WO2017148989A1 - Suspension de détergent pouvant être versée, comprenant une phase fluide colorée et des particules en suspension - Google Patents

Suspension de détergent pouvant être versée, comprenant une phase fluide colorée et des particules en suspension Download PDF

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Publication number
WO2017148989A1
WO2017148989A1 PCT/EP2017/054722 EP2017054722W WO2017148989A1 WO 2017148989 A1 WO2017148989 A1 WO 2017148989A1 EP 2017054722 W EP2017054722 W EP 2017054722W WO 2017148989 A1 WO2017148989 A1 WO 2017148989A1
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WO
WIPO (PCT)
Prior art keywords
suspension
detergent
water
range
suspension according
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PCT/EP2017/054722
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English (en)
Inventor
Elena Maria Gabriella Barbuzzi
Maria Petra J VAN DEURZEN
Kees Bert Geerse
Robert Jan MOLL
Ferdinando TARENTINI
Original Assignee
Unilever N.V.
Unilever Plc
Conopco, Inc., D/B/A Unilever
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Application filed by Unilever N.V., Unilever Plc, Conopco, Inc., D/B/A Unilever filed Critical Unilever N.V.
Publication of WO2017148989A1 publication Critical patent/WO2017148989A1/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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/003—Colloidal solutions, e.g. gels; Thixotropic solutions or pastes
    • 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
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/0013—Liquid compositions with insoluble particles in suspension
    • 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
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2065—Polyhydric alcohols
    • 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
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/33—Amino carboxylic acids
    • 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
    • C11D3/40—Dyes ; Pigments

Definitions

  • the present invention relates to a pourable detergent suspension comprising 85-99.2 wt.% of a dyed fluid phase and 0.8-15 wt.% of suspended, particles having a diameter in the range of 0.1 -2 mm, said detergent suspension comprising:
  • liquid component selected from water, glycerol and mixtures thereof, said liquid component comprising 8-25% water and at least 20% glycerol, by weight of the detergent suspension;
  • the combination of the liquid component and the one or more aminocarboxylate chelants represents at least 60 wt.% of the detergent suspension; wherein the suspension has a water activity of not more than 0.7; and wherein the dyed fluid phase has a reflective color represented by a chromaticity (a * ), chromaticity (b * ) and a lightness (L * ) expressed by the CIE Lab color coordinate system meeting the following conditions:
  • the detergent suspension of the present invention combines a very attractive appearance with high stability and is easy to manufacture.
  • Detergent formulations typically contain a number of different active components, including surfactants, builders, enzymes and bleaching agents.
  • Surfactants are employed to release stains and soil and to disperse the released components into the cleaning liquid. Enzymes help to remove stubborn stains of proteins, starch and lipids by hydrolyzing these components.
  • Bleaching agents are employed in detergent compositions to remove bleachable stains, such as those associated with tea, coffee, red wine, and various fruit and vegetable products, by oxidizing the components that make up these stains.
  • Typical bleaching agents for use in detergent formulations are chlorine- and peroxygen-based compounds, such as hypochlorite and percarbonate bleach, respectively.
  • Builders are incorporated in detergent formulations to complex magnesium and calcium ions as well as to maintain alkaline pH conditions.
  • Phosphorous based builders such as phosphates
  • Phosphorous based builders have been used for many years in a wide variety of detergent compositions.
  • alternative building agents have been developed and these alternative builders have found their way into commercial detergent products.
  • the aminocarboxylate chelant L- glutamic-N,N-diacetate is an example of an environmentally friendly builder that is used in commercial detergent products.
  • aminocarboxylate chelants are present in detergent formulations in the form of their (fully deprotonated) sodium salts.
  • Aqueous solutions of aminocarboxylate salts are alkaline.
  • Liquid detergent formulations have been developed as these products offer the advantage over powdered formulations that they are easy to dose, may contain higher concentrations of active ingredients, suffer less from moisture spoilage during storage and/or are more easily dispersed into aqueous cleaning liquid.
  • liquid detergent compositions that deliver cleaning, spotting and filming performance similar to that of a powdered formulation it is necessary to include components that remain undissolved in the liquid product matrix. These undissolved components need to be homogeneously suspended throughout the product to guarantee a constant, optimum cleaning result. Although this may be achieved by instructing the user to shake the product before use, it is clearly preferable to provide the liquid detergent formulation in the form of a suspension that remains stable during the lifecycle of the product. This objective, however, is very difficult to achieve as suspensions demix over time because suspended particles are subject to sedimentation and
  • Bleaching agents and enzymes are moisture-sensitive detergent ingredients that lose their activity over time if the water activity of a detergent composition is too high.
  • EP-A 1 129 160 describes liquid aqueous cleaning compositions containing water, glycerol, builder, enzyme and thickener.
  • WO 2013/092276 describes detergent formulations containing GLDA, water, citric acid, nonionic surfactant, coated spray-dried percarbonate, enzymes and other ingredients.
  • WO 2014/107578 describes detergent compositions containing water, glycerol,
  • polyaminocarboxylic acid chelating agent
  • nonionic surfactant nonionic surfactant
  • enzymes enzymes
  • EP-A 1 129 160 describes liquid aqueous cleaning compositions containing water, glycerol, builder, enzyme and thickener.
  • US 2010/0081600 describes a liquid detergent composition exhibiting an at least two color effects, said composition comprising:
  • a colored interference pigment having a color and showing an absorbance minimum in the range from about 380 to about 750 nm range of the light spectrum
  • a dye system i. a colored interference pigment having a color and showing an absorbance minimum in the range from about 380 to about 750 nm range of the light spectrum
  • DE-A 10 2014 212643 relates to liquid ADW detergent compositions comprising a liquid and a solid enzyme formulation.
  • Example 1 describes a liquid ADW detergent containing glycerol, water, dye and solid enzyme.
  • WO 2015/181570 relates to an aqueous gel or liquid detergent composition, comprising: ⁇ 5 to 60 wt% of an aminocarboxylate builder;
  • the pourable detergent composition of the present invention comprises a blue or green coloured fluid phase and light specks of particles that are suspended in the coloured fluid phase.
  • the combination of the liquid component and the aminocarboxylate chelant forms a homogeneous fluid that contains the dye and that at the same time is capable of keeping the particles in suspension.
  • glycerol and aminocarboxylate chelants are hygroscopic ingredients that are capable of reducing the water activity of water containing compositions.
  • the pourable detergent suspension of the present invention comprises 85-99.2 wt.% of a dyed fluid phase and 0.8-15 wt.% of suspended, particles having a diameter in the range of 0.1 -2 mm, said suspension comprising:
  • liquid component selected from water, glycerol and mixtures thereof, said liquid component comprising 8-25% water and at least 20% glycerol, by weight of the detergent suspension;
  • the combination of the liquid component and the one or more aminocarboxylate chelants represents at least 60 wt.% of the detergent suspension; wherein the suspension has a water activity at 20°C of not more than 0.7; and wherein the dyed fluid phase has a reflective color represented by a chromaticity (a*), chromaticity (b*) and a lightness (L*) expressed by the CI E Lab color coordinate system meeting the following conditions:
  • the aminocarboxylate chelant renders the suspension sufficiently viscous to keep the particles in suspension.
  • the combination of aminocarboxylate chelant and glycerol ensures that even if the suspension contains a significant quantity of water activity can be reduced to 0.75 or less.
  • a low water activity is important, for instance, in case the particles contain moisture sensitive ingredients, such as bleaching agent or enzymes.
  • the invention also provides a packaged detergent product comprising a container and a suspension as described herein below, said container comprising a container wall and an outlet, and said suspension being contained inside the container, wherein at least a part of the container wall is translucent or transparent.
  • the invention also allows to provide for the suspension being packaged in a single dose unit such as a sachet (pouch) or capsule.
  • a first aspect of the invention relates to a pourable detergent suspension comprising 85-99.2 wt.% of a dyed fluid phase and 0.8-15 wt.% of suspended, particles having a diameter in the range of 0.1 -2 mm, said suspension comprising:
  • liquid component selected from water, glycerol and mixtures thereof, said liquid component comprising 8-25% water and at least 20% glycerol, by weight of the detergent suspension;
  • the combination of the liquid component and the one or more aminocarboxylate chelants represents at least 60 wt.% of the detergent suspension; wherein the suspension has a water activity at 20°C of not more than 0.7; and wherein the dyed fluid phase has a reflective color represented by a chromaticity (a * ), chromaticity (b * ) and a lightness (L * ) expressed by the CIE Lab color coordinate system meeting the following conditions:
  • pourable refers to a composition that is able to flow under ambient conditions.
  • Thixotropic compositions that can be rendered pourable by shear thinning are also regarded as pourable.
  • particles refers to a particulate matter in liquid or solid form, preferably solid form.
  • aminocarboxylate chelant refers to compounds containing one or more nitrogen atoms connected through carbon atoms to one or more carboxyl groups, which form strong complexes with metal ions by donation of electron pairs from the nitrogen and oxygen atoms to the metal ion to form multiple chelate rings.
  • thixotropic refers to compositions (e.g. gels or fluids) that are viscous under quiescent conditions and that become less viscous when shaken, agitated, or otherwise stressed. In thixotropic compositions, this so called “shear thinning effect" is reversible, i.e. the composition will return to a more viscous state once it is no longer subjected to shear stress.
  • a Lab color space is a color-opponent space with dimension L for lightness and a and b for the color-opponent dimensions, based on nonlinearly compressed (e.g. CI E XYZ color space) coordinates.
  • the L*a*b* color space includes all perceivable colors.
  • One of the most important attributes of the L*a*b*-model is device independence. This means that the colors are defined independent of their nature of creation or the device they are displayed on.
  • the red/green opponent colors are represented along the a* axis, with green at negative a* values and red at positive a* values.
  • the yellow/blue opponent colors are represented along the b* axis, with blue at negative b* values and yellow at positive b* values.
  • the scaling and limits of the a* and b* axes runs in the range of -100 to 100. Whenever reference is made herein to water content, unless indicated otherwise, said water content includes unbound (free) as well as bound water.
  • a parameter such as a concentration or a ratio
  • a certain upper limit it should be understood that in the absence of a specified lower limit the lower limit for said parameter is 0.
  • the quantified amount or quantified concentration relates to said component per se, even though it may be common practice to add such a component in the form of a solution or of a blend with one or more other ingredients.
  • the detergent suspension of the present invention preferably comprises 87-98.5 wt.% of a dyed fluid phase and 1 .5-13 wt.% of suspended, particles having a diameter in the range of 0.1 -2 mm. Most preferably, the detergent suspension comprises 90-98 wt.% of a dyed fluid phase and 2-12 wt.% of suspended, particles having a diameter in the range of 0.1 -2 mm.
  • the combination of glycerol, water and the one or more amincarboxylate chelants typically represent at least 63 wt.%, preferably at least 65 wt.% of the detergent suspension.
  • the detergent suspension typically has a water activity of 0.2 to 0.6 at 20°C. More preferably, the water activity of the detergent suspension at 20°C is in the range of 0.3 to 0.5, most preferably of 0.35 to 0.45.
  • the fluid phase of the detergent suspension of the present invention largely consists of glycerol, water and aminocarboxylate chelant.
  • the fluid phase may additionally contain liquid and non-liquid components in dissolved or non-dissolved form. Only dissolved components and non-dissolved components that are present as particles/droplets having a diameter of less than 100 ⁇ are considered as part of the fluid phase.
  • the combination of the liquid component and the one or more aminocarboxylate chelants represents at least 63 wt.%, more preferably at least 65 wt.% and most preferably at least 67-95 wt.% of the detergent suspension.
  • the detergent suspension of the present invention preferably contains water and the one or more aminocarboxylate chelants in a weight ratio of not more than 2:1 , preferably of not more than 1 .5:1 , most preferably of not more than 1 .2:1 . Water and the one or more
  • aminocarboxylate chelats are typically contained in the detergent suspension in a weight ratio of at least 1 :3, more preferably of at least 1 :2 and most preferably of at least 1 :1 .8.
  • the one or more dye substances are preferably contained in the detergent suspension in a concentration of 0.02-0.5 wt.%, more preferably of 0.03-0.3 wt.%.
  • the one or more dye substances employed in the detergent suspension preferably are water- soluble dye substances.
  • the one or more dye substances that are contained in the fluid phase of the detergent suspension are preferably at least partly present in the fluid phase in dissolved form. More preferably, at least 50 wt.% of the one or more dye substances is dissolved in the fluid phase at 20°C.
  • the fluid phase can suitably contain other detergent ingredients besides the liquid
  • aminocarboxylate chelant examples include surfactants, anti-scaling agents, glass corrosion inhibitors, anti- tarnishing agents, perfumes and combinations thereof.
  • the detergent suspension contains at least 0.5 wt.%, more preferably at least 0.8 wt.% and most preferably at least 1 .5 wt.% of particles having a diameter of 0.2-1 .5 mm.
  • the particles preferably do not contain added dye substances.
  • the particles preferably contain less than 0.01 wt.%, more preferably less than 0.001 wt.% of dye substances.
  • the particles in the detergent suspension preferably contain at least 50 wt.% of solid component selected from bleaching agents, bleach activators, water-soluble salts, carbohydrates, enzymes and combinations thereof. According to a particularly preferred embodiment, the particles are white or off-white.
  • Solid component selected from bleaching agents, bleach activators, water-soluble salts, carbohydrates, enzymes and combinations thereof. According to a particularly preferred embodiment, the particles are white or off-white.
  • the detergent suspension preferably contains 40-70 wt.%, more preferably 43-67 wt.% and most preferably 45-65 wt.% of the liquid component.
  • Glycerol and water are preferably contained in the pourable detergent suspension in a weight ratio that lies within the range of 2:3 to 1 :6, more preferably within the range of 1 :2 to 1 :5, most preferably within the range of 1 :2.2 to 1 :4.
  • the pourable detergent suspension preferably contains up to 75 wt.%, more preferably 30-60 wt.% and most preferably 32-50 wt.% glycerol.
  • the water content of the detergent suspension preferably is in the range of 10-22 wt.% and most preferably in the range of 12-20 wt.%.
  • the pourable detergent suspension preferably contains at least 10 wt.%, more preferably 12- 35 wt.% and most preferably 13-30 wt.% of the one or more aminocarboxylate chelants.
  • the one or more aminocarboxylate chelants are selected from glutamic acid N,N- diacetic acid (GLDA), methylglycinediacetic acid (MGDA), iminodisuccinic acid (IDS), ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DTPA), hydroxyethyliminodiacetic acid (HEIDA), Nitrilotriacetic acid (NTA), aspartic acid
  • GLDA glutamic acid N,N- diacetic acid
  • MGDA methylglycinediacetic acid
  • IDS iminodisuccinic acid
  • EDTA ethylenediaminetetraacetic acid
  • DTPA diethylenetriaminepentaacetic acid
  • HEIDA hydroxyethyliminodiacetic acid
  • NTA Nitrilotriacetic acid
  • AES diethoxysuccinic acid
  • ASDA -diacetic acid
  • HEDTA hydroxyethylenediaminetetraacetic acid
  • HEEDTA hydroxyethylethylenediaminetriacetic acid
  • IDF iminodifumaric
  • I DT iminoditartaric acid
  • I DMAL iminodimalic acid
  • EDDF ethylenediaminedifumaric acid
  • EDDM ethylenediamineditartaric acid
  • EDDS ethylenediaminedisuccinic acid
  • EDDMAL dipicolinic acid, and their salts.
  • the one or more aminocarboxylate chelants are selected from GLDA, MGDA, IDS, HEI DA, EDDS and NTA, and their salts. In an even more preferred embodiment, the one or more aminocarboxylate chelants are selected from GLDA, MGDA, I DS and their salts. Most preferably, the the one or more aminocarboxylate chelants are selected from GLDA and salts thereof.
  • the GLDA employed in the present suspension preferably is an alkali metal salt of glutamic- ⁇ , ⁇ -diacetic acid. More preferably, the GLDA employed is a sodium salt of glutamic-N,N- diacetic acid. Most preferably, the GLDA employed is a tetra sodium salt of glutamic-N,N- diacetic acid.
  • the present detergent suspension preferably contains 0.5-30 wt.% of one or more
  • surfactants within the invention, are components within the classification as described in "Surfactant Science Series", Vol.82, Handbook of detergents, part A: Properties, chapter 2 (Surfactants, classification), G. Broze (ed.).
  • the detergent composition contains 0.5-30 wt.%, preferably 1 -20 wt.%, more preferably 1 .3-10 wt.% of one or more surfactants.
  • the surfactants are selected from one or more non- ionic surfactants.
  • the composition contains 0.1 -15 wt.%, more preferably 0.5-10 wt.% and most preferably 1 -5 wt.% of a nonionic surfactant or a mixture of two or more non-ionic surfactants.
  • nonionic surfactants that may be employed in the present composition include the condensation products of hydrophobic alkyl, alkenyl, or alkyl aromatic compounds bearing functional groups having free reactive hydrogen available for condensation with hydrophilic alkylene oxide, such as ethylene oxide, propylene oxide, butylene oxide, polyethylene oxide or polyethylene glycol to form nonionic surfactants.
  • functional groups include hydroxy, carboxy, mercapto, amino or amido groups.
  • Examples of useful hydrophobes of commercial nonionic surfactants include C8-C18 alkyl fatty alcohols, C8-C14 alkyl phenols, C8-C18 alkyl fatty acids, C8-C18 alkyl mercaptans, C8- C18 alkyl fatty amines, C8-C18 alkyl amides and C8-C18 alkyl fatty alkanolamides.
  • suitable ethoxylated fatty alcohols may be chosen from ethoxylated cetyl alcohol, ethoxylated ketostearyl alcohol, ethoxylated isotridecyl alcohol, ethoxylated lauric alcohol, ethoxylated oleyl alcohol and mixtures thereof.
  • suitable nonionic surfactants for use in the invention are found in the low- to non-foaming ethoxylated/ propoxylated straight- chain alcohols of the PlurafacTM LF series, supplied by the BASF and the SynperonicTM NCA series supplied by Croda.
  • end-capped ethoxylated alcohols available as the SLF 18 series from BASF and the alkylpolyethylene glycol ethers made from a linear, saturated C16-C18 fatty alcohol of the LutensolTM AT series, supplied by BASF.
  • suitable nonionics to apply in the composition of the invention are modified fatty alcohol polyglycolethers available as DehyponTM 3697 GRA or DehyponTM Wet from BASF/Cognis.
  • nonionics from the LutensolTM TO series of BASF which are alkylpolyethylene glycol ethers made from a saturated iso-C13 alcohol.
  • Amineoxide surfactants may also be used in the present invention as anti- redeposition surfactant.
  • Suitable amineoxide surfactants are C10-C15 alkyl dimethylamine oxide and C10-C15 acylamido alkyl dimethylamine oxide.
  • the inventors have found that, a detergent composition that is not only chemically but also physically very stable can be produced if the nonionic surfactant employed is solid at ambient temperature.
  • the present composition contains 0.1 -30 wt.%, more preferably 0.5-20 wt.%, further preferred 1 - 10 wt.%, and most preferably 1 -5 wt.% of nonionic surfactant that is solid at 25°C.
  • the total amount present preferably is less than 5 wt.%, and more preferably not more than 2 wt.%. Furthermore, if an anionic surfactant is present, it is preferred that an antifoam agent to suppress foaming is present.
  • suitable anionic surfactants are methylester sulphonates or sodium lauryl sulphate. It is preferred that no anionic surfactant is present in the composition of the current invention.
  • the detergent suspension of the present invention contains a structuring biopolymer.
  • biopolymer that is capable of structuring water (e.g. through gelation) makes it possible to prepare a fluid product with excellent rheological properties.
  • the pourable product contains at least 0.1 % of structuring biopolymer by weight of water. Even more preferably, the product contains 0.2-3%, most preferably 0.3-2% of structuring biopolymer by weight of water.
  • structuring biopolymers that can be employed include xanthan gum, locust bean gum, guar gum, gum Arabic, gellan gum, carrageenan, carboxmethyl cellulose, microcrystalline cellulose, microfibrous cellulose and combinations thereof. More preferably, the structuring biopolymer is selected from xanthan gum, guar gum, carboxymethyl cellulose, microfibrous cellulose and combinations thereof. Most preferably, the structuring biopolymer is xanthan gum. Builders
  • the pourable detergent suspension may contain additional water-softening builders.
  • phosphorous based builders such as phosphates have been used as builders, but due to environmental pressures other builders are preferred.
  • organic builders such as citrate and inorganic builders such as carbonates, in particular sodium carbonate.
  • Citrate is preferably contained in the pourable detergent suspension in a concentration of 0.1 - 4 wt.%, more preferably of 0.2-2 wt.%, most preferably of 0.25-1 .2 wt.% citric acid equivalent.
  • the detergent suspension contains 3-30 wt.%, more preferably 5-25 wt.%, most preferably 7-20 wt.% of sodium carbonate.
  • Silicates may be added to the formulation.
  • Silicates can act as builder, buffering agent or article care agent.
  • Preferred silicates are sodium silicate such as sodium disillicate, sodium metasilicate and crystalline phyllosilicates and mixtures thereof.
  • Silicates are preferably used in the detergent suspension in a concentration of 0.5 to 8%, more preferably of 0.8 to 6% by weight of the suspension.
  • enzymes suitable for use in the detergent suspension of this invention include lipases, cellulases, peroxidases, proteases (proteolytic enzymes), amylases (amylolytic enzymes) and others which degrade, alter or facilitate the degradation or alteration of biochemical soils and stains encountered in cleansing situations so as to remove more easily the soil or stain from the object being washed to make the soil or stain more removable in a subsequent cleansing step. Both degradation and alteration can improve soil removal.
  • the one or more active enzymes contained in the present suspension are selected from protease, amylase, cellulase, peroxidase, mannanase, pectate lyase and lipase. Most preferably, the active enzyme is selected from protease, amylase and combinations thereof.
  • the suspension of the present invention typically contains at least 10 mg/kg, more preferably at least 20 mg/kg, even more preferably at least 50 mg/kg and most preferably at least 100 mg/kg of active enzyme.
  • the concentration of active enzyme preferably does not exceed 50 g/kg, more preferably it does not exceed 40 g/kg and most preferably it does not exceed 30 g/kg.
  • the suspension contains at least 10 mg/kg, more preferably at least 20 mg/kg and most preferably at least 50 mg/kg of active amylase.
  • the suspension contains at least 100 mg/kg, more preferably at least 200 mg/kg and most preferably at least 400 mg/kg of active protease.
  • Enzymes may be added in liquid or in encapsulated form.
  • encapsulated enzymes are enzyme granule types D, E and HS by Genencor and granule types , T, GT, TXT and EvityTM of Novozymes.
  • proteolytic enzymes in this invention include metal loproteases and serine proteases, including neutral or alkaline microbial serine protease, such as subtilisins (EC 3.4.21 .62).
  • the proteolytic enzymes for use in the present invention can be those derived from bacteria of fungi. Chemically or genetically modified mutants (variants) are included.
  • Preferred proteolytic enzymes are those derived from
  • Bacillus such as B. lentus, B. gibsonii, B. subtilis, B. licheniformis, B. alkalophilus, B.
  • amyloliquefaciens and Bacillus pumilus of which B. lentus and B. gibsonii are most preferred.
  • proteolytic enzymes are ExcellaseTM, ProperaseTM, PurafectTM, PurafectTM Prime, PurafectTM Ox by Genencor; and those sold under the trade names BlazeTM,
  • OvozymeTM SavinaseTM, AlcalaseTM, EverlaseTM, EsperaseTM, RelaseTM, PolarzymeTM, LiquinaseTM and CoronaseTM by Novozymes.
  • amylolytic enzymes for use in the present invention can be those derived from bacteria or fungi. Chemically or genetically modified mutants (variants) are included.
  • Preferred amylolytic enzyme is an alpha-amylase derived from a strain of Bacillus, such as B. subtilis, B.
  • amylolytic enzymes are produced and distributed under the trade name of StainzymeTM, StainzymeTM Plus, TermamylTM, NatalaseTM and DuramylTM by Novozymes; as well as PoweraseTM, PurastarTM, PurastarTM Oxam by Genencor. StainzymeTM, StainzymeTM Plus and PoweraseTM are the preferred amylases.
  • the suspension contains active protease and the protease activity of the freshly prepared suspension decreases by not more than 70%, more preferably by not more than 50% and most preferably by not more than 20% when the suspension is stored in a closed container for 8 weeks at 20 °C.
  • Well known enzyme stabilizers such as polyalcohols/borax, calcium, formate or protease inhibitors like 4-formylphenyl boronic acid may also be present in the suspension.
  • the present detergent suspension preferably contains at least 0.3 wt.%, more preferably 1 -15 wt.% and most preferably 2-12 wt.% of bleaching agent.
  • the bleaching agent may suitably comprise a chlorine-, or bromine-releasing agent or a peroxygen compound.
  • the bleaching agent is selected from peroxides (including peroxide salts such as sodium percarbonate), organic peracids, salts of organic peracids and combinations thereof. More preferably, the bleaching agent is a peroxide. Most preferably, the bleaching agent is a percarbonate.
  • peroxides are acids and corresponding salts of monopersulphate, perborate monohydrate, perborate tetrahydrate, and percarbonate.
  • Organic peracids useful herein include alkyl peroxy acids and aryl peroxyacids such as peroxybenzoic acid and ring substituted peroxybenzoic acids (e.g. peroxy-alpha- naphthoic acid), aliphatic and substituted aliphatic monoperoxy acids (e.g. peroxylauric acid and peroxystearic acid), and phthaloyl amido peroxy caproic acid (PAP).
  • peroxybenzoic acid and ring substituted peroxybenzoic acids e.g. peroxy-alpha- naphthoic acid
  • aliphatic and substituted aliphatic monoperoxy acids e.g. peroxylauric acid and peroxystearic acid
  • PAP phthaloyl amido peroxy caproic acid
  • diperoxy acids useful herein include alkyl diperoxy acids and aryldiperoxy acids, such as 1 , 12 di-peroxy-dodecanedioic acid (DPDA), 1 ,9 diperoxyazelaic acid, diperoxybrassylic acid, diperoxysebacic acid and diperoxy-isophthalic acid, and 2 decyldiperoxybutane 1 ,4 dioic acid.
  • DPDA di-peroxy-dodecanedioic acid
  • the detergent suspension of the present invention preferably contains bleaching agent in the form of particles. More preferably, the suspension contains 0.3-15 wt.%, more preferably 0.5- 10 wt.% of particles of bleaching agent. According to a preferred embodiment, the particles of bleaching agent are coated particles comprising one or more core particles that contain the bleaching agent, which one or more core particles are enclosed by a water-soluble coating. The water-soluble coating
  • a coating agent selected from alkali sulphate, alkali carbonate or alkali chloride and combinations thereof.
  • the detergent suspension may contain one or more bleach activators such as peroxyacid bleach precursors.
  • Peroxyacid bleach precursors are well known in the art. As non-limiting examples can be named ⁇ , ⁇ , ⁇ ', ⁇ '-tetraacetyl ethylene diamine (TAED), sodium
  • SNOBS nonanoyloxybenzene sulphonate
  • a bleach catalyst such as the manganese complex, e.g. Mn-Me TACN, as described in EP-A-0458397, or the sulphonimines of US-A-5,041 ,232 and US-A- 5,047,163, can be incorporated.
  • Cobalt or iron catalysts can also be used.
  • the detergent suspension may suitably contain one or more dispersing polymers.
  • Dispersing polymers as referred to in this invention are chosen from the group of anti-spotting agents and/or anti-scaling agents.
  • Suitable anti-spotting polymeric agents include hydrophobically modified polycarboxylic acids such as AcusolTM 460 ND (ex Dow) and AlcosperseTM 747 by
  • AkzoNobel whereas also synthetic clays, and preferably those synthetic clays which have a high surface area are very useful to prevent spots, in particular those formed where soil and dispersed remnants are present at places where the water collects on the glass and spots formed when the water subsequently evaporates.
  • suitable anti-scaling agents include organic phosphonates, amino carboxylates, polyfunctionally-substituted compounds, and mixtures thereof.
  • Particularly preferred anti-scaling agents are organic phosphonates such as alpha-hydroxy-2 phenyl ethyl diphosphonate, ethylene diphosphonate, hydroxy 1 ,1 - hexylidene, vinylidene 1 , 1 -diphosphonate, 1 ,2-dihydroxyethane 1 ,1 -diphosphonate and hydroxy-ethylene 1 , 1 - diphosphonate.
  • organic phosphonates such as alpha-hydroxy-2 phenyl ethyl diphosphonate, ethylene diphosphonate, hydroxy 1 ,1 - hexylidene, vinylidene 1 , 1 -diphosphonate, 1 ,2-dihydroxyethane 1 ,1 -diphosphonate and hydroxy-ethylene 1 , 1 - diphosphonate.
  • EDHP hydroxy-ethylene 1 , 1 - diphosphonate
  • 2- phosphono-butane 1 ,2,4-tricar
  • Suitable anti-scaling agents are water soluble dispersing polymers prepared from an allyloxybenzenesulfonic acid monomer, a methallyl sulfonic acid monomer, a copolymerizable nonionic monomer and a copolymerizable olefinically unsaturated carboxylic acid monomer as described in US 5 547 612 or known as acrylic sulphonated polymers as described in EP 851 022.
  • Polymers of this type include polyacrylate with methyl methacrylate, sodium methallyl sulphonate and sulphophenol methallyl ether such as AlcosperseTM 240 supplied (AkzoNobel).
  • terpolymer containing polyacrylate with 2-acrylamido-2 methylpropane sulphonic acid such as Acumer 3100 supplied by Dow.
  • polymers and co-polymers of acrylic acid having a molecular weight between 500 and 20,000 can also be used, such as homo-polymeric polycarboxylic acid compounds with acrylic acid as the monomeric unit.
  • the average weight of such homo-polymers in the acid form preferably ranges from 1 ,000 to 100,000 particularly from 3,000 to 10,000 e.g. SokolanTM PA 25 from BASF or AcusolTM 425 from Dow.
  • polycarboxylates co-polymers derived from monomers of acrylic acid and maleic acid such as CP 5 from BASF.
  • the average molecular weight of these polymers in the acid form preferably ranges from 4,000 to 70,000.
  • SokalanTMCP42 SokalanTM CP50 from BASF or AlcoguardTM 4160 from AkzoNobel may also be used.
  • Mixture of anti-scaling agents may also be used. Particularly useful is a mixture of organic phosphonates and polymers of acrylic acid. It is preferable if the level of dispersing polymers ranges from 0.2 to 10 wt.% of the total suspension, preferably from 0.5 to 8 wt.%, and further preferred from 1 to 6 wt.%.
  • Glass corrosion inhibitors can prevent the irreversible corrosion and iridescence of glass surfaces in machine dishwash detergents.
  • the detergent suspension may suitably contain glass corrosion inhibitors.
  • Suitable glass corrosion agents can be selected from the group the group consisting of salts of zinc, bismuth, aluminum, tin, magnesium, calcium, strontium, titanium, zirconium, manganese, lanthanum, mixtures thereof and precursors thereof. Most preferred are salts of bismuth, magnesium or zinc or combinations thereof.
  • Preferred levels of glass corrosion inhibitors in the present suspension are 0.01 -2 wt.%, more preferably 0.1 - 0.5 wt.%.
  • Anti-tarnishing agents may prevent or reduce the tarnishing, corrosion or oxidation of metals such as silver, copper, aluminium and stainless steel.
  • Anti-tarnishing agents such as benzotriazole or bis-benzotriazole and substituted or substituted derivatives thereof and those described in EP 723 577 (Unilever) may also be included in the suspension.
  • Other anti- tarnishing agents that may be included in the detergent suspension are mentioned in WO 94/26860 and WO 94/26859.
  • Suitable redox active agents are for example complexes chosen from the group of cerium, cobalt, hafnium, gallium, manganese, titanium, vanadium, zinc or zirconium, in which the metal are in the oxidation state of II , II , IV V or VI .
  • the formulation such as perfume, colorant or preservatives.
  • the desired viscosity profile of the detergent suspension depends on the end use of the product. It may be a liquid, gel or a paste depending on the application. Rheology
  • the detergent suspension is a thixotropic composition.
  • thixotropic means that the product is viscous under quiescent conditions and become less viscous when shaken, agitated, or otherwise stressed.
  • compositions this so called “shear thinning effect" is reversible, i.e. the composition will return to a more viscous state once it is no longer subjected to shear stress.
  • This thixotropic behavior of the detergent suspension can be demonstrated by measuring the storage modulus (G') and the loss modulus (G") of the product as a function of angular frequency ( ⁇ ) on a rheometer in oscillatory mode. Both G' and G" of the pourable product increase as a function of angular frequency ( ⁇ ), be it that G" increases at a faster rate than G'.
  • angular frequency ( ⁇ ) G" of the pourable product is lower than G', but at an ⁇ in the range of 0.05-50 rad/s G" surpasses G'.
  • Both the storage modulus (G') and the loss modulus (G") of the pourable product are determined at 20°C using Anton Paar® MCR 302 rheometer, using plate-plate geometry, spindle PP50/S (sandblasted) and a gap size of 3mm. The program settings applied are as follows:
  • the setting in which the measuring points are gathered is the 'no time settings'. In this modus the apparatus waits for a steady state situation before it takes his measuring point. ⁇ Every decade six measuring points are taken.
  • oscillatory rheology it is possible to quantify both the viscous-like and the elastic-like properties of a material at different time scales.
  • the basic principle of an oscillatory rheometer is to induce a sinusoidal shear deformation in the sample and measure the resultant stress response; the time scale probed is determined by the frequency of oscillation, ⁇ , of the shear deformation.
  • the stress in the sample is proportional to the rate of strain deformation, where the proportionality constant is the viscosity of the fluid.
  • Viscoelastic materials show a response that contains both in-phase and out-of-phase contributions. These contributions reveal the extents of solid-like and liquid-like behavior. As a consequence, the total stress response shows a phase shift ⁇ with respect to the applied strain deformation that lies between that of solids and liquids, 0 ⁇ /2.
  • the viscoelastic behaviour of the system at ⁇ is characterised by the storage modulus, G'(oo), and the loss modulus, ⁇ "( ⁇ ), which respectively characterise the solid-like and fluid-like contributions to the measured stress response.
  • the detergent suspension is a thixotropic suspension having a storage modulus at 20°C (G'(oo)) and a loss modulus at 20°C (G" ( ⁇ )), both moduli measured as a function of angular frequency ( ⁇ ) on a rheometer in oscillatory mode operating at a strain of 0.1 %, wherein:
  • a detergent suspension having a storage modulus (G') and a loss modulus (G") that meet at least one of the following conditions:
  • the pourable detergent suspension typically has a storage modulus (G') at 0.2 rad/s in the range of 1 to 100 Pa, more preferably in the range of 8 to 30 Pa, most preferably in the range of 10 to 20 Pa.
  • the loss modulus (G") of the pourable detergent suspension at 0.2 rad/s preferably is in the range of 1 to 100 Pa, more preferably in the range of 3 to 60 Pa, most preferably in the range of 8 to 30 Pa.
  • the pourable detergent composition is in particular suitable to be packaged in a container comprising a container wall and an outlet, such as a bottle, to allow adaptation of the detergent dosing to the amount of soil on the dish ware.
  • a container or bottle is suitable for multiple use.
  • the container has at least one translucent outer wall.
  • the pourable detergent composition can be packaged in a container suitable for single use.
  • such a single use container holds one unit of the detergent formulation and is at least partly made from water-soluble material.
  • Examples of containers that may be used in accordance with this embodiment are sachets (pouches) and capsules.
  • the single use container is not only water-insoluble, but also water-permeable. More particularly, it is preferred that the container is made of a water-permeable and water-soluble polymer selected from polyvinyl alcohol, cellulose ethers, polyethylene oxide, starch, polyvinylpyrrolidone, polyacrylamide, polyvinyl methyl ether-maleic anhydride, polymaleic anhydride, styrene maleic anhydride, hydroxyethylcellulose, methylcellulose, polyethylene glycols, carboxymethylcelluloseose, polyacrylic acid salts, alginates, acrylamide copolymers, guar gum, casein, ethylene-maleic anhydride resin series, polyethylene imine, ethyl hydroxyethylcellulose, ethyl methylcellulose, hydroxyethyl methylcellulose and combinations thereof. Even more preferably, the single use container is made of polyvinyl alcohol, polyethelene oxide, polyvinylpyrrolidone
  • the single use container is made of a water-permeable and water-insoluble polymer selected from butyral resin, polyvinyl acetal, polyvinyl butyral-co- vinyl alcohol-co-vinyl acetate), polyvinyl butyrate, polyvinyl acetate and combinations and co- monomers thereof.
  • a water-permeable and water-insoluble polymer selected from butyral resin, polyvinyl acetal, polyvinyl butyral-co- vinyl alcohol-co-vinyl acetate), polyvinyl butyrate, polyvinyl acetate and combinations and co- monomers thereof.
  • the single use container is made of polyvinyl alcohol, a copolymer of polyvinyl alcohol and combinations thereof.
  • Polyvinyl alcohols preferred have a weight average molecular weight between 1 ,000 and 300,000, more preferably, between 2,000 and 150,000, and most preferably, between 3,000 and 100,000.
  • the container comprises 5-40 ml, more preferably 8-30- ml and most preferably 10-20-ml of the detergent formulation.
  • a thixotropic machine dishwashing product was prepared on the basis of the recipe that is shown in Table 1 .
  • Table 1 A thixotropic machine dishwashing product was prepared on the basis of the recipe that is shown in Table 1 .
  • the product was prepared as follows: a liquid premix was made by mixing glycerol and xanthan gum to a homogeneous suspension. Next, water was added under constant stirring. After that DissolvineTM GL 47-S and citric acid were dosed at ambient temperature. Next, the DissolvineTM PD-S was mixed in. Finally the remaining ingredients were added to the mix under stirring. All ingredients were mixed in under vacuum to minimize formation of air bubbles.
  • the product so obtained was filled into a bottle made of transparent polypropylene.
  • the detergent product was a stable suspension that did not suffer from phase separation or sedimentation when stored under ambient conditions.
  • the product had a very attractive blue colour and showed light specks percarbonate particles suspended in blue fluid.
  • the product was quite viscous but could be poured from the bottle without any problems.

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Abstract

L'invention concerne une suspension de détergent pouvant être versée comprenant 85-99,2 % d'une phase fluide colorée et 0,8-15 % en poids de particules en suspension présentant un diamètre dans la plage de 0,1-2 mm, ladite suspension comprenant : • 35-75 % en poids de constituant liquide choisi parmi l'eau, le glycérol et des mélanges correspondants, ledit constituant liquide comprenant 8-25 % d'eau et au moins 20 % de glycérol, en poids de la suspension de détergent ; • 8-50 % en poids d'un ou de plusieurs agents chélatants de type aminocarboxylate ; • 0,01-1 % en poids d'une ou plusieurs substances colorantes ; la combinaison du constituant liquide et dudit un ou desdits plusieurs agents chélatants de type aminocarboxylate représentant au moins 60 % en poids de la suspension de détergent ; la suspension présentant une activité de l'eau à 20°C ne dépassant pas 0,7 ; et la phase fluide colorée présentant une couleur réfléchissante représentée par une chromaticité (a*), une chromaticité (b*) et une clarté (L *), exprimées par le système de coordonnées de couleur CIE Lab répondant aux conditions suivantes : (a* + b*) ≤ 20 ; 20 ≤ L* ≤ 60 ; et à au moins l'une des conditions suivantes : b* ≤ 0 ; -40 ≤ a* ≤ 50 ; (a* + b*) ≤ 0 ; 25 ≤ L* ≤ 50. La composition de détergent pouvant être versée combine un aspect visuel très attrayant avec une stabilité élevée et est facile à fabriquer.
PCT/EP2017/054722 2016-03-02 2017-03-01 Suspension de détergent pouvant être versée, comprenant une phase fluide colorée et des particules en suspension WO2017148989A1 (fr)

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Citations (16)

* Cited by examiner, † Cited by third party
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US4751015A (en) 1987-03-17 1988-06-14 Lever Brothers Company Quaternary ammonium or phosphonium substituted peroxy carbonic acid precursors and their use in detergent bleach compositions
US5041232A (en) 1990-03-16 1991-08-20 Lever Brothers Company, Division Of Conopco, Inc. Sulfonimines as bleach catalysts
US5047163A (en) 1990-03-16 1991-09-10 Lever Brothers Company, Division Of Conopco, Inc. Activation of bleach precursors with sulfonimines
EP0458397A2 (fr) 1990-05-21 1991-11-27 Unilever N.V. Activation du blanchiment
WO1994026860A1 (fr) 1993-05-08 1994-11-24 Henkel Kommanditgesellschaft Auf Aktien Produits de protection de l'argent contre la corrosion ii
WO1994026859A1 (fr) 1993-05-08 1994-11-24 Henkel Kommanditgesellschaft Auf Aktien Produit i de protection de l'argent contre la corrosion
EP0723577A1 (fr) 1993-10-14 1996-07-31 Unilever N.V. Compositions detergentes contenant des agents empechant le ternissement de l'argent
US5547612A (en) 1995-02-17 1996-08-20 National Starch And Chemical Investment Holding Corporation Compositions of water soluble polymers containing allyloxybenzenesulfonic acid monomer and methallyl sulfonic acid monomer and methods for use in aqueous systems
EP0851022A2 (fr) 1996-12-23 1998-07-01 Unilever N.V. Compositions de rincage contenant des polymères antitartres
EP1129160A1 (fr) 1998-11-12 2001-09-05 Henkel Kommanditgesellschaft auf Aktien Detergents aqueux pour lave-vaisselle
US20100081600A1 (en) 2008-09-30 2010-04-01 Jean-Pol Boutique Liquid detergent compositions exhibiting two or multicolor effect
WO2013092276A1 (fr) 2011-12-22 2013-06-27 Unilever N.V. Composition détergente comprenant du n,n-diacétate d'acide glutamique, de l'eau et un agent de blanchiment
WO2013160023A1 (fr) * 2012-04-23 2013-10-31 Unilever Plc Compositions de détergent pour lessive liquide isotrope aqueux structuré de façon externe
WO2014107578A1 (fr) 2013-01-03 2014-07-10 Basf Corporation Composition détergente homogène
WO2015181570A1 (fr) 2014-05-30 2015-12-03 Reckitt Benckiser (Brands) Limited Composition de détergent améliorée
DE102014212643A1 (de) 2014-06-30 2015-12-31 Henkel Ag & Co. Kgaa Flüssiges Reinigungsmittel enthaltend flüssige und feste Enzymformulierungen

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4751015A (en) 1987-03-17 1988-06-14 Lever Brothers Company Quaternary ammonium or phosphonium substituted peroxy carbonic acid precursors and their use in detergent bleach compositions
US5041232A (en) 1990-03-16 1991-08-20 Lever Brothers Company, Division Of Conopco, Inc. Sulfonimines as bleach catalysts
US5047163A (en) 1990-03-16 1991-09-10 Lever Brothers Company, Division Of Conopco, Inc. Activation of bleach precursors with sulfonimines
EP0458397A2 (fr) 1990-05-21 1991-11-27 Unilever N.V. Activation du blanchiment
WO1994026860A1 (fr) 1993-05-08 1994-11-24 Henkel Kommanditgesellschaft Auf Aktien Produits de protection de l'argent contre la corrosion ii
WO1994026859A1 (fr) 1993-05-08 1994-11-24 Henkel Kommanditgesellschaft Auf Aktien Produit i de protection de l'argent contre la corrosion
EP0723577A1 (fr) 1993-10-14 1996-07-31 Unilever N.V. Compositions detergentes contenant des agents empechant le ternissement de l'argent
US5547612A (en) 1995-02-17 1996-08-20 National Starch And Chemical Investment Holding Corporation Compositions of water soluble polymers containing allyloxybenzenesulfonic acid monomer and methallyl sulfonic acid monomer and methods for use in aqueous systems
EP0851022A2 (fr) 1996-12-23 1998-07-01 Unilever N.V. Compositions de rincage contenant des polymères antitartres
EP1129160A1 (fr) 1998-11-12 2001-09-05 Henkel Kommanditgesellschaft auf Aktien Detergents aqueux pour lave-vaisselle
US20100081600A1 (en) 2008-09-30 2010-04-01 Jean-Pol Boutique Liquid detergent compositions exhibiting two or multicolor effect
WO2013092276A1 (fr) 2011-12-22 2013-06-27 Unilever N.V. Composition détergente comprenant du n,n-diacétate d'acide glutamique, de l'eau et un agent de blanchiment
WO2013160023A1 (fr) * 2012-04-23 2013-10-31 Unilever Plc Compositions de détergent pour lessive liquide isotrope aqueux structuré de façon externe
WO2014107578A1 (fr) 2013-01-03 2014-07-10 Basf Corporation Composition détergente homogène
WO2015181570A1 (fr) 2014-05-30 2015-12-03 Reckitt Benckiser (Brands) Limited Composition de détergent améliorée
DE102014212643A1 (de) 2014-06-30 2015-12-31 Henkel Ag & Co. Kgaa Flüssiges Reinigungsmittel enthaltend flüssige und feste Enzymformulierungen

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G. BROZE: ""Surfactant Science Series", Vol.82, Handbook of detergents, part A: Properties", vol. 82, article "chapter 2 (Surfactants, classification)"

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