WO2004111177A1 - Composant de detergent et son procede de preparation - Google Patents

Composant de detergent et son procede de preparation Download PDF

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Publication number
WO2004111177A1
WO2004111177A1 PCT/EP2004/005131 EP2004005131W WO2004111177A1 WO 2004111177 A1 WO2004111177 A1 WO 2004111177A1 EP 2004005131 W EP2004005131 W EP 2004005131W WO 2004111177 A1 WO2004111177 A1 WO 2004111177A1
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WO
WIPO (PCT)
Prior art keywords
detergent
gelling agent
ingredient
component
organic
Prior art date
Application number
PCT/EP2004/005131
Other languages
English (en)
Inventor
Harmannus Tammes
Remy Antal Verburgh
Original Assignee
Unilever Plc
Unilever Nv
Hindustan Lever Limited
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 Plc, Unilever Nv, Hindustan Lever Limited filed Critical Unilever Plc
Publication of WO2004111177A1 publication Critical patent/WO2004111177A1/fr

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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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special 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
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/22—Carbohydrates or derivatives thereof
    • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin

Definitions

  • the present invention relates to a granular detergent component suitable for incorporation into particulate laundry detergent compositions, and a novel process for its preparation..
  • detergent ingredients are available in liquid form. This can be for a variety of reasons, for example storage stability.
  • Detergent surfactants may be available as solids, but in many cases are commercially available only as solutions, generally aqueous solutions of relatively low concentration, typically below 50 wt%, for example, 30 to 40 wt%.
  • aqueous solutions of relatively low concentration typically below 50 wt%, for example, 30 to 40 wt%.
  • water-soluble quaternary ammonium cationic surfactants having a single long hydrocarbon chain or branched, especially mid-chain branched anionic surfactants mobile solutions of higher concentration are not obtainable because gelling occurs.
  • complete drying is not effective because the compounds either form sticky solids which are not suitable for handling and processing and/or decompose at the temperatures necessary for effective drying.
  • polymers are available as aqueous solutions and some ingredients are available as emulsions. While these materials may be suitable for inclusion in liquid detergent compositions, or for incorporation in detergent powders via traditional slurry-making and spray- drying processes, the large amount of associated water can pose problems in preparing granular detergent compositions or components by non-spray-drying (mixing and granulation) processes .
  • WO 96/17042A discloses detergent granules containing a .water-soluble cationic surfactant and an inorganic carrier, the granules also containing an anionic surfactant in a weight ratio to the cationic surfactant of less than 1:1, and preferably less than 0.5:1.
  • the inorganic carrier material is zeolite.
  • the granules are prepared by evaporating and concentrating a solution of the cationic and anionic surfactants to a concentration above 50 wt%, and then granulating with the carrier material. The presence of the anionic surfactant prevents gelling during the concentration step.
  • WO 98/53037A discloses a process for the preparation of cationic surfactant granules, in which a aqueous solution or dispersion of cationic surfactant, optionally plus sodium silicate and/or filler, is dried in the presence of a drying gas, preferably air, at a temperature of less than 250 0 C.
  • a drying gas preferably air
  • the preferred drying method is co-current spray-drying.
  • the present inventors have now discovered a particularly convenient process for manufacturing detergent components which are made up of liquid ingredients.
  • the invention accordingly provides a process for the preparation of a particulate detergent component comprising an organic gelling agent, which process comprises absorbing an aqueous solution, dispersion or emulsion of detergent ingredient into the gelling agent and removing water by an evaporative process.
  • the present invention provides a detergent component comprising an organic gelling agent.
  • this carrier comprises a material, such as a detergency builder, which would subsequently be added to a finished detergent mixture.
  • a mixture of liquid detergent ingredient and gelling agent the liquid detergent ingredient content of the powder or granules produced can be made higher than when using carrier and liquid detergent ingredient alone.
  • the solution of liquid detergent ingredient and organic gelling agent and carrier powder may be brought together by any convenient means.
  • the solution is added to a carrier powder in a high, medium or low shear mixer.
  • the aqueous solution, dispersion or emulsion is sprayed on to a carrier powder as it is agitated.
  • the carrier powder may conveniently be granulated during this process.
  • the carrier powder is fluidised in a fluid bed reactor and the surfactant solution sprayed on to or in to the fluid bed.
  • a granular material is formed which may subsequently be dried in the fluid bed or externally.
  • some or all of the surfactant solution is added to the carrier powder, optionally along with other powders, in a high or medium shear mixer or a flash before being passed into a fluid bed reactor for addition of extra surfactant solution, if required, and drying.
  • the process of the present invention comprises dissolving an organic gelling agent in an aqueous solution, dispersion or emulsion of detergent ingredient and drying to produce a solid powder.
  • the gelling agent may be added in any convenient form. Preferably, it will be added as a dry solid since this minimises the amount of water to be evaporated. However, it may be added as an aqueous solution or as a non aqueous solution, provided the solvent is miscible with water and compatible with the detergent ingredient .
  • the amount to be added can be easily determined by simple experiment but will preferably be in the range of 1% to 20% dry weight of gelling agent to dry weight of detergent ingredient, more preferably in the range 2% - 10% and most preferably in the range 4% - 6%.
  • a low temperature drying process is preferably used when the detergent component contains only surfactant and organic gelling agent.
  • suitable techniques are well known to those skilled in the art including freeze drying, vacuum evaporation and low relative humidity drying.
  • the liquid detergent ingredient and a carrier powder may be brought together by any convenient means.
  • the aqueous solution, dispersion or emulsion of detergent ingredient is added to the carrier powder in a high, medium or low shear mixer.
  • the aqueous solution, dispersion or emulsion of detergent ingredient is sprayed on to the carrier powder as it is agitated.
  • the solution/carrier mix may be in the form of a damp powder or a slurry and appropriate solutions are known to those skilled in the art to handle such materials.
  • An important feature is that temperature must be kept below the level at which the advantages of the invention are lost. Typically this will be achieved at below 80 0 C. - S -
  • Lodige CB machine or moderate-speed mixers such as a Lodige KM machine Other suitable equipment includes Drais R
  • a low- or high-shear mixer granulator has a stirring action and/or a cutting action which are operated independently of one another.
  • Preferred types of low- or high-shear mixer granulators are mixers of the Fukae R FS-G series; Diosna V series ex Dierks & Sohne, Germany; Pharma
  • the low shear mixer may conveniently comprise a gas fluidisation granulator, preferably operated at a superficial air velocity of about 0.1-1.2 ms , either under positive or negative relative pressure and with an air inlet temperature ranging from -10° or 5°C up to 30°C with an optional step at up to 80 °C, or in some cases, up to 200 °C.
  • An operational temperature inside the bed of from ambient temperature to 60 0 C is typical.
  • the droplet size in the spray relative to the particle size of the solids is adjusted to control granule size, bulk density and the yield of the process.
  • the process comprises spraying droplets of the surfactant solution containing organic gelling agent to contact a particulate solid starting material in a low-shear granulator, wherein the 0. ⁇ 12 average droplet diameter
  • (Sauter Mean Diameter) of the liquid binder is not greater than 10 times, preferably not greater than 5 times, more preferably not greater than 2 times and most preferably not greater than the average particle diameter of that fraction of the total solid starting material which has a d- 3 , 2 particle diameter of from 20 ⁇ m to 200 ⁇ m. If more than 90% by weight of the solid starting material has a d 3(2 average particle diameter less than 20 ⁇ m then the U ⁇ 12 average particle diameter of the total solid starting material is taken to be 20 ⁇ m and if more than 90% by weight of the solid starting material has a d 3 , 2 average particle diameter greater than 200 ⁇ m then the d 3 , 2 average particle diameter of the total solid starting material is taken to be 200 ⁇ m.
  • the process of the present invention can be applied to any- detergent ingredient which is available in liquid form.
  • any surfactant available associated with water as a solvent It is especially applicable to surfactants which are difficult or impossible to obtain in a solid form suitable for further powder processing.
  • it is envisaged that it could be applied to any suitable surfactant to improve its powder handling characteristics. It is likely to find most application in the treatment of anionic and non-ionic surfactants, which comprise the bulk of the surfactant component of most detergent powder compositions.
  • Anionic surfactants are well-known to those skilled in the art. Examples include alkylbenzene sulphonates, particularly linear alkylbenzene sulphonates having an alkyl chain length of Cs-Cis; primary and secondary alkylsulphates, particularly C 8 -C 20 primary alkyl sulphates; alkyl ether sulphates; olefin sulphonates; alkyl xylene sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
  • Sodium salts are generally preferred. - S -
  • Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C 8 -C 20 aliphatic alcohols ethoxylated with an average of from 1 to 20 moles of ethylene oxide per mole of alcohol, and more especially the C 10 -C 15 primary and secondary aliphatic alcohols ethoxylated with an average of from 1 to 10 moles of ethylene oxide per mole of alcohol.
  • Non-ethoxylated nonionic surfactants include alkylpolyglycosides, glycerol monoethers, and polyhydroxyamides (glucamide) .
  • Water-soluble cationic surfactants include quaternary ammonium salts of the general formula R 1 R 2 R 3 R 4 N X wherein
  • Ri is a relatively long (Cg-Cis) hydrocarbon chain, typically an alkyl, hydroxyalkyl or ethoxylated alkyl group, optionally interrupted with a heteroatom or an ester or amide group; each of R 2 , R 3 and R 4 (which may be the same or different) is a short-chain (C 1 -C 3 ) alkyl or substituted alkyl group; and X is a solubilising anion, for example a chloride, bromide or methosulphate ion.
  • Other classes of cationic surfactant include cationic esters (for example, choline esters) .
  • Zwitterionic surfactants include betaines.
  • An especially preferred material is cocoamidopropyl betaine (CAPB) , in which RQ is C 12 -C 14 alkyl and m is 3.
  • CAPB cocoamidopropyl betaine
  • Preferred amphoteric surfactants include alkyl amine oxides of the general formula R 7 R 8 R 9 N-K) wherein R 7 is typically a Cs-Ci S alkyl group, for example, C 12 -C 14 alkyl, and Rs and
  • Rg which may be the same or different, are C 1 -C 3 alkyl or hydroxyalkyl groups, for example, methyl groups.
  • the most preferred amine oxide is coco dimethylamine oxide, in which R 7 is C 12 -C 14 alkyl and Rs and Rg are methyl groups.
  • detergent ingredients which are available in liquid form include polymers, antifoams and sequestrants .
  • the organic gelling agent may comprise any composition capable of forming a gel and drying to a friable solid. Suitable materials include gelatines, the alginates and alganic acids, pectins and starches. One factor in the choice of gelling agent will be its behaviour at the pH of the aqueous surfactant. A particularly favoured gelling agent is gelatine.
  • Granular detergent products typically consist of one or more types of granular component, often admixed with one or more post dosed powdered ingredients.
  • the granular components may be sprayed with one or more liquid materials after they have been formed.
  • Detergent compositions of the invention comprise surfactant and organic gelling agent, along with any residual water and/or usual impurities, and may also contain other detergent-active compounds and detergency builders, and may optionally contain bleaching components and other active ingredients, as outlined below, to enhance performance and properties. Any one or more of such other materials may alternatively be incorporated wholly or partly in the granular component of the present invention, with the remaining components supplied in any convenient form. This may comprise one or more other granular components, each containing a single ingredient and/or a mixture of ingredients. Alternatively, one or more of the other ingredients may be post dosed in powder or liquid form. A combination of the two methods may be used.
  • a single granular component according to any aspect of the present invention may be sold as a finished product. Alternatively, it may be used in conjunction with other components to produce the finished detergent product. Where a detergent composition according to the invention contains more than one granular component at least one of the granular components must be in accordance with the present invention. Any or all of the other granular components may also be in accordance with the present invention.
  • Detergent-active compounds may be chosen from soap and non-soap anionic, cationic, nonionic, amphoteric and zwitterionic detergent-active compounds, and mixtures thereof.
  • detergent-active compounds are available and are fully described in the literature, for example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.
  • the preferred detergent-active compounds that are used are soaps and synthetic non-soap anionic and nonionic compounds.
  • the total amount of surfactant present is suitably within the range of from 5 to 40 wt%.
  • Cationic, amphoteric and zwitterionic surfactants may also form part of the surfactant system. They will generally be present in combination with anionic surfactants, the weight ratio of anionic surfactant to cationic, amphoteric or zwitterionic surfactant being at least 1:1.
  • the detergent compositions of the invention also contain one or more detergency builders.
  • the total amount of detergency builder in the compositions will suitably range from 5 to 80 wt%, preferably from 10 to 60 wt%.
  • detergency builder is combined with surfactant solution and organic gelling agent. In this case all or part of the detergency builder may be added at this stage, any shortfall being added in a post dosing stage.
  • Preferred builders are alkali metal aluminosilicates, more especially crystalline alkali metal aluminosilicates zeolites) , preferably in sodium salt form.
  • the compositions of the invention may also contain phosphate builders, for example, sodium tripolyphosphate, either alone or in combination with aluminosilicates .
  • zeolite A The aluminosilicate used in most commercial particulate detergent compositions is zeolite A.
  • maximum aluminium zeolite P zeolite MAP
  • Zeolite MAP is an alkali metal aluminosilicate of the P type having a silicon to aluminium ratio not exceeding 1.33, preferably not exceeding 1.15, and more preferably not exceeding 1.07.
  • Zeolite or phosphate builders may suitably be present in a total amount of from 5 to 60 wt%, preferably from 10 to 50 wt%.
  • the zeolites may be supplemented by other inorganic builders, for example, amorphous aluminosilicates, or layered silicates such as SKS- 6 ex Clariant.
  • the zeolites may be supplemented by organic builders, for example, polycarboxylate polymers such as polyacrylates and acrylic/maleic copolymers; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates; and sulphonated fatty acid salts.
  • polycarboxylate polymers such as polyacrylates and acrylic/maleic copolymers
  • monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and
  • organic builders are citrates, suitably used in amounts of from 1 to 30 wt%, preferably from 2 to 15 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%.
  • Builders both inorganic and organic, are preferably present in alkali metal salt, especially sodium salt, form.
  • Detergent compositions according to the invention may also suitably contain a bleach system.
  • a bleach system Preferably this will include a peroxy bleach compound, for example, an inorganic persalt or an organic peroxyacid, capable of yielding hydrogen peroxide in aqueous solution.
  • Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate, the latter being especially preferred.
  • the sodium percarbonate may have a protective coating against destabilisation by moisture.
  • the peroxy bleach compound is suitably present in an amount of from 5 to 35 wt%, preferably from 10 to 25 wt% .
  • the peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures.
  • the bleach precursor is suitably present in an amount of from 1 to 8 wt%, preferably from 2 to 5 wt% .
  • Preferred bleach precursors are peroxycarboxylic acid precursors, more especially peracetic acid precursors and peroxybenzoic acid precursors; and peroxycarbonic acid precursors.
  • An especially preferred bleach precursor suitable for use in the present invention is N, N, N 1 ,N 1 -tetracetyl ethylenediamine (TAED).
  • a bleach stabiliser may also be present.
  • Suitable bleach stabilisers include ethylenediamine tetraacetate (EDTA) , diethylenetriamine pentaacetate (DTPA) , ethylenediamine disuccinate (EDDS) , and the polyphosphonates such as the Dequests (Trade Mark) , ethylenediamine tetramethylene phosphonate (EDTMP) and diethylenetriamine pentamethylene phosphate (DETPMP) .
  • EDTA ethylenediamine tetraacetate
  • DTPA diethylenetriamine pentaacetate
  • EDDS ethylenediamine disuccinate
  • polyphosphonates such as the Dequests (Trade Mark) , ethylenediamine tetramethylene phosphonate (EDTMP) and diethylenetriamine pentamethylene phosphate (DETPMP) .
  • compositions of the invention may contain alkali metal, preferably sodium, carbonate, in order to increase detergency and ease processing.
  • alkali metal preferably sodium, carbonate
  • Sodium carbonate may suitably be present in amounts ranging from 1 to 60 wt%, preferably from 2 to 40 wt%.
  • Sodium silicate may also be present, suitably in an amount of from 0.1 to 5 wt%.
  • Powder flow may be improved by the incorporation of a small amount of a powder structurant.
  • powder structurants include, for example, fatty acids (or fatty acid soaps) , sugars, acrylate or acrylate/maleate polymers, sodium silicate, and dicarboxylic acids (for example, Sokalan (Trade Mark) DCS ex BASF) .
  • fatty acids or fatty acid soaps
  • sugars for example, acrylate or acrylate/maleate polymers
  • sodium silicate for example, Sokalan (Trade Mark) DCS ex BASF
  • dicarboxylic acids for example, Sokalan (Trade Mark) DCS ex BASF
  • fatty acid soap suitably present in an amount of from 1 to 5 wt%.
  • antiredeposition agents such as cellulosic polymers; soil release agents; anti-dye-transfer agents; fluorescers; inorganic salts such as sodium sulphate; enzymes (proteases, lipases, amylases, cellulases) ; dyes; coloured speckles; perfumes; and fabric conditioning compounds. This list is not intended to be exhaustive.
  • the detergent compositions of the invention are in particulate form.
  • Particulate detergent compositions comprise powders, and tablets of compacted powder.
  • the organic gellant/surfactant component may be added to compositions comprising any suitable bulk density. Powders of low to moderate bulk density are commonly prepared by spray-drying a slurry, and optionally postdosing further ingredients by dry-mixing. If such a process is used the organic gellant/surfactant component of the present invention is preferably added at the postdosing dry mixing stage .
  • the bulk density of the organic gellant and surfactant component in combination with produced by non spray drying routes may be lower that that of powders commonly produced by such routes .
  • the processes and components of the present invention are, therefore, particularly advantageous when used to produce low bulk density detergent compositions by the non spray drying route .
  • “Concentrated” or “compact” powders may be prepared by mixing and granulating processes, for example, using a highspeed mixer/granulator, or other non-tower processes. Such processes may also be adapted to produce low bulk density powders.
  • the organic gellant/surfactant component may be added at a post dosing dry mixing stage, or may be formed in-situ during a suitable processing stage where organic gellant and surfactant are combined in the presence of other components of the detergent composition.

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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)
  • Molecular Biology (AREA)
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  • Detergent Compositions (AREA)

Abstract

L'invention porte sur un procédé de préparation d'un composant de détergent particulaire comprenant un agent organique gélifiant, ce procédé consistant à absorber un ingrédient de détergent liquide qui est une solution aqueuse, une dispersion ou une émulsion d'ingrédient du détergent, dans l'agent gélifiant et éliminer l'eau par un procédé d'évaporation.
PCT/EP2004/005131 2003-06-06 2004-05-12 Composant de detergent et son procede de preparation WO2004111177A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0313139.8 2003-06-06
GB0313139A GB0313139D0 (en) 2003-06-06 2003-06-06 Detergent component and process for preparation

Publications (1)

Publication Number Publication Date
WO2004111177A1 true WO2004111177A1 (fr) 2004-12-23

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1460646A (en) * 1973-10-15 1977-01-06 Procter & Gamble Detergent composition and process
US5173200A (en) * 1989-04-04 1992-12-22 Creative Products Resource Associates, Ltd. Low-solvent gelled dryer-added fabric softener sheet
WO1994012613A1 (fr) * 1992-12-03 1994-06-09 Unilever Plc Protection d'additifs
EP0922449A2 (fr) * 1997-10-31 1999-06-16 National Starch and Chemical Investment Holding Corporation Utilisation d'un dérivé d'amidon traité par enzymes en tant qu'agent d'encapsulage
WO2000046337A1 (fr) * 1999-02-02 2000-08-10 Quest International B.V. Composition detergente
WO2001038471A1 (fr) * 1999-11-24 2001-05-31 Henkel Kommanditgesellschaft Auf Aktien Procede de production de microemulsions contenant des enzymes et d'enzymes microencapsulees
WO2001079414A1 (fr) * 2000-04-15 2001-10-25 Cognis Deutschland Gmbh & Co. Kg Procede de production de granules tensioactifs non ioniques

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1460646A (en) * 1973-10-15 1977-01-06 Procter & Gamble Detergent composition and process
US5173200A (en) * 1989-04-04 1992-12-22 Creative Products Resource Associates, Ltd. Low-solvent gelled dryer-added fabric softener sheet
WO1994012613A1 (fr) * 1992-12-03 1994-06-09 Unilever Plc Protection d'additifs
EP0922449A2 (fr) * 1997-10-31 1999-06-16 National Starch and Chemical Investment Holding Corporation Utilisation d'un dérivé d'amidon traité par enzymes en tant qu'agent d'encapsulage
WO2000046337A1 (fr) * 1999-02-02 2000-08-10 Quest International B.V. Composition detergente
WO2001038471A1 (fr) * 1999-11-24 2001-05-31 Henkel Kommanditgesellschaft Auf Aktien Procede de production de microemulsions contenant des enzymes et d'enzymes microencapsulees
WO2001079414A1 (fr) * 2000-04-15 2001-10-25 Cognis Deutschland Gmbh & Co. Kg Procede de production de granules tensioactifs non ioniques

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