invention relates to a structuring system comprising a hydrated sodium carbonate and at least one structurant selected from the group consisting of hydrated aluminium material, silica material or mixtures thereof.
  • structural system refers to a selected material or mixture of materials which retains high amounts of moisture and the structuring system when added to a composition for example a detergent bar composition with the primary purpose of retaining water in the composition at high levels enables the bar to retain moisture at high levels without compromising on the bar properties.
  • the structuring system of the present invention includes 0.5wt% to 70wt% hydrated sodium carbonate.
  • the amount of water content that the hydrated sodium carbonate contains is at its highest state of hydration (i.e. 10 mole of water per mole of sodium carbonate).
  • a substantial portion of the hydrated sodium carbonate is sodium decahydrate. It is preferred that at least 20 parts of the total content of hydrated sodium carbonate present in the structuring system is at its highest state of hydration, more preferably at least 60 parts, still preferably at least 70 parts, still more preferably 80 parts, further preferably 90 parts and most preferably all of the hydrated sodium carbonate present in the structuring system is at its highest state of hydration.
  • the hydrated sodium carbonate is fully hydrated, and can absorb water such that at least 20% of its weight is water and it has an equilibrium relative humidity at 25°C of less than 60%. In this way, it can absorb significant amounts of moisture ‘locked away’ so that it does not readily evaporate and effect detergent bar properties upon storage.
  • the amount of hydrated sodium carbonate in the structuring system of the present invention is at least 1wt%, still preferably at least 2.5wt%, further preferably at least 5wt%, more preferably 10wt% and most preferably at least 15wt%, but typically not more than 60wt%, still preferably not more than 50wt% and most preferably not more than 30wt% based on the weight of the structuring system.
  • hydrated sodium carbonate is stable with respect to moisture loss up to 40°C. This means that the water associated with the hydrated sodium carbonate remains in a stable state when heated up to 40°C, beyond 40°C the sodium carbonate decahydrate dissolves in its own water of crystallisation and results in sodium carbonate solution, this then is not stable with respect to moisture loss.
  • the structuring system of the present invention includes a structurant selected from hydrated aluminium material, silica material or mixtures thereof.
  • structurant refers to a material which tend to bind the water such that the amount of water content is maintained in the composition, for example a detergent bar composition.
  • the structurant according to the present invention includes hydrated aluminium material.
  • the hydrated aluminium material refers to aluminium-based material that has associated water content.
  • the hydrated aluminium material is preferably alumina hydroxide, alumina gel or mixtures thereof. More preferably, the hydrated aluminium material is alumina hydroxide.
  • the amount of hydrated aluminium material in the structuring system of the present invention is at least 1wt%, still preferably at least 2.5wt%, further preferably at least 5wt%, more preferably 10wt% and most preferably at least 15wt%, but typically not more than 27wt%, still preferably not more than 25wt% and most preferably not more than 20wt% based on the weight of the structuring system.
  • Disclosed structuring system includes 0.5 to 30 wt% of at least one of alumina hydroxide, alumina gel, amorphous silica, hydrated silica or mixtures thereof, more preferably at a level of 10 to 30 wt% and most preferably at a level of 15 to 30 wt%.
  • Silica material :
  • the structurant according to the present invention includes a silica material.
  • silica material according to the present invention includes but is not limited to silica, silicon dioxide, silica material in different forms including crystalline silica, amorphous silica, silicates, hydrated silica, fumed silica, precipitated silica, gel silica and colloidal silica.
  • Preferred forms herein are amorphous silica, hydrated silica, polymer of hydrated silica or mixtures thereof. More preferably the silica material is hydrated silica.
  • silicates which may be used are sodium neutral silicates or alkaline silicates with a weight ratio of Si0 2 to Na 2 0 in the range from 1.6:1 to 3.4:1.
  • the silica material can be incorporated in the structuring system at a level from 0.5wt% to 30 wt%, preferably from 10wt% to about 30wt%, and more preferably from 15wt% to 30wt%, of the structuring system.
  • the structuring system according to the present invention includes 0.5 to 30 wt.% hydrated sodium carbonate and 0.5 to 30 wt.% hydrated alumina material.
  • the structuring system of the present invention includes 10wt% to 45wt% water content.
  • the structuring system has a total moisture content from 12 to 45 wt.%.
  • the water content of the structuring system is 15wt%, further preferably 17wt%, more preferably 18wt% and most preferably 20wt%, but typically not more than 40wt%, still preferably not more than 38wt% and most preferably not more than 35wt% based on the weight of the structuring system.
  • water content refers to water associated with a high water retaining material in a way that it can only be removed by heating. The water may be chemically bound or otherwise associated with the material such that the water content is maintained and not easily lost for example from the structuring system or a detergent composition having the structuring system.
  • the water content can be determined through thermo gravimetric analysis (TGA) using a Parkin Elmer Thermogravimetric Analyzer TGA8000.
  • TGA thermo gravimetric analysis
  • Thermogravimetric Analyzer TGA8000 The TGA is conducted by heating the sample strongly under a N 2 atmosphere with heating rate of 10°C/min in the range of 30°C to 250°C.
  • a process for preparing a structuring system having the step of neutralising the carbonic acid or partially neutralised salt of carbonic acid using a strong alkali selected from a silicate, alkaline aluminium containing material and mixtures thereof.
  • the alkaline aluminium containing material is an alkali metal salt of aluminate.
  • the alkali metal salt of aluminate is either a sodium aluminate or a potassium aluminate, more preferably it is sodium aluminate.
  • the sodium aluminate is in the form of a solution, preferably an aqueous solution with a solid content in the range from 30 to 75wt%, more preferably 45 to 65wt% still preferably 45 to 55wt%, more preferably, 40wt% to 55 wt%.
  • the sodium aluminate When the sodium aluminate is in the form of a sold it is with a moisture content of 4 to 35wt%, more preferably with a moisture content of 4 to 25wt%.
  • the alkaline aluminium material is sodium aluminate wherein the AI 2 O 3 to Na 2 0 is in the ratio of 0.5:1 to 1.64:1 , preferably 0.8:1 to 1.55:1 , more preferably 1 :1 to 1.5:1.
  • the strong alkali may be alkali metal salt of silicate, preferably sodium silicate or potassium silicate, more preferably a sodium silicate. When the strong alkali is a sodium silicate in a solid form, preferably it has a moisture content of 4 to 35wt%.
  • the partially neutralised salt of carbonic acid is a bicarbonate of an alkali metal, preferably sodium bicarbonate.
  • the neutralisation process involves mixing the strong alkali and the carbonic acid or partially neutralised salt of carbonic acid and stirring the mixture to provide a homogeneous mixture, the stirring time is preferably from 2 to 15 minutes, at continuous stirring.
  • the strong alkaline material is sodium aluminate
  • a measured amount of sodium aluminate is added to a mixer and small amounts of carbonic acid or partially neutralised salt of carbonic acid, preferably sodium bicarbonate is added along with continuous stirring until all of the sodium bicarbonate is added and the stirring is further continued until a homogeneous dry structuring system according to the present invention is obtained.
  • Disclosed process may preferably involve addition of other ingredients. It is generally not required to add additional water during the neutralisation step when sodium aluminate used is at 45% purity and the remaining 55% is water by weight of the alkaline material. If required small amounts of around 5 to 10 wt% water may be added additionally.
  • a maximum of 65wt% of water may be present, preferably the water content in the slurry is not more than 60wt%, still preferably not more than 55wt%, and most preferably not more than 50wt% by weight of the slurry.
  • the invention in a third aspect, relates to a high-moisture detergent composition comprising the structuring system.
  • Disclosed high-moisture detergent composition preferably includes 5 to 80 wt.% detergent active. More preferably, the detergent composition includes from 10 to 40wt% detergent active.
  • the amount of detergent active in the high-moisture detergent composition is at least 10 wt%, still preferably at least 15 wt%, further preferably at least 20 wt% and most preferably at least 25 wt%, but typically not more than 55wt%, still preferably not more than 45wt% and most preferably not more than 35 wt% of the detergent composition.
  • the detergent active may be chosen from any one of anionic, nonionic, cationic, zwitterionic, amphoteric surfactants and mixtures thereof.
  • the nonionic and anionic surfactants of the surfactant system may be chosen from the surfactants described "Surface Active Agents" Vol. 1 , by Schwartz & Perry,
  • the surfactants used are saturated.
  • Suitable anionic detergent compounds which may be used are usually water- soluble alkali metal salts of organic sulphates and sulphonates having alkyl radicals containing from about 8 to about 22 carbon atoms, the term alkyl being used to include the alkyl portion of higher acyl radicals.
  • suitable synthetic anionic detergent compounds are sodium and potassium alkyl sulphates, especially those obtained by sulphating higher Cs to Cie alcohols, produced for example from tallow or coconut oil, sodium and potassium alkyl Cg to C20 benzene sulphonates, particularly sodium linear secondary alkyl C10 to C15 benzene sulphonates; and sodium alkyl glyceryl ether sulphates, especially those ethers of the higher alcohols derived from tallow or coconut oil and synthetic alcohols derived from petroleum.
  • the preferred water-soluble synthetic anionic detergent active compounds are the alkali metal (such as sodium and potassium) and alkaline earth metal (such as calcium and magnesium) salts of higher alkyl benzene sulphonates, alpha olefin sulphonates and their mixtures with higher alkyl sulphates, and the higher fatty acid monoglyceride sulphates.
  • Most preferred anionic surfactants are sodium lauryl ether sulfate (SLES), particularly preferred with 1 to 3 ethoxy groups, sodium C10 to C15 alkyl benzene sulphonates and sodium C12 to Cie alkyl sulphates.
  • surfactants such as those described in EP-A-328 177 (Unilever), which show resistance to salting-out, the alkyl polyglycoside surfactants described in EP-A-070 074, and alkyl monoglycosides.
  • the chains of the surfactants may be branched or linear.
  • Other anionic detergent actives are soaps.
  • soap denotes salts of carboxylic fatty acids.
  • the soap may be derived from any of the triglycerides conventionally used in soap manufacture-consequently the carboxylate anions in the soap may contain from 8 to 22 carbon atoms.
  • the preferred ones are C12-C18 fatty acid soaps.
  • the fatty acid soap used preferably contains from about 16 to about 22 carbon atoms, preferably in a straight chain configuration.
  • the anionic contribution from soap is preferably from 0 to 30 wt% of the total anionic, more preferably from 0 to 15wt%, still preferably from 0 to 5 wt% of the total anionic.
  • At least 50 wt % of the anionic surfactant is selected from: sodium Cn to C15 alkyl benzene sulphonates; and, sodium C12 to Cis alkyl sulphates. Even more preferably, the anionic surfactant is sodium Cn to C15 alkyl benzene sulphonates.
  • Suitable nonionic detergent compounds which may be used include, in particular, the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide either alone or with propylene oxide.
  • Preferred nonionic detergent compounds are O Q to C22 alkyl phenol- ethylene oxide condensates, generally 5 to 25 EO, i.e. 5 to 25 units of ethylene oxide per molecule, and the condensation products of aliphatic Cs to Cis primary or secondary linear or branched alcohols with ethylene oxide, generally 5 to 50 EO.
  • the non-ionic is 10 to 50 EO, more preferably 20 to 35 EO.
  • Alkyl ethoxylates are particularly preferred.
  • cationic, amphoteric or zwitterionic detergent actives are included in the compositions according to the invention.
  • Suitable cationic detergent actives that can be incorporated are alkyl substituted quarternary ammonium halide salts e.g. bis
  • Suitable amphoteric detergent-active compounds that optionally can be employed are derivatives of aliphatic secondary and tertiary amines containing an alkyl group of 8 to 18 carbon atoms and an aliphatic radical substituted by an anionic water-solubilizing group, for instance sodium 3-dodecylaminopropionate, sodium 3-dodecylaminopropane sulphonate and sodium N-2hydroxydodecyl-N-methyltaurate.
  • Suitable zwitterionic detergent-active compounds that optionally can be employed are derivatives of aliphatic quaternary ammonium, sulphonium and phosphonium compounds having an aliphatic radical of from 8 to 18 carbon atoms and an aliphatic radical substituted by an anionic water-solubilising group, for instance 3-(N-N-dimethyl- N-hexadecylammonium) propane-1- sulphonate betaine, 3-(dodecylmethyl sulphonium) propane-1 -sulphonate betaine and 3- (cetylmethyl phosphonium) ethane sulphonate betaine.
  • Builders 3-(N-N-dimethyl- N-hexadecylammonium) propane-1- sulphonate betaine, 3-(dodecylmethyl sulphonium) propane-1 -sulphonate betaine and 3- (cetylmethyl phosphonium) ethane sulphonate betaine.
  • the hydrated alkali metal carbonate also functions as detergency builder and preferably no additional builder may be added to the composition. However if desired further builders may be added in small amounts.
  • detergency builders used in the formulation are preferably inorganic and suitable builders include, for example, alkali metal aluminosilicates (zeolites), alkali metal carbonate, sodium tripolyphosphate (STPP), tetrasodium pyrophosphate (TSPP), citrates, sodium nitrilotriacetate (NTA) and combinations of these.
  • the phosphate builders are present in an amount ranging from 0 to 5 wt%, still preferably from 0 to 3 wt%, further preferably from 0 to 2.5 wt% and most preferably the detergent composition includes no phosphate builders.
  • Suitable inorganic particulates can be selected from zeolites, calcites, dolomites, feldspars, other carbonates, bicarbonates, borates, sulphates, feldspars, talc, kaolin, soapstone and polymeric materials such as polyethylene.
  • the most preferred inorganic particulates are calcium carbonate (as Calcite), mixtures of calcium and magnesium carbonates (as dolomite), sodium hydrogen carbonate, sodium/potassium sulphate, sodium/potassium chloride, zeolite, feldspars, talc, kaolin, silica and soapstone.
  • detergent bar composition include water-insoluble material, customarily referred to as filler that helps to form the structure of the bar.
  • Clays notably kaolin and bentonite are conventional for this purpose. If a water insoluble detergency builder is present, this will also contribute to the content of water-insoluble material.
  • Calcite, talc, kaolin, feldspar and dolomite and mixtures thereof are particularly preferred due to their low cost and colour.
  • the detergent composition of this invention may optionally include various other materials, both soluble and insoluble.
  • the minor and conventional ingredients preferably selected from antiredeposition agents such as sodium carboxymethyl cellulose, fluorescers, colour, germicides, opacifiers, humectants such as glycerol, polyethylene glycols, preservatives and perfumes, also bleaches, bleach precursors, bleach stabilisers, sequestrants, soil release agents (usually polymers) and other polymers, polysaccharides such as starch or modified starches and celluloses may optionally be incorporated up to 10wt%.
  • Enzymes may also be included, notably proteases, lipases, cellulases, mannanases, and amylases.
  • Water-soluble salts such as sodium sulphate may be included as a filler.
  • the water-soluble alkali metal salts of those sulphur oxo acids which are reducing agents may be included in the composition as bleaches.
  • the detergent composition of the present invention has less than 5wt% starch or its derivatives more preferably less than 3wt% starch or its derivatives, still preferably less than 2wt% starch or its derivatives, and it is most preferred than the detergent composition of the present invention has no starch, celluloses or modified starch added to the composition.
  • moisture content in the finished detergent composition is maintained from 12% to 40%, preferably from 15% to 30%, more preferably from 1 1 wt% to 30wt%, yet more preferably from 20% to 27%, by weight of the finished detergent composition.
  • Detergent bar composition preferably from 15% to 30%, more preferably from 1 1 wt% to 30wt%, yet more preferably from 20% to 27%, by weight of the finished detergent composition.
  • the high moisture detergent composition is a shaped detergent composition formed into any shape, which is convenient to use by the consumer.
  • the cross-sectional area of the bar will generally be such that the bar can be held conveniently in one hand, usually above 800 mm 2 with a thickness above 15 mm.
  • the cross-sectional configuration for the bar may be, for example, rectangular, square, oval or circular.
  • Detergent bar composition according to the present invention includes 5 wt% to 70 wt% of the structuring system, preferably, the amount of structuring system in the detergent bar composition of the present invention is at least 15 wt%, still preferably at least 20wt%, further preferably at least 25wt%, more preferably 30wt% and most preferably at least 35wt%, but typically not more than 50wt%, still preferably not more than 45wt% and most preferably not more than 40 wt% based on the weight of the detergent bar composition.
  • detergent bar composition of the present invention comprises at least 15%, more preferably at least about 20%, and most preferably at least about 25%, by weight of the detergent bar composition, of water.
  • the level of water can be still higher, e.g. 30%, 35%, or even 40%, but is typically not greater than about 60%, preferably not greater than about 55%, and more preferably not greater than about 50%, by weight of the detergent bar composition.
  • the water activity of the detergent bar composition is preferably in the range from 0.779 to 0.788 when measured at a temperature of 45°C.
  • Water activity is a measure of water loss encountered during storage from a substance. It is expressed in terms of relative humidity (%) and was measured using a water activity meter (e.g. TH 200 Thermo constanter from Novasina)
  • An essential feature of the invention is that the combination structurant selected from the group consisting of the hydrated aluminium material, silica material or mixtures thereof along with the hydrated sodium carbonate helps in improving the water structuring and thus retention of the water in the structuring system, further when the structuring system is incorporated in a detergent bar composition the structuring system provides for immediate hardening of the bar, preferably within 1 hour of extrusion.
  • crystallization and recrystallization in presence of hydrated alumina material and/or silica material is believed to be responsible for accelerating the formation of hydrated sodium carbonate and the quick formation of hydrates even in presence of large amounts of water thus providing the desired bar properties as disclosed in the present invention.
  • the high-moisture detergent composition is in the form of solid free-flowing detergent composition which includes a particulate, powder or granular composition.
  • the solid free flowing detergent composition may be prepared by any of the method well known to the person skilled in the art.
  • the base powder of the detergent composition may be prepared preferably by spray drying or non-tower route.
  • the base powder of the detergent composition generally includes detergent active, builders, polymers and fillers.
  • the prepared base powder is generally post-dosed with heat-sensitive ingredients and fillers for formulating the composition.
  • the structuring system of the present invention having high-levels of moisture content may be used to replace the fillers added in the post-dosing stage without compromising on the free- flowing and the anticaking properties desired by the consumers.
  • Solid free-flowing detergent composition having the structuring system according to the present invention further provides the benefits of using less chemical based fillers, provides products with low bulk density as compared to composition with chemical based fillers, provide improved flow properties to powder prepared through the non- tower route process and enabling the formulators to provide concentrated products without bringing about consumer habit change.
  • Solid free flowing detergent composition includes 25 wt% to 60 wt% of the structuring system, preferably, the amount of structuring system in the detergent composition of the present invention is at least 30 wt%, still preferably at least 35 wt%, further preferably at least 40 wt%, more preferably 45 wt% and most preferably at least 65wt%, but typically not more than 60 wt%, still preferably not more than 55 wt% and most preferably not more than 50 wt% based on the weight of the detergent composition.
  • fillers Similar to the detergent bars, some amount of fillers is also added to a solid detergent composition such as described herein and fillers serves the purpose of providing optimum flow characteristics.
  • the fillers however are known to be included at higher levels to formulate detergent composition with optimum costs. Fillers add to the insoluble content in the composition and make the composition less attractive to the end consumer. It is desired to remove these fillers to provide superior products which does not cause greying of the fabrics and increase the environmental impact of the products. Replacement of the fillers with the structuring system of the present invention thus provides the benefit of achieving a detergent composition which has lower amounts of insoluble and has good powder properties like flow characteristics.
  • Replacement of fillers with the structuring system also delivers the desired low density to the detergent composition enabling the composition to deliver the required levels of the actives without changing consumer habits; the volumetric dosage of the
  • composition is unaltered.
  • Preferably solid free flowing detergent composition of the present invention comprise at least about 1 1%, more preferably at least about 15%, and more preferably at least about 25%, by weight of the detergent composition, of water content.
  • the level of water content can be still higher, e.g. 30%, 35%, or even 40%, but is typically not greater than about 60%, preferably not greater than about 55%, and more preferably not greater than about 50%, by weight of the detergent composition.
  • preparing in-situ a structuring system by mixing a strong alkali with a carbonic acid or a partially neutralised water soluble salt of carbonic acid; ii. adding either a preformed detergent active to the structuring system of step (i) or preparing a detergent active in-situ to form an extrudable dough; and, iii. extruding the dough of step (ii) into a detergent bar.
  • additional ingredients are added into the dough prior to the extruding step.
  • the process for preparing the detergent bar composition involves in-situ formation of hydrated sodium carbonate.
  • the formation of hydrated sodium carbonate in-situ involves the step of mixing a strong alkali with a carbonic acid or a precursor of carbonic acid which may be a partially neutralized water soluble salt of carbonic acid.
  • strong alkali in a range of 2 to 25 parts is mixed with 5 parts to 45 parts of carbonic acid or a precursor of carbonic acid which may be a partially neutralized water soluble salt thereof.
  • the strong alkali may be preferably selected from alkaline aluminium containing material, preferably an aluminate. Still more preferably alkali metal salt of aluminate, silicate, or mixtures thereof.
  • the alkali metal is selected from sodium, potassium, more preferably sodium.
  • the strong alkali is a sodium aluminate or a sodium silicate, sodium aluminate is the most preferred.
  • the sodium aluminate is preferably with a solid content of 15 to 55% and preferably the ratio of AI 2 O 3 to Na 2 0 ratio is in the range from 0.5 to 1.55:1.
  • the detergent active may be added either in the acid form or in the neutralised salt form.
  • the neutralization of the detergent active by strong alkali is effected either before the addition of the carbonic acid, after the reaction between the strong alkali and the carbonic acid or simultaneously added along with the carbonic acid.
  • carbonic acid instead of carbonic acid, a partially neutralized water- soluble salt of carbonic acid may also be used.
  • the mixing and neutralisation is carried out in any mixer conventionally used in soap/detergent manufacture and is preferably a high shear-kneading mixer.
  • the preferred mixer includes ploughshare mixer, mixers with kneading members of sigma type, multiwiping overlap, single curve or double arm.
  • the double arm kneading mixers can be overlapping or tangential design.
  • the partially neutralized water soluble salt of carbonic acid is a bicarbonate salt of an alkali metal.
  • the alkali metal is sodium or potassium, more preferably sodium.
  • the formed dough is preferably allowed to cool either by keeping it open to atmosphere or passing through a chilled roll mill.
  • the chilled roll mill had three or five horizontal parallel, closely spaced, driven counter rotating rolls
  • the residence time on the mill is preferably around 5 to 10 seconds and the temperature of the mixture reduces to about 25 to 30°C during milling.
  • Next step involves extruding the dough, in this step the dough is fed to a plodder of conventional construction having a pair of counter-rotating worms in a single cooled barrel fitted with a tapered extrusion head at the outlet of which was an extrusion die maintained at a temperature of 25 to 30°C.
  • the plodder had the usual stationary perforated plate fitted against the outlet end of the worm at the entrance to the tapered extrusion head so that the material was forced through the perforations of the plate, but this plate could be omitted.
  • the plodded material emerged at a temperature of 25 to 30°C, as a continuous rod of a rectangular cross section (7.6 cmx3.9 cm, and lying on its wide face) corresponding to the rectangular extrusion opening in the die.
  • the extruded rod was cut directly (e.g. 3 seconds after extrusion) to produce individual detergent bars, of the same cross section as the rod and each 10 cm long. Although the rod was soft it could be cut smoothly, using continuous vertically moving cutters, without being substantially distorted by the action of the cutter blades.
  • the detergent bars were passed continuously through a holding conveyor maintained at a temperature of 15 to 20°C (or, if desired, a cooling tunnel could be used).
  • the bars were hard enough to be pressed (in well-known manner, using a soap press), wrapped in paper and packed, or wrapped and packed without pressing.
  • the bars were hard and firm and had a smooth feel in use, when both freshly made and after ageing.
  • the structuring system For preparing the structuring system, 160 grams of sodium aluminate solution with a solid content of 45 wt% and around 55 wt% water was taken in a plastic beaker. To the sodium aluminate solution, 200 grams of sodium bicarbonate powder was added slowly and the mixture was stirred continuously with a stainless steel spatula. In the initial stages, post addition of sodium bicarbonate, the mixture is a thin slurry that builds in rigidity after approximately 4 to 6 minutes. As the reaction progresses, the temperature of the mixture rises and the rigidity also increases to yield a structuring system.
  • the structuring system is in a dry form, it has a bound water content of about 10 to 45 wt% and comprises hydrated sodium carbonate and alumina hydroxide (hydrated aluminium material).
  • the bound water content in the structuring system was measured using a Parkin Elmer Thermogravimetric Analyzer TGA8000.
  • a specified amount of the prepared structuring system of Example 1 was placed in the sample holder of the instrument and heated from 30°C to 250°C at the rate of 10°C per minute.
  • the weight of the sample decreased because of moisture loss, the weight loss in the sample starting from 40°C was recorded and the amount of bound water content (wt%) was determined.
  • the amount of bound water content of the structuring system prepared according to Example 1 was 35 wt%.
  • Example 2 Preparation of high-moisture detergent bar composition according to the present invention
  • Process I For the preparation of a 100 kg batch of high-moisture detergent bar according to the present invention 31.05wt% of sodium aluminate solution with a solid content of 45wt% and remaining 55wt% water was taken in a sigma mixer. Next 38wt% sodium bicarbonate powder was slowly added with continuous mixing in the sigma mixer for a duration of around 10 to 15 minutes, during this period the temperature of the mixture rises and the initial milky slurry gradually hardens to a rigid structuring system.
  • the dough was cooled by either keeping it open to atmosphere or passing through a chilled roll mill. Thereafter the dough is passed through an extruder and formed into a shaped rod and cut directly (e.g. 3 seconds after extrusion) to produce individual detergent bars, of the same cross section as the rod and each 10.3 cm long. Although the rod was soft it could be cut smoothly, without being substantially distorted by the action of the cutter blades. The bars were hard and firm and had a smooth feel in use, both when freshly made and after ageing.
  • Process II In an alternative method for preparation of the detergent bar having the structuring system according to the present invention, 31.05 wt% of sodium aluminate solution with a solid content of 45wt% and remaining 55wt% water was taken in a sigma mixer. Next 17.55 wt% acid precursor of LAS with a purity of 90% was added and the mixing was continued for 5 minutes to allow complete neutralisation of the acid precursor of LAS. Thereafter 38wt% sodium bicarbonate powder was slowly added with continuous mixing in the sigma mixer for a duration of around 10 to 15 minutes, during this period the temperature of the mixture rises and the initial milky slurry gradually hardens to a rigid structuring system.
  • Penetration value indicates the hardness of the bar which was measured using a cone penetrometer, the details of a typical instrument and the method of measurement is given below.
  • Range of measurement 0 to 40mm
  • Range of verification 20 in steps of 5
  • Procedure of measurement The entire mass (comprised of penetrometer needle and standard weight) resting on the test sample was allowed to drop freely on the test sample, the penetrometer needle penetrates the test mass to a specific distance for a specified period of time, and the distance was recorded to 1/10 th of mm. The average of at least 3 reading was taken and provided in Table 1 below.
  • the detergent bar according to the present invention was also evaluated for sensory attributes using the test methods given hereinafter and the evaluation results were recorded and provided in the Table 1a below.
  • a wash down protocol technique was followed for estimation of grittiness by feel using a group of trained panellists.
  • the wash down protocol involves holding the detergent bar under running water and evaluating the surface feel of the bar by rubbing the bar with hand with 40 rotations.
  • Detergent bar with acceptable quality generally have a feel score in the range of 7.8 to 8. Wear/%Wear: For determining, the wear of the bars, the initial weight of the bar was taken. A single wash down protocol was followed in which a desized 100% woven cotton fabric was immersed in a bowl of water (the water hardness was 6FH Ca:Mg- 2:1 ). The fabric is then held up in both hands and allowed to drain for 10sec. Thereafter the fabric was laid flat in the enamel tray.
  • the test bar was immersed momentarily in 2.0L of water (6 FH Ca:Mg 2:1 ) and a first face of the bar was rubbed 5 times along the length of the wet fabric, such that there is no overlapping of rubbed areas. Thereafter the wet fabric was turned over and the bar was rubbed another 5 times along the length of the wet fabric using the same face of the bar. The bar is again immersed momentarily in water and then a second face of the bar is rubbed along the length of a second wet fabric, in a similar operation as conducted on the first fabric.
  • the weight loss after the above process is noted and express as: a) weight loss in grams and b) % loss in weight.
  • the above test was done in triplicate.
  • Density The density of the bar is measured by the standard method and calculated using the formula:
  • Example 3 Evaluation of detergent bar composition according to the invention and a comparative detergent bar composition
  • Comparative detergent bar For the preparation of a comparative detergent bar (Comp A) 36wt% of acid precursor of LAS anionic surfactant was mixed with 25.75wt% sodium carbonate in a sigma mixer to form a neutralized paste to this paste 10wt% water and 28.1wt% corn starch was added to form a dough. The dough was allowed to cool by keeping it open to the atmosphere. Once cooled, the dough was passed through an extruder and formed into a shaped rods and cut directly (e.g. 3 seconds after extrusion) to produce individual detergent bars, of the same cross section as the rod and each 10.3 cm long. The final bar composition is provided in Table 3.
  • Example 3 For the preparation of a detergent bar according to the present invention (Ex 3), 30wt% of sodium aluminate solution with a solid content of 45wt% and remaining 55wt% water was taken in a sigma mixer. Next 34wt% sodium bicarbonate powder was slowly added with continuous mixing in the sigma mixer for a duration of around 10 to 15, during this period the temperature of the mixture rises and the initial milky slurry gradually hardens to a rigid structuring system. To the formed structuring system, 36wt% acid precursor of LAS was added and the mixing is continued for 5 minutes to allow complete neutralisation of the acid precursor of LAS and the obtained dough was cooled by keeping it open to atmosphere.
  • the dough was passed through an extruder and formed into a shaped rods and cut directly (e.g. 3 seconds after extrusion) to produce individual detergent bars, of the same cross section as the rod and each 10.3 cm long.
  • the final bar composition is provided in Table 3.
  • Penetration value indicates the rigidity or hardness of the bar and the value was determined using a standard cone penetrometer (Petrotest PNR10).
  • Petrotest PNR10 a standard cone penetrometer
  • the needlepoint of the penetrometer was adjusted on the flat surface of the sample detergent bar so that it makes point contact on the surface. The adjustment was accurately made using a side lift-lit lamp and the shadow of needle-tip and needle-tip itself were made to coincide.
  • the scale was adjusted to zero and the instrument was switched on. The instrument measures the depth of penetration of the needle for a time duration of 5 seconds. The penetration value was recorded and the above procedure was repeated thrice at different point on the bar surface.
  • the moisture content of the detergent bar was determined by powdering the detergent bar and keeping 1 gm of the powder material on the pan of a hot air oven and heated up to 130°C. The material was kept for a period of 1 hour or until the weight was constant. The weight of the powdered material at the end of 1 hour was measured and from the weight loss calculation the % of moisture content was calculated and provided in the Table 1.
  • Example 4 Powder detergent composition comprising the structuring system according to the present invention
  • a spray dried base powder was prepared having the composition as provided in Table 4.
  • Comp B For preparing the comparative spray dried powder detergent composition (Comp B) specified amount of sodium carbonate was added to the prepared spray dried base powder as given in Table 4.
  • spray dried powder detergent composition (Ex 4) according to the present invention specified amount of structuring system comprising 42wt% moisture content prepared according to Example 1 was added to the prepared spray dried base powder as given in Table 4.
  • the data shown in table 4 indicates that the composition (Ex 4) prepared according to the present invention having the structuring system has higher moisture content as compared to the comparative detergent composition (Comp B) and is still free flowing.

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Abstract

La présente invention concerne un système structurant contenant un carbonate de sodium hydraté, qui conserve des niveaux élevés d'humidité. La présente invention concerne également une composition détergente et en particulier des pains détergents contenant ledit système structurant sans compromettre les propriétés des pains. L'objet de la présente invention est de pourvoir à une composition détergente contenant un système structurant qui conserve des niveaux élevés d'humidité sans affecter négativement l'aspect physique ou autres attributs sensoriels, où ledit objet peut être atteint par la présente invention. En particulier, on a découvert contre toute attente qu'un système structurant amélioré à base d'une combinaison de carbonate de sodium hydraté et d'un matériau d'aluminium hydraté, d'un matériau de silice ou d'un mélange de ceux-ci peut être utilisé pour obtenir une composition détergente qui est capable de conserver des niveaux élevés d'humidité sans compromettre les propriétés physiques et les attributs sensoriels.
PCT/EP2018/084120 2017-12-12 2018-12-10 Système structurant conservant une humidité élevée pour composition détergente Ceased WO2019115435A1 (fr)

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WO2022040488A1 (fr) * 2020-08-21 2022-02-24 Dow Global Technologies Llc Composition de détergent en pain sans savon
WO2022258605A1 (fr) 2021-06-10 2022-12-15 Unilever Ip Holdings B.V. Barres de savon en gel de silice à teneur élevée en agent d'humidité et leur procédé de préparation
WO2025056485A1 (fr) 2023-09-11 2025-03-20 Unilever Ip Holdings B.V. Pains de savon de silice polymère à haute teneur en humidité de faible tfm

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CN113773916A (zh) * 2020-11-05 2021-12-10 杭州英诺克新材料有限公司 一种原位生成的结构化液体洗涤剂制备方法及其应用

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022040488A1 (fr) * 2020-08-21 2022-02-24 Dow Global Technologies Llc Composition de détergent en pain sans savon
JP2023539088A (ja) * 2020-08-21 2023-09-13 ダウ グローバル テクノロジーズ エルエルシー 非石鹸洗剤バー組成物
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WO2022258605A1 (fr) 2021-06-10 2022-12-15 Unilever Ip Holdings B.V. Barres de savon en gel de silice à teneur élevée en agent d'humidité et leur procédé de préparation
WO2025056485A1 (fr) 2023-09-11 2025-03-20 Unilever Ip Holdings B.V. Pains de savon de silice polymère à haute teneur en humidité de faible tfm

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