EP3415605A1

EP3415605A1 - Water-soluble unit dose article comprising a solid laundry detergent composition

Info

Publication number: EP3415605A1
Application number: EP17176203.2A
Authority: EP
Inventors: Nigel Patrick Somerville Roberts; Alan Thomas Brooker; Carly Pickering; Ned Peter BUIJS
Original assignee: Procter and Gamble Co
Current assignee: Procter and Gamble Co
Priority date: 2017-06-15
Filing date: 2017-06-15
Publication date: 2018-12-19
Also published as: WO2018231886A1

Abstract

Water-soluble unit dose article comprising a water-soluble film and containing a solid laundry detergent composition and an encapsulated perfume. The solid composition is formulated to provide a relatively low pH upon dilution.

Description

FIELD OF THE INVENTION

The present invention relates to water-soluble unit dose articles containing solid laundry detergent compositions and methods of using them.

BACKGROUND OF THE INVENTION

Water-soluble laundry unit dose articles are known and are liked by consumers due to their ease and efficiency of use in the laundry operation. Water-soluble unit dose articles comprise water-soluble film defining at least one internal compartment. A laundry detergent composition is housed within the internal compartment. Upon exposure to water, the water-soluble film dissolves/disintegrates releasing the laundry detergent composition into the surrounding water.
The laundry detergent composition may be a solid laundry detergent composition. Such detergent compositions comprise known laundry detergent treatment actives. One preferred active ingredient is a core/shell perfume capsule.
Due to their compact form, water-soluble unit dose articles have limited space for formulating the solid laundry detergent compositions. This can result in lower than desired cleaning performance as extra detergent composition cannot simply be added to compensate for any under-performance. Addition of further detergent composition to the water-soluble unit dose article would require making the unit dose article bigger making it less convenient and also could contribute to negatives such as impaired dissolution when additional water soluble film would be required to accommodate the bigger water soluble unit dose article and/or reduced structural stability of the unit dose article especially when further stretching the original water soluble film to accommodate the bigger water soluble unit dose article (the film may not provide sufficient structural stability for the volume of solid detergent composition added).
Therefore, there is a need in the art to provide improved performance of said water-soluble unit dose articles without addition of increased levels of solid laundry detergent composition to the unit dose articles.
It was surprisingly found that a water-soluble unit dose article comprising a solid laundry detergent composition having a particular pH (upon dilution of the solid laundry detergent composition) provided improved fabric freshness performance of a core/shell perfume capsule formulated into said solid laundry detergent composition as compared to water-soluble unit dose articles having a solid laundry detergent composition having a higher pH (upon dilution of the solid laundry detergent composition) as known from the art.

SUMMARY OF THE INVENTION

A first aspect of the present invention is a water-soluble unit dose article comprising a water-soluble film and a solid laundry detergent composition, wherein the water-soluble film defines a first internal compartment and wherein the solid laundry detergent composition is comprised within the first internal compartment, and wherein the water soluble unit dose article composition comprises a capsule, wherein the capsule comprises a shell and a core wherein the core comprises a perfume; and
wherein the solid composition at 1wt% dilution in deionized water at 20°C, has an equilibrium pH in the range of from 6.5 to 9.0, preferably between 6.7 and 8.8.
A second aspect of the present invention is a method of washing comprising the steps of adding the water-soluble unit dose article according to the present invention to sufficient water to dilute the solid laundry detergent composition by a factor of at least 300 fold to create a wash liquor and contacting fabrics to be washed with said wash liquor.
A third aspect of the present invention is the use of a solid laundry detergent composition comprising a non-soap surfactant and having at 1wt% dilution in deionized water at 20°C an equilibrium pH in the range of from 6.5 to 9.0 in a water-soluble unit dose article to improve the performance of a capsule wherein the capsule comprises a shell and a core wherein the core comprises a perfume.

DETAILED DESCRIPTION OF THE INVENTION

Water-soluble unit dose article

The present invention is to a water-soluble unit dose article comprising a water-soluble film and a solid laundry detergent composition.
The water-soluble film is described in more detail below.
The solid laundry detergent composition is described in more detail below.
The water-soluble unit dose article comprises the water-soluble film shaped such that the unit-dose article comprises at least a first internal compartment surrounded by the water-soluble film. The compartment should be understood as meaning a closed internal space within the unit dose article, which holds the solid laundry detergent composition. The unit dose article may comprise a first water-soluble film and a second water-soluble film sealed to one another such to define the internal compartment. The water-soluble unit dose article is constructed such that the solid laundry detergent composition is comprised within the first internal compartment. The water-soluble unit dose article is constructed such that the solid laundry detergent composition does not leak out of the compartment during storage. However, upon addition of the water-soluble unit dose article to water, the water-soluble film dissolves and releases the contents of the internal compartment into the wash liquor.
During manufacture, a first water-soluble film may be shaped to comprise an open compartment into which the solid laundry detergent composition is added. A second water-soluble film is then laid over the first film in such an orientation as to close the opening of the compartment. The first and second films are then sealed together along a seal region.
The unit dose article may comprise more than one compartment, even at least two compartments, or even at least three compartments. The compartments may be arranged in superposed orientation, i.e. one positioned on top of the other. In such an orientation the unit dose article will comprise at least three films, top, middle and bottom. Alternatively, the compartments may be positioned in a side-by-side orientation, i.e. one orientated next to the other. The compartments may even be orientated in a 'tyre and rim' arrangement, i.e. a first compartment is positioned next to a second compartment, but the first compartment at least partially surrounds the second compartment, but does not completely enclose the second compartment. Alternatively, one compartment may be completely enclosed within another compartment.
Wherein the unit dose article comprises at least two compartments, one of the compartments may be smaller than the other compartment. Wherein the unit dose article comprises at least three compartments, two of the compartments may be smaller than the third compartment, and preferably the smaller compartments are superposed on the larger compartment. The superposed compartments preferably are orientated side-by-side.
In a multi-compartment orientation, the detergent composition according to the present invention may be comprised in at least one of the compartments. It may for example be comprised in just one compartment, or may be comprised in two compartments, or even in three compartments.
Each compartment may comprise the same or different compositions. The different compositions could all be in the same form, or they may be in different forms.
The water-soluble unit dose article may comprise at least a first compartment and a second compartment, preferably at least a first compartment, a second compartment and a third compartment. Preferably, the compartments are arranged in a side-by-side arrangement, a superposed arrangement or a mixture thereof. Preferably, at least the second compartment, more preferably at least the second compartment and the third compartment are superposed onto the first compartment. The second compartment and the third compartment are preferably arranged in a side-by-side arrangement superposed onto the first compartment.
The first i.e. bottom compartment preferably comprises the free flowing solid detergent composition. The second and subsequent compartments i.e. superposed compartments comprise a liquid, a solid or a mixture thereof, preferably a liquid. All compartments might comprise a gas in addition to the enclosed compositions, preferably will comprise a gas. Without wishing to be bound by theory, such a gas will create an 'air space' in the compartment and will facilitate free flowing of the enclosed compositions, and furthermore can act as an additional barrier against eventual compartment to compartment active migration through the film. Preferably the gas is air.
The water-soluble unit dose article comprises a capsule wherein the capsule comprises a shell and a core wherein the core comprises a perfume.
Preferably, the solid laundry detergent composition comprises a capsule, wherein the capsule comprises a shell and a core wherein the core comprises a perfume.
Those skilled in the art will be aware of ways to make such capsules using techniques commonly known in the art.
Preferably, the capsule is in the form of an agglomerate or a spray-dried particle.
A perfume microcapsule composition in the form of an agglomerate can be used. Such agglomerate may be made by any suitable agglomerating technique.
For the addition of the capsule by spray drying, spray drying processes for forming detergent compositions are well known in the art and typically involve the steps of forming a detergent slurry, often warmed to 60-80°C using at least in part heat of anionic surfactant neutralization (e.g. neutralization of linear alkyl benzene sulphonic acid). The slurry has typically a water content of between 30%-60% and may comprise a builder, a neutralized or acid-form anionic surfactant, a nonionic surfactant, a neutralizing alkali such as soda ash or sodium carbonate, an inorganic salt or salts such as sodium sulphate, water, processing aids, and organic polymers in a crutcher. The detergent slurry is pumped to the top of a spray drying tower, and sprayed from nozzles in the tower to form atomized droplets.
These compositions can also be prepared by continuous slurry making. By continuous slurry making is meant a process in which components are fed continuously and substantially simultaneously to a slurry making vessel while mixed, the slurry is removed to the spray tower at a rate which maintains an essentially constant volume in the vessel. Hot air is pumped through the spray drying towers such that when the atomized droplets are sprayed into the hot air, they dry into a solid as the free moisture evaporates. The spray-dried granules thus formed are then collected at the bottom of the tower.
Preferably, the solid laundry detergent composition comprising between 0.05% and 10%, preferably between 0.1% and 7.5%, more preferably between 0.15% and 5%, most preferably between 0.2% and 2.5% by weight of the liquid laundry detergent composition of the perfume. Any suitable perfume may be used. Those skilled in the art will be aware of suitable perfumes to be encapsulated in the capsule.
Preferably, the shell material comprises polyacrylate, aminoplast, polyacrylamide, silicones, silica, polystyrene, polyurea, polyurethanes, resorcinol, gelatin, polyamides, or mixtures thereof, preferably aminoplast, polyacrylate or a mixture thereof.
Preferably the shell material comprises an aminoplast. The aminoplast may comprise a polyurea, polyurethane, and/or polyureaurethane. The aminoplast may comprise an aminoplast copolymer, such as melamine-formaldehyde, urea-formaldehyde, cross-linked melamine formaldehyde, or mixtures thereof. Preferably the shell comprises an aminoplast wherein the aminoplast is melamine formaldehyde.
Preferably, the shell material comprises a material selected from the group consisting of a polyacrylate, a polyethylene glycol acrylate, a polyurethane acrylate, an epoxy acrylate, a polymethacrylate, a polyethylene glycol methacrylate, a polyurethane methacrylate, an epoxy methacrylate, and mixtures thereof. The shell material may comprise a polyacrylate polymer. The shell may comprise from about 50% to about 100%, or from about 70% to about 100%, or from about 80% to about 100% of a polyacrylate polymer. The polyacrylate may comprise a polyacrylate cross linked polymer.
Preferably, the shell material comprises a polymer derived from a material that comprises one or more multifunctional acrylate moieties. The multifunctional acrylate moiety may be selected from the group consisting of tri-functional acrylate, tetra- functional acrylate, penta-functional acrylate, hexa-functional acrylate, hepta-functional acrylate and mixtures thereof. Preferably the shell material comprises a polyacrylate that comprises a moiety selected from the group consisting of an amine acrylate moiety, methacrylate moiety, a carboxylic acid acrylate moiety, carboxylic acid methacrylate moiety, and combinations thereof.
Preferably the shell material may include a material that comprises one or more multifunctional acrylate and/or methacrylate moieties. The ratio of material that comprises one or more multifunctional acrylate moieties to material that comprises one or more methacrylate moieties may be from about 99:1 to about 6:4, or from about 99:1 to about 8:1, or from about 99:1 to about 8.5:1. The multifunctional acrylate moiety may be selected from the group consisting of tri-functional acrylate, tetra- functional acrylate, penta-functional acrylate, hexa-functional acrylate, hepta-functional acrylate and mixtures thereof. Preferably the shell material may include a polyacrylate that comprises a moiety selected from the group consisting of an amine acrylate moiety, methacrylate moiety, a carboxylic acid acrylate moiety, carboxylic acid methacrylate moiety and combinations thereof.
Polystyrene shell material may comprise polyestyrene cross-linked with divinylbenzene. Said polyurea shell material may comprise urea crosslinked with formaldehyde, urea crosslinked with gluteraldehyde, and mixtures thereof.
The polyurea shell may comprise a polyurea which is preferably the reaction product of the polymerisation between at least one polyisocyanate comprising at least two isocyanate functional groups and at least one amine.
The core/polyacrylate shell encapsulate may comprise an emulsifier, wherein the emulsifier is preferably selected from anionic emulsifiers, nonionic emulsifiers, cationic emulsifiers or mixtures thereof, preferably nonionic emulsifiers.
The core/polyacrylate shell encapsulate may comprise from 0.1 % to 1.1% by weight of the core/shell encapsulate of polyvinyl alcohol. Preferably, the polyvinyl alcohol has at least one the following properties, or a mixture thereof:

(i) a hydrolysis degree from 55% to 99%;
(ii) a viscosity of from 40 mPa.s to 120 mPa.s in 4% water solution at 20°C;
(iii) a degree of polymerization of from 1,500 to 2,500;
(iv) number average molecular weight of from 65,000 Da to 110,000 Da.

The polyacrylate core of the core/shell encapsulate may comprise greater than 10% by weight of the core of a partitioning modifier. Preferably, the portioning modifier comprises a material selected from the group consisting of propan-2-yl tetradecanoate, vegetable oil, modified vegetable oil and mixtures thereof. Preferably, said modified vegetable oil is esterified and/or brominated. Preferably said partitioning modifier comprises propan-2-yl tetradecanoate.
The capsule may be coated with a deposition aid, a cationic polymer, a non-ionic polymer, an anionic polymer, or mixtures thereof. Suitable polymers may be selected from the group consisting of: polyvinylformaldehyde, partially hydroxylated polyvinylformaldehyde, polyvinylamine, polyethyleneimine, ethoxylated polyethyleneimine, polyvinylalcohol, chitosan and chitosan derivatives and combinations thereof.

Water-soluble film

The film of the present invention is soluble or dispersible in water. The water-soluble film preferably has a thickness of from 20 to 150 micron, preferably 35 to 125 micron, even more preferably 50 to 110 micron, most preferably about 76 micron.
Preferably, the film has a water-solubility of at least 50%, preferably at least 75% or even at least 95%, as measured by the method set out here after using a glass-filter with a maximum pore size of 20 microns:

5 grams ±0.1 gram of film material is added in a pre-weighed 3L beaker and 2L ± 5ml of distilled water is added. This is stirred vigorously on a magnetic stirrer, Labline model No. 1250 or equivalent and 5 cm magnetic stirrer, set at 600 rpm, for 30 minutes at 30°C. Then, the mixture is filtered through a folded qualitative sintered-glass filter with a pore size as defined above (max. 20 micron). The water is dried off from the collected filtrate by any conventional method, and the weight of the remaining material is determined (which is the dissolved or dispersed fraction). Then, the percentage solubility or dispersability can be calculated.

Preferred film materials are preferably polymeric materials. The film material can, for example, be obtained by casting, blow-moulding, extrusion or blown extrusion of the polymeric material, as known in the art.
Preferred polymers, copolymers or derivatives thereof suitable for use as pouch material are selected from polyvinyl alcohols, polyvinyl pyrrolidone, polyalkylene oxides, acrylamide, acrylic acid, cellulose, cellulose ethers, cellulose esters, cellulose amides, polyvinyl acetates, polycarboxylic acids and salts, polyaminoacids or peptides, polyamides, polyacrylamide, copolymers of maleic/acrylic acids, polysaccharides including starch and gelatine, natural gums such as xanthum and carragum. More preferred polymers are selected from polyacrylates and water-soluble acrylate copolymers, methylcellulose, carboxymethylcellulose sodium, dextrin, ethylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose, maltodextrin, polymethacrylates, and most preferably selected from polyvinyl alcohols, polyvinyl alcohol copolymers and hydroxypropyl methyl cellulose (HPMC), and combinations thereof. Preferably, the level of polymer in the pouch material, for example a PVA polymer, is at least 60%. The polymer can have any weight average molecular weight, preferably from about 1000 to 1,000,000, more preferably from about 10,000 to 300,000 yet more preferably from about 20,000 to 150,000.
Mixtures of polymers and/or copolymers can also be used as the pouch material, especially mixtures of polyvinylalcohol polymers and/or copolymers, especially mixtures of polyvinylalcohol homopolymers and/or anionic polyvinylalcohol copolymers preferably selected from sulphonated and carboxylated anionic polyvinylalcohol copolymers especially carboxylated anionic polyvinylalcohol copolymers. Most preferably the water soluble film comprises a blend of a polyvinylalcohol homopolymer and a carboxylated anionic polyvinylalcohol copolymer.
Preferred films exhibit good dissolution in cold water, meaning unheated distilled water. Preferably such films exhibit good dissolution at temperatures of 24°C, even more preferably at 10°C. By good dissolution it is meant that the film exhibits water-solubility of at least 50%, preferably at least 75% or even at least 95%, as measured by the method set out here after using a glass-filter with a maximum pore size of 20 microns, described above.
Preferred films are those supplied by Monosol under the trade references M8630, M8900, M8779, M8310.
The film may be opaque, transparent or translucent. The film may comprise a printed area.
The area of print may be achieved using standard techniques, such as flexographic printing or inkjet printing.
The film may comprise an aversive agent, for example a bittering agent. Suitable bittering agents include, but are not limited to, naringin, sucrose octaacetate, quinine hydrochloride, denatonium benzoate, or mixtures thereof. Any suitable level of aversive agent may be used in the film. Suitable levels include, but are not limited to, 1 to 5000ppm, or even 100 to 2500ppm, or even 250 to 2000rpm.

Solid laundry detergent composition

The first internal compartment comprises a solid laundry detergent composition. The solid laundry detergent composition may comprise solid particulates or may be a single homogenous solid. Preferably, the solid laundry detergent composition comprises particles. This means the solid laundry detergent composition comprises individual solid particles as opposed to the solid being a single homogenous solid. The particles may be free-flowing or may be compacted, preferably free-flowing.
The particles may be spray-dried particles, agglomerates, extrudates or a mixture thereof. Those skilled in the art will know how to make spray-dried particles, agglomerates or extrudates using techniques commonly known in the art.
The solid particulate laundry detergent composition preferably has a mean particle size of between 400 microns and 1000 microns, more preferably between 450 microns and 850 microns.
Preferably, the solid particulate laundry detergent composition has a bulk density of between 400 and 1000g/l, more preferably between 500 and 800g/l, as measured through ISO 697 test method.
Preferably, the solid particulate laundry detergent composition fills between 25% and 95%, preferably between 30% and 90%, more preferably between 40% and 80% of the available volume within the first compartment, the remaining volume preferably filled with a gas. The gas may be any suitable gas. The gas may comprise oxygen, nitrogen, carbon dioxide or a mixture thereof. The gas may be air.
The first compartment preferably comprises between 1g and 25g, preferably between 5g and 20g, more preferably between 8g and 18g of the solid particulate laundry composition.
The solid particulate laundry detergent composition is preferably free flowing within the first internal compartment. That is to say, if the water-soluble unit dose article is moved or repositioned, the solid particulate laundry detergent composition can be seen to freely move, or flow within the first internal compartment. This is opposed to where the solid particulate laundry detergent composition is compressed such as happens when excess air is drawn out of the first internal compartment so that the film contracts and compresses around the solid particulate laundry detergent composition. Such water-soluble unit dose articles comprising compressed solids are commonly known from the art.
The solid laundry detergent composition comprises a non-soap surfactant. Preferably, the solid laundry detergent composition comprises between 20% and 75%, more preferably between 30% and 70%, most preferably between 40% and 60% by weight of the solid laundry detergent composition of the non-soap surfactant
The non-soap surfactant may comprise a non-soap anionic surfactant, a non-ionic surfactant or a mixture thereof, preferably a non-soap anionic surfactant. The solid composition may comprise a non-soap anionic surfactant, preferably, the solid laundry detergent composition comprises between 20% and 75%, more preferably between 30% and 70%, most preferably between 40% and 60% by weight of the solid laundry detergent composition of the non-soap anionic surfactant.
Preferably, the non-soap anionic surfactant comprises linear alkylbenzene sulphonate, alkoxylated alkyl sulphate or a mixture thereof, more preferably a mixture thereof. Preferably, the ratio of linear alkylbenzene sulphonate to alkoxylated alkyl sulphate preferably the ratio of linear alkylbenzene sulphonate to ethoxylated alkyl sulphate is from 1:2 to 20:1, preferably from 1.1:1 to 15:1, more preferably from 1.2:1 to 10:1, even more preferably from 1.3:1 to 5:1, even more preferably from 1.4:1 to 3:1, most preferably from 2:1 to 3:1.
Preferably, the alkoxylated alkyl sulphate is an ethoxylated alkyl sulphate with an average degree of ethoxylation of between 0.5 and 7, preferably between 0.5 and 5, more preferably between 0.5 and 3, even more preferably from 1 to 2 most preferably 1) and an average alkyl chain length of between 8 and 18. Preferably the alkoxylated alkyl sulphate has an average alkyl chain length between 10 and 16, more preferably between 12 and 14. Preferably, the linear alkylbenzene sulphonate is a C₁₀-C₁₆ linear alkylbenzene sulphonate or a C₁₁-C₁₄ linear alkylbenzene sulphonate or a mixture thereof.
When present, preferably the non-ionic surfactant is selected from an alkoxylated alcohol preferably selected from a natural or olefin derived fatty alcohol alkoxylate, an oxo-synthesised fatty alcohol alkoxylate, Guerbet fatty alcohol alkoxylates, alkyl phenol alcohol alkoxylates or a mixture thereof. The alcohol alkoxylate may have an average degree of alkoxylation of between 0.5 and 10, preferably between 1 and 9, more preferably between 3 and 8, more preferably a degree of ethoxylation of between 0.5 and 10, preferably between 1 and 9, more preferably between 3 and 8, most preferably between 5 and 8 or even from about 7 to about 8. The alcohol alkoxylate may have an average alkyl chain length of between 8 and 18, preferably between 10 and 16, more preferably between 12 and 15.
The solid composition at 1wt% dilution in deionized water at 20°C has an equilibrium pH in the range of from 6.5 to 9.0, preferably between 6.7 and 8.8, more preferably between 7 and 8. Without wishing to be bound by theory, the specific low pH of the solid laundry detergent composition provides for improved fabric cleaning or treatment performance of the water-soluble unit dose article according to the present invention as compared to water-soluble unit dose articles wherein the solid laundry detergent composition has a higher pH. Such higher pH solid laundry detergent composition formulated into water-soluble unit dose articles are known in the art.
Those skilled in the art will know how to measure the pH using common known techniques. A preferred method is to obtain a 10g sample accurately weighed to two decimal places, of the solid laundry detergent composition. The sample should preferably be obtained using a Pascall sampler in a dust cabinet. Add the 10g sample to a plastic beaker and add 200 ml of carbon dioxide-free de-ionised water. Agitate using a magnetic stirrer on a stirring plate at 150 rpm until fully dissolved and for at least 15 minutes. Transfer the contents of the beaker to a 1 litre volumetric flask and make up to 1 litre with Cardon dioxide-free de-ionised water. Mix well and take a 100 mls ± 1 ml aliquot using a 100 mls pipette immediately. Measure and record the pH and temperature of the sample using a pH meter capable of reading to ±0.01pH units, with stirring, ensuring temperature is 20°C +/- 0.5°C.
The solid laundry detergent composition may comprise between 0% and 10% by weight of the solid laundry detergent composition of carbonate salts. The carbonate salts may be selected from sodium carbonate, potassium carbonate, sodium bicarbonate, sodium bicarbonate, burkeite, sequicarbonate, habit modified carbonate, crystal growth modified burkeite or a mixture thereof, preferably sodium carbonate.
The solid laundry detergent composition may comprise a material selected from zeolite, sodium sulphate, silica, organic acid or a mixture thereof, preferably wherein the solid laundry detergent composition comprises between 10% and 35%, more preferably between 12% and 25% by weight of the solid laundry detergent composition of the material.
The solid laundry detergent composition may comprise an organic acid, preferably between 1% and 10% by weight of the solid laundry detergent composition of an organic acid and/or a salt thereof. Preferably, the organic acid is a carboxylic acid, preferably a polycarboxylic acid, more preferably the organic acid is selected from citric acid, malic acid, lactic acid, propionic acid, valeric acid, caproic acid, carbonic acid, adipic acid, gluconic acid, methylglycinediacetic acid or a mixture thereof, most preferably citric acid. Without wishing to be bound by theory such materials may be used to control the pH of the laundry detergent composition.
The solid laundry detergent composition may comprise an adjunct ingredient, wherein the adjunct ingredient is preferably selected from cationic polymers, brighteners, enzymes, dye transfer inhibitors, chelants including aminocarboxylate and aminophosphonate chelants such as HEDP, acrylate-based polymers, perfumes, polyester terephthalate polymers, PEG-based polymers, ethoxylated polyethyleneimines, polysaccharides, amine oxide, aesthetic dyes, hueing dyes, antifoams, bleaching actives, or a mixture thereof.
Preferred acrylate-based polymers are acrylate/maleate random copolymers.
Preferred cationic polysaccharides are cationically-modified polysaccharides. Preferably, the cationically modified polysaccharide is selected from cationic guar gums, cationic cellulosic polymers, and mixtures thereof, most preferably cationic cellulosic polymers even more preferably cationically modified hydroxyethyl cellulose, most preferably, hydroxyethyl cellulose derivatised with trimethyl ammonium substituted epoxide.
Preferably, the particulate laundry detergent composition comprises agglomerates. Preferably, the agglomerates comprise non-soap surfactant, silica and sodium sulphate.
Another aspect of the present invention is the use of a solid laundry detergent composition comprising a non-soap surfactant and having at 1wt% dilution in deionized water at 20°C an equilibrium pH in the range of from 6.5 to 9.0 in a water-soluble unit dose article as according to the present invention to improve the performance of the capsule wherein the capsule comprises a shell and a core wherein the core comprises a perfume.

Method of washing

An aspect of the present invention is a method of washing comprising the steps of adding the water-soluble unit dose article according to the present invention to sufficient water to dilute the solid particulate laundry detergent composition by a factor of at least 300 fold to create a wash liquor and contacting fabrics to be washed with said wash liquor.
The method may be performed in a hand wash operation, an automatic laundry washing machine or a mixture thereof.

Process of making

Those skilled in the art will know how to make the unit dose article and particulate laundry detergent composition of the present invention using known techniques in the art:

Water soluble pouch making :

During manufacture, a first water-soluble film may be shaped to comprise an open compartment into which the detergent composition is added. A second water-soluble film is then laid over the first film in such an orientation as to close the opening of the compartment. The first and second films are then sealed together along a seal region using known sealing means such as solvent, heat or a mixture thereof.

Preparation of free-flowing detergent powders :

Highly preferred are free-flowing detergent powders. Without wishing to be bound by theory, free-flowing detergent powders are found to have improved dissolution when formulated in a water soluble pouch compared to compressed powders, leaving less detergent residues behind accordingly. Highly free-flowing detergent powders can be prepared by the following process.
Surfactant-containing particles can be prepared by spray-drying, agglomeration or other processes such as drum drying etc. Such agglomerates are preferred due to the high surfactant loading that can be achieved. However other processes can be used. The surfactant agglomerates preferably contain anionic surfactant, including LAS. An especially preferred feature is that the surfactant agglomerates contain a mixture of anionic surfactants, especially LAS and AES surfactant.
To improve the flowability and stability of the detergent powder(s), smaller particles are usually removed by sieving. It is especially preferred to sieve the surfactant agglomerates plus other detergent ingredients prior to any subsequent coating step. The surfactant agglomerates, plus other granular detergent ingredients such as HEDP, are sieved to remove particles smaller than 600 microns. The surfactant particles, plus any other detergent ingredients that are optionally added, are then put into a mixer where they are dusted or coated with a fine powder to provide a protective layer on the surface. An example of such a process is where blown powders are coated with non-ionic surfactant as a binder and then zeolite. It has been found, though, that dusting or coating the surfactant agglomerates (and other optional detergent ingredients) in this instance with a blend of micronized sodium sulphate and zeolite gives good results for flowability as well as appearance etc. Inclusion of a liquid binder to help the adhesion of the fine powder(s) to the surface of the larger surfactant agglomerates is also an option.
A suitable detergent mix can be prepared as follows. Surfactant agglomerates containing a blend of LAS and AExS anionic surfactants are prepared and dried to give particles with a total surfactant activity of 60% comprising a 2:1 blend of LAS to AExS surfactants. The particles contain 20% of hydrophilic silica. A suitable silica is 22S from Evonik. The balance consists of ground sodium sulphate, water and miscellaneous. The fine particles are then removed by sieving the agglomerates on a 600 micron mesh sieve. Oversize particles are removed by sieving the agglomerates through a 1400 micron mesh size sieve.
3kg of the sieved surfactant agglomerates are then put into a 6-litre internal volume paddle mixer from Forberg. 300g of ground sodium sulphate (d90 < 100 microns) and 100g of sodium aluminosilicate type 4A are then added to the mixer and the mixer is run at maximum speed for 2 minutes, thus coating the surface of the agglomerates with sulphate and zeolite. The coated agglomerates are then removed and blended with other detergent materials to give a free-flowing detergent mixture suitable for use.
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm."

EXAMPLES

The below test shows a consistently improved perfume headspace performance profile for low versus high pH perfume comprising powder compositions within a water soluble pouch.

Test Method:

In order to show the impact in providing improved perfume headspace benefits of formulating with a low pH powder vs high pH powder contained within a pouch, a full scale wash test has been conducted in combination with a Gas Chromatography (GC) headspace analysis. 4 Tonrose bath towels (ca 2 kg, sourced from Tonrose Ltd, Tonrose House, Petre Road, Accrington, Lancashire, BB5 5JB- United Kingdom) were washed in a Miele washing machine (model 3922 - cotton short cycle, 60°C, city water -7.8gpg-, total wash time 1hour 25mins). 0.5g of GP-4314 Powdered Antifoam suds suppressor technology (sourced from the Dow Corning company) has been added to prevent over-sudsing. The wash cycle was stopped after 39 minutes, i.e. 2 minutes prior to onset of rinse cycle, and a sample of the wash water was taken using a 10ml syringe. 5mls of this wash solution is added to a 20ml headspace vial (Sigma # Vials= SU860097, Caps= SU860101) and submitted for GC analysis of Ester content in headspace. A total of 6 replicates (3 different washes and 2 samples per wash) were tested for both the low pH test product and the high pH reference products. Relative averaged testing results are summarized below.

Test products:

LAS/AE1S Agglomerate

Constituent	%w/w Base Powder
LAS Linear alkyl benzene sulfonate	50
C12-14 Alky Ethoxylate (1) Sulphate	20
Sodium Sulphate	7.5
Silica	18.75
Free water	3.75
Total	100

Liquid Additive Mix

Constituent	%w/w
Ethoxylated Polyethyleneimine (PEI600EO20 - 80%)	20
PEG-Vinyl Acetate co-polymer (72.5%)	27
Nonionic surfactant (C24AE7)	24
Perfume Accord	29
Total	100

Perfume Accord

	Composition
Benzyl Acetate	1.5 mL
Allyl Cyclohexane Propionate	1.5 mL
Hexyl Acetate	1.5 mL
Frutene	1.5 mL
Verdox (OTBCA)	1.5 mL
Allyl Amyl Glycolate	1.5 mL
Flor Acetate TRICYCLODECENYL ACETATE	1.5 mL
Hedione (Methyl Dihydro Jasmonate)	1.5 mL
Hexyl Salicylate	1.5mL
Cyclohexyl Salicylate	1.5 mL
Eucalyptol	1.5 mL
Geraniol	1.5 mL
Citronellol	1.5 mL

Test Base - Low pH

Constituent	%w/w Base Powder
LAS/AE1S Agglomerate	66.27
Carboxymethyl cellulose (98%) (Finnfix GDA ex CP Kelco)	1.75
Brightener 49 Tinopal® CBS-X	1.15
Texcare SRA300 Soil release polymer	0.53
Na HEDP Etidronic Acid (86.8%)	14.09
Zeolite	2.17
Acusol 4445N Polymer (92.6%)	4.03
Dow Corning GP-4314 Powdered Antifoam (12% active)	2.31
Lipase (18.5mg/g)	1.97
Stainzyme Plus (14.4mg/g)	1.14
Protease	1.72
Cellulase (15.6mg/g)	1.39
Mannanase (4mg/g)	1.50

Reference Base - High pH

Constituent	%w/w Base Powder
LAS/AE1S Agglomerate	51.25
Carboxymethyl cellulose (98%) (Finnfix GDA ex CP Kelco)	1.35
Brightener 49 Tinopal® CBS-X	0.89
Texcare SRA300 Soil release polymer	0.41
Na HEDP Etidronic Acid (86.8%)	10.89
Zeolite	1.68
Acusol 4445N Polymer (92.6%)	3.11
Dow Corning GP-4314 Powdered Antifoam (12% active)	1.79
Lipase (18.5mg/g)	1.53
Stainzyme Plus (14.4mg/g)	0.88
Protease	1.33
Cellulase (15.6mg/g)	1.07
Mannanase (4mg/g)	1.16
Sodium Carbonate	22.67

Products Tested :

High pH Ref : 13.9g of High pH reference base formulation contained in a PVA film* pouch & 1.75ml of Liquid additive mix formulation.
Low pH Test leg : 10.75g of Low pH reference formulation contained in a PVA film* pouch & 1.75ml Liquid additive mix formulation.

Results

The results tabulated below show an improved perfume headspace performance for benzyl acetate and methyl dihydro jasmonite perfume materials for a low versus high pH powder formulation (expressed as relative amount of PRM in headspace). Beyond for allyl amyl glycolate, no material was detected in the headspace for the high pH formulation, contrary to the low pH formulation.

% Change in PRM level in headspace

Benzyl acetate 213%

Methyl dihydro jasmonite 121%

Claims

A water-soluble unit dose article comprising a water-soluble film and a solid laundry detergent composition, wherein the water-soluble film defines a first internal compartment and wherein the solid laundry detergent composition is comprised within the first internal compartment, and wherein the water soluble unit dose article composition comprises a capsule, wherein the capsule comprises a shell and a core wherein the core comprises a perfume; and
wherein the solid composition at 1wt% dilution in deionized water at 20°C, has an equilibrium pH in the range of from 6.5 to 9.0, preferably between 6.7 and 8.8.
The water-soluble unit dose article according to claim 1, wherein the solid laundry detergent composition comprises from 0wt% to 10wt% of carbonate salt, preferably wherein the carbonate salts are selected from sodium carbonate, potassium carbonate, sodium bicarbonate, sodium bicarbonate, burkeite, sequicarbonate, habit modified carbonate, crystal growth modified burkeite or a mixture thereof, preferably sodium carbonate.
The water-soluble unit dose article according to any preceding claims wherein the solid laundry detergent composition comprises the capsule and preferably wherein the solid laundry detergent composition comprising between 0.05% and 10%, preferably between 0.1% and 7.5%, more preferably between 0.15% and 5%, most preferably between 0.2% and 2.5% by weight of the liquid laundry detergent composition of the perfume.
The water-soluble unit dose article according to any preceding claims, wherein the shell material comprises, aminoplast, polyacrylate, polyacrylamide, silicones, silica, polystyrene, polyurea, polyurethanes, resorcinol, gelatin, polyamides, or mixtures thereof, preferably aminoplast, polyacrylate or a mixture thereof, more preferably wherein the aminoplast is melamine formaldehyde.
The water-soluble unit dose article according to any preceding claims wherein the solid laundry detergent composition comprises a non-soap surfactant preferably wherein the non-soap surfactant comprises a non-soap anionic surfactant comprises linear alkylbenzene sulphonate, alkoxylated alkyl sulphate or a mixture thereof, more preferably a mixture thereof wherein the ratio of linear alkylbenzene sulphonate to alkoxylated alkyl sulphate preferably the ratio of linear alkylbenzene sulphonate to ethoxylated alkyl sulphate is from 1:2 to 20:1, preferably from 1.1:1 to 15:1, more preferably from 1.2:1 to 10:1, even more preferably from 1.3:1 to 5:1, even more preferably from 1.4:1 to 3:1, most preferably from 2:1 to 3:1.
The water-soluble unit dose article according to claim 5, wherein the solid laundry detergent composition comprises between 20% and 75%, preferably between 30% and 70%, more preferably between 40% and 60% by weight of the solid laundry detergent composition of the non-soap anionic surfactant.
The water-soluble unit dose article according to any preceding claims wherein the solid laundry detergent composition comprises between 1% and 10% by weight of the solid laundry detergent composition of an organic acid and wherein preferably the organic acid is a carboxylic acid, preferably a polycarboxylic acid, more preferably the organic acid is selected from citric acid, malic acid, lactic acid, propionic acid, valeric acid, caproic acid, carbonic acid, adipic acid, gluconic acid, methylglycinediacetic acid or a mixture thereof, most preferably citric acid.
The water-soluble unit dose article according to any preceding claims wherein the solid laundry detergent composition is a free flowing particulate solid, a compressed particulate solid or a mixture thereof and has a mean particle size between 400 microns and 1000 microns, preferably between 450 microns and 850 microns.
The water-soluble unit dose article according to any preceding claims wherein the solid laundry detergent composition has a bulk density of between 400 and 1000g/l, preferably between 500 and 800g/l.
The water-soluble unit dose article according to any preceding claims wherein the first compartment comprises between 1g and 25g, preferably between 5g and 20 g, preferably between 8g and 18g of the solid laundry composition.
The water-soluble unit dose article according to any preceding claims wherein the water-soluble film comprises polyvinyl alcohol, preferably wherein the water-soluble film comprises polyvinyl alcohol polymer or copolymer, preferably a blend of polyvinylalcohol polymers and/or polyvinylalcohol copolymers, more preferably selected from sulphonated and carboxylated anionic polyvinylalcohol copolymers especially carboxylated anionic polyvinylalcohol copolymers, most preferably a blend of a polyvinylalcohol homopolymer and a carboxylated anionic polyvinylalcohol copolymer.
The water-soluble unit dose article according to any preceding claims wherein the water-soluble unit dose article comprises at least a first compartment and a second compartment, preferably at least a first compartment, a second compartment and a third compartment.
The water-soluble unit dose article according to claim 12 wherein the compartments are arranged in a side-by-side arrangement, a superposed arrangement or a mixture thereof, preferably wherein at least one compartment, preferably wherein at least two compartments are superposed onto a third compartment, even more preferably wherein at least one of the superposed compartments comprises a liquid, preferably wherein the both superposed compartments comprise a liquid.
A method of washing comprising the steps of adding the water-soluble unit dose article according to any preceding claims to sufficient water to dilute the solid laundry detergent composition by a factor of at least 300 fold to create a wash liquor and contacting fabrics to be washed with said wash liquor.
Use of a solid laundry detergent composition comprising a non-soap surfactant and having at 1wt% dilution in deionized water at 20°C an equilibrium pH in the range of from 6.5 to 9.0 in a water-soluble unit dose article to improve the performance of a capsule wherein the capsule comprises a shell and a core wherein the core comprises a perfume.