C4434/C
FORM - 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
FABRIC CARE COMPOSITIONS
HINDUSTAN UNILEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India
The following specification particularly describes the invention and the manner in which it is to be performed

WO 2006/097227 PCT/EP2006/002116

FABRIC CARE COMPOSITIONS
Field of the Invention
The present invention relates to fabric care compositions. More specifically, the invention relates to fabric care compositions for ironing which reduce the wrinkling of fabrics in particular the dry or in-wear wrinkling giving fabrics an all-day-ironed look.
Background of the Invention
Fabric care compositions which reduce the wrinkling of fabrics being worn are known.

Mechanical wrinkle reduction techniques, such as heat and pressure, for example in ironing, are effective ways of flattening garments. However the effect is not permanent and wrinkles reappear due to a range of shear, torsion and
compressive deformation forces applied in wear. The body's
heat and humidity work on the fabric to relax it and hence to enhance the wrinkling of these deformational forces.
The prior art anti-wrinkle teaching can be rationalised into three approaches;
(a) using lubricants to improve recovery from crease,
(b) using cross-linkers and film formers to stiffen the fibres to resist creases in the first place, and
(c) combining (a) and (b).
The lubricants used in the prior art include silicones eg PDMS, aminosilicones, modified silicones, silicone copolymers,

WO 2006/097227 PCT/EP2006/002116

softeners (e.g. quaternary ammonium compounds) and other lubricants such as clays, waxes, polyolefins, synthetic and natural oils.
Film formers and cross-linkers used in the prior art include:
Natural Polymers - enzymes, proteins, cyclodextrins, polysaccharides e.g. starch, chitin, chitosan, cellulose, 3-1,4-polysaccharides, SCMC, guar gum, HEC etc.,
Synthetic Polymers - polyamides, polyurethanes, polyamines, polyolefins, polyols, PEGs, polystyrene, PVA, PVC, vinyl polymers, acrylics,
Film forming polymers - copolymers, adhesives,
Reactive polymers - epichlorohydrin containing, isocyanate containing, epoxy containing curables,
Elastomeric polymers - thermoplastic silicone elastomers,
Small Molecules - salts, amino acids, sugars, saccharides, oligosaccharides, alcohols, acids, and
Crosslinkers - methylol urea based, carboxylic acid, formaldehyde, ammonia, triazine, epoxide.
WO 2004/018762A1 (Philips) discloses on wrinkle benefit using fusible elastomer film formers with cross-linked particles to improve recovery from wrinkle in spray or iron cartridge applications.

WO 2006/097227 PCT/EP2006/002116

WO 2004/048677 (Philips) discloses film formers for recovery in spray or iron cartridge applications including fusible elastomers + polycation salt for x-linking of elastomer.
WO 2001/25381-5 (Ciba) disclose compositions with (A) a fabric softener, (B) an additive and (C) selected polyorganosilicones to endow fabrics in domestic applications with anti-pilling, elasticity, hydrophilicity, drape, and wrinkle recovery respectively. These properties are endowed by the organosilicone. Amongst the additives polysilicic acid is mentioned.
WO 2002/088293' and US-A1-2002/019236 (Unilever) both disclose fabric care compositions comprising coated particles
comprising a solid core with a 03,2 average particle size of
between 10 to 700 run in diameter and a coating of silicone polymer covalently bonded to the solid core. Silica is mentioned in a list of suitable solid core materials.
EP 1201817(Al) (Procter & Gamble) discloses aminosilicones
with sterically hindered functional groups for in-wear wrinkle resistance, which are preferably delivered from a spray during domestic ironing process.
EP 1096060(Al)(Procter & Gamble) discloses water-soluble silicone lubricants in combination with various polymeric compounds (film formers) which are said to provide fabrics with a wrinkle recovery angle of at least +15 units over and above water.

EP 953675(A2,A3) (Dow Corning) a textile fabric coated with an elastomeric silicone-based compound with a reinforcing filler preferably a silica + a second laminar filler preferably talc

WO 2006/097227 PCT/EP2006/002116

and mica. The coated fabrics amongst other benefit have less friction and are used for car seat belts. No teaching exists on the wrinkle benefit of the mixed silicone + particulate fillers.
GB 842027 (Monsanto Chemicals) discloses textile friction enhancing compositions based on silica nanoparticles dispersed inside an oil emulsion droplets. The oil can be any of the known textile oils including mineral or vegetable oils. The oil to silica ratio exceeds 6 and deposition levels of 3-7%
oil and 0.1-0.5% of silica per weight of fabric are preferred.
US 2635056 (Monsanto) discloses treating textiles and fabrics with an aquasol of silica plus a polyhydic alcohol such as glycerol. The blends are termed alco-aquasols and provide exceptional slip resistance to textiles and surprisingly good handle and fabric feel attributed to the presence of glycerol. The silica to glycerol ratio used in the example is 1.4. It is stated that polyhydric alcohol level should not exceed twice that of silica.
WO-2001/083875 (Ajinomoto Co.) discloses the application of silica and a softener in addition to other care ingredients to nylon tights so as to provide skin care benefits when the tights are worn.
EP 1024119 (A2,A3) (Relats) discloses textile articles made of
SiO2-containing fibres and procedure for improving their
thermal stability.

JP 04255767 (Nichihan Kenkyusho K.K.) discloses coating compositions for textiles comprising a synthetic emulsion (acrylic), colloidal or microparticle metal oxide silica gel

WO 2006/097227 PCT/EP2006/002116

and a zeolite to provide textile coatings with good antibacterial, deodorising, drying and heat retention properties.
NL 8900473 (Hesco Fashion Netherlands) discloses the
manufacture of viscose rayon-polyester coated with a mixture of a nonionic fatty acid condensates fabric softener and a blocking agent (blocking free movement of warp and weft -friction enhancer) acidic silica dispersion. The ratio of the softener to silica is 1:1 and the level applied 1% of silica and 1% of softener.
EP 0474207, EP 1178150, US 5102930, US 3077460 and US 2881146 disclose fabric treatment compositions comprising silica, an organopolysiloxane and a catalyst/curing agent to cause a polymer film to form on the fabrics.
EP 1371718 discloses polymeric nanoparticles and their use as fabric care additives.
There has been no product available on the market that meets consumers need for an effective in-wear wrinkle or all-day-ironed look benefit.
Therefore, there is a need for an effective and efficient means for eliminating or reducing wrinkling in fabrics and clothing in-wear after they have been ironed whilst the fabrics maintains a good handle, softness and comfort in wear.
Objects of the Invention
The present invention seeks to address one or more of the above-mentioned problems.

WO 2006/097227 PCT/EP2006/002116

Summary of the Invention
According to one aspect of the present invention there is provided an ironing aid fabric treatment composition comprising:
a) a nanoparticle dispersion comprising particles having an average particle size in the range 5 to 500 nm,
b) a lubricant phase comprising a lubricant selected from silicone oil, sucrose polyester oil and mixtures thereof,
and
c) water
wherein the weight ratio of a) : b) is in the range 4 : 1 to 1: 4.
with the proviso that when the colloidal nanoparticle dispersion comprises a silicone resin the composition is not delivered through an iron.
According to a further aspect of the present invention there is provided a method of treating a fabric which comprises applying to the fabric an iron aid fabric treatment composition comprising:
a) a colloidal nanoparticle dispersion comprising particles having an average particle size in the range 1 to 500 nm,
b) a lubricant phase,
c) water
wherein the ratio of a) : b) is in the range 4 : 1 to 1 : A, and

WO 2006/097227 PCT/EP2006/002116

simultaneously with said application or thereafter, ironing said fabric under elevated temperature and pressure, with the proviso that when the colloidal nanoparticle dispersion comprises a silicone resin the composition is not delivered through the iron.
Surprisingly, it has been found that certain nano-particulate friction enhancers when combined with certain lubricants at certain particle to lubricant ratios work in synergy to
noticeably reduce the tendency of fabrics to wrinkle in wear. The balance of the nanoparticles and lubricant phase provides the desired properties by virtue of their physical properties. The compositions of the invention are free from catalysts and curing agents and do not react to form a film when deposited
on the fabric. Preferred nanoparticle phases include
colloidal silica and silicone resins, preferred lubricants are silicone oils and sucrose polyester oils. Preferred ratios of particle phase to lubricant phase range from 3 : 1 to 1 : 3 more preferably 2:1 to 1:2.

The in-wear wrinkle benefit from a combination of particulate phase + lubricant phase has been found for rinse cycle fabric care products and ironing spray application.
Detailed Description of the Invention
The compositions of the present invention are typically for use in a spray form with a conventional steam iron. The compositions are typically aqueous.

WO 2006/097227 PCT/EP2006/002116

Nanoparticles
The compositions of the present invention comprise a nanoparticle dispersion. The particles may be inorganic or organic or a mixture of one or more types of nanoparticles.
Suitable inorganic nano-particles include silicas, Si02, titania, Ti02, alumina, Al2O3, zinc oxide, ZnO, and the mixed
oxides class such as ITO (indium-tin oxide, In2O3-SnO2.

The widely commercial and preferred inorganic nanoparticle are amorphous silicas available in the sol or colloidal form as defined on page 330 of The Chemistry of Silica, by R K Iler, Wiley-Interscience, New York, 1979.

Silica nanoparticles could also be of non-siliceous core as long as the surface of the nanoparticle is coated with silica as described on page 330 of Iler's book. The core can be of organic polymeric nature.

Suitable organic particles include those derived from silicon (such as silicone resins). The organic particles are preferably not of the type which comprise a solid core coated with a polymer, such as a silicone polymer. The organic
particles are preferably non-coated and comprise solid
particles of polymer or resin. In the context of the present invention, "nanoparticle" denotes particles have an average particle size ranging from 5 to 500 run. Larger particle size silica also aid crease resistance but apparently they are not
as effective as those between 15-100 run. Preferably all of the particles have a particle size below 500 nm, more preferably below 100 nm.

WO 2006/097227 PCT/EP2006/002116

It has been found that a particle size of 500 nm or less provides excellent crease resistance on poplin fibres and a particle size of 300 nm or less provides excellent crease resistance on cotton fibres.
Dispersions having an average particle size in the range 10 to 50 nm are particularly useful. The amount to deposit between 0.25 to 2% and preferably between 0.25 to 0.5 wt% owf (0.0025 to 0.005 g/g of fabric).

Inorganic nanoparticle depending on their structure can provide additional benefits - aid odour absorption during the wear, increase longer lasting freshness, reduced glare and shine on ironing items, resistance to staining, and ease of
stain removal in following washes can be achieved.
Preferred nanoparticles for use in the invention are colloidal silica. The term ‘colloidal silica' here refers to dispersions or sols of discrete particles of amorphous silica, which are preferably stable. Reacted silica is the
hydrophobic fumed silica as used in anti-foaming emulsions mentioned above.
Commercial colloidal silica is available containing up to 50% silica with particle diameter between 10-21 nm under the trade name Ludox (ex Grace Davison) and Snowtex (ex Nissan). Particular examples include Ludox CI (a cationic silica) and Ludox HS50 (an anionic silica), both having a particle size of 20 nm. The quoted size represents the linear diameter of the particle.
It is well known in the art that the surface of silica particles can be easily modified to endow them with additional benefits. For example modification with aluminates allows

WO 2006/097227 PCT/EP2006/002116

surface charge modification (positive charge). Silicas can be modifies organically (organosols as described on page 412 of the above reference). The preferred silicas have suitable modification for surface charge and/or other textile functional benefits including antimicrobial, dermal and transdermal, controlled release of fragrance and repellent agents, improved abrasion stability, water and oil, dirt repellency, and UV protection as described in Journal of Sol-Gel Science and Technology 27, 43-52, 2003 by B Mahltig and H Bottcher; Modified Silica Sol coatings for Water-Repellent Textiles.
Lubricant phase
The lubricant phase of interest include silicone oils and oily sugar derivatives.
The silicone lubricants of interest include the classical three classes of non-reactive silicone polymers (PDMS),
reactive silicone polymers (silanol terminated PDMS) and
modified silicone polymers (amino/amide functional siloxanes, non-ionic modified siloxanes or polyether modified siloxanes). Preferred silicones are PDMS types in emulsion or microemulsion format, which are commercially available, for
example, Dow Corning 1716 (cationic) microemulsion, etc. Also DC amino silicones 2-8669 nonionic microemulsion, 2-8203 nonionic microemulsion, 28197 nonionic macroemulsion.
Another class of preferred silicones are those ex Wacker including Wetsoft CTA (amino glycol PDMS), Finish CT 34E (amino PDMS emulsion), Finish CT 208E (amino OH PDMS emulsion), Finish CT 96 E (amino PDMS emulsion), and their Fluid L range, Fluid L 652 for example (amino PDMS).

WO 2006/097227 PCT/EP2006/002116

Although silicone oils are preferred to improve the fabric handle and softness non-silicone lubricants such as sucrose polyester oils can provide the lubrication needed for fabric recovery from wrinkle. WO2002/019236A1 (Unilever) provides a fuller list of silicone polymers of interest and EP1205538 (Unilever) the class of drying oils.
A preferred class of commercial materials in which the particulate phase and a lubricant phase are combined include 10 but not limited to Dow Corning's silicone + reacted silica blends marketed as anti-foaming agents including DOW CORNING® Antifoam B, DOW CORNING® 544, DOW CORNING® Q2-3302 ANTIFOAM COMPOUND, DOW CORNING® 1581 WATER REPELLENT, DOW CORNING® 2- 1912 FLUID.

Another preferred class of materials in which the particulate phase and the lubricant phase are combined include but not limited to Dow Corning MQ silicone resin range which contains a PDMS silicone oil and a silicone resin nano-particulate
phase.
It is particularly preferred that the nanoparticle is silica or silicone resins, more preferably colloidal silica or reacted fume silica.

WO 2006/097227 PCT/EP2006/002116

Suitable sucrose polyester oils are the reaction products of fatty acid methyl ester (FAME) of natural oils and sucrose. Suitable oils and their preparation are described in EP323670B1, EP383404B1, WO2001/46210, W098/16538 and WO01/46359A1.
Preferred oils are derived from natural oils predominantly comprising C16 and C18 hydrocarbon chains e.g. palm kernel oil.
Water
The composition is aqueous. Demineralised water is most preferred.
Demineralised water means water where a large proportion, if not substantially all, of the dissolved salts have been removed. Water where the hardness ions (Ca (II) and Mg (II)) have simply been replaced by other ions (such as Na (I)) is not as preferred. The term demineralised water, also includes
distilled water.
If the composition is an ironing aid spray composition, then the water present should have a French Hardness of 20 or below, preferably 12 or below, more preferably 5 or below. Water with a French Hardness of 12 to 20 is usually termed Medium water, whilst that with a French Hardness of 5 to 12, soft water and that with a French Hardness of less than 5, very soft water).
Perfume
Perfume ingredients (or fragrance ingredients) are well known to those skilled in the art, and are described in Perfume and

WO 2006/097227 PCT/EP2006/002116

Flavor Chemicals, Steffan Arctander (ISDN 75-91398). The solubility of individual perfume ingredients in water can be represented by the calculated partition coefficient (ClogP) of the ingredient between distilled water and octanol at 20°C. The lower the value of ClogP, the more water soluble the ingredient. The, ClogP values are most conveniently calculated by the 11CLOGP11 program, available from Daylight CIS.
Preservative
Where the composition is an ironing aid spray composition, it may further comprise between 0.1 ppm and 3 wt% of a preferably water-soluble preservative. The preservative preferably should not release or decompose to chemicals which are potentially harmful to the ironer at the temperatures encountered in a steam iron, i.e. preferably at 150, 200 or even 250°C. A guide to safe limits of numerous chemicals is provided by occupational Exposure Limits which are available from OHSE and are listed in EH40, available from HMSO.
Many known preservatives, e.g. Bronopol" (Myacide), DowicilTm 75 or 200, Germaben" II GermallTm 1 15, Germal 1 TM I I, Glycac i 1 TM, GlydantTM, GlydantTl plus, Oxaban Tm A and Suttocide TI can release or breakdown to harmful or irritating chemicals (e.g. formaldehyde) at the temperatures encountered in steam irons.
If a preservative, other than those defined as preferable, is to be included in the composition, then it should not be present at an amount of greater than 0.5 wt%.
Preferred preservatives include those selected from aromatic, linear or branched C1-C20 alcohols and mixtures thereof, and

WO 2006/097227 PCT/EP2006/002116

may be present in an amount of between 0.1 ppm and 3wt% or preferably 0.5 and lwt%. Preferably, at least one preservative is selected from benzyl alcohol (phenoxy methanol) and phenoxy ethanol and mixtures thereof. Of these preservatives, benzyl alcohol is more preferred. If benzyl alcohol is used,
preferably a high purity grade is employed, to minimise the presence of the known impurity, benzaldehyde, which is preferably essentially absent from the composition according to the invention, i.e., so low that the ironing aid composition can still be safely used.
A particularly preferred preservative comprises at least one isothiazolone-based compound, e.g., Kathon TM CG ICP II (available from Rohm and Haas), a 3:1 mixture of 5-chloro-2-methyl-3(2H)-isothiazolone and 2- methyl-3(2H)-isothiazolone with a low salt content.
Buffers
Where the composition is an ironing aid spray composition, it is preferred that composition is neutral or slightly alkaline, as is most tap water. Therefore buffers may be included in the composition of the present invention in order to adjust the pH of the solution such that it is greater than or equal
to 6, preferably 7 to 9 more preferably 7 to 8. Such buffers may be included in amounts of between 0.0001, preferably 0.001 to 0.1 or 1 wt%.
Auxiliary Solvent:
An auxiliary solvent may be included in the invention in an amount of 0.01 to 5 or possibly 20 wt%, more preferably 0.1 to 5 or 10 wt%, most preferably 0.2 to 1 or 2 wt%.

WO 2006/097227 PCT/EP2006/002116

Suitable auxiliary solvents include dipropylene glycol, glycerin, propylene glycol, ethanol and isopropyl alcohol (IPA) and mixtures thereof. The most preferred of these is dipropylene glycol. We have found that dipropylene glycol may be especially useful in ironing applications as a humidifier to facilitate ironing.
The amount of ethanol and/or isopropyl alcohol (IPA) in the composition preferably does not exceed 5% by weight.

The total level of solvent in an ironing aid composition, including the solvent that can be present in the water-soluble perfume, can therefore be up to and including about 25 wt%, more preferably 15, 10, 5, or even 2 or 3 wt%.

Preparation of an ironing aid composition
The ironing aid spray composition may be provided as a
concentrate for dilution by the end consumer.

Preferably, the dilution is such that one part of concentrate
is diluted with between 0.5 to 100, more preferably, between 1
and 10, most preferably between 2 and 5 parts of water (w/w).
The exact composition of the concentrate can be easily calculated given the desired end concentration in the ironing
aid composition and the dilution factor.
For example when the end concentration of perfume in the-composition has to be between 3.0 and 5.0 wt % than the dilution factor will be limited to at most 20. It will be obvious to the skilled person that when higher dilution factors are used e.g. 100, the diluted ironing aid composition will necessarily comprise lower maximal perfume levels.

WO 2006/097227 PCT/EP2006/002116

The compositions further contain surfactants, superspreaders, softening agents as known to the skilled person in the art.
Further Optional Ingredients
Other optional nonionic softeners, bactericides, soil-releases agents may also be incorporated.
Such compositions may also contain one or more optional
ingredients conventionally included in liquid rinse fabric conditioning compositions such as pH buffering agents, perfume carriers, fluorescers, colourants, hydrotropes, antifoaming agents, anti-redeposition agents, poly-electrolytes, enzymes,
optical brightening agents, anti-shrinking agents, anti-wrinkle agents, anti-spotting agents, antioxidants, sunscreens, anti-corrosion agents, drape imparting agents, anti-static agents, polymeric viscosity modifiers, ironing aids and dyes.

Preparation of compositions
The composition may be prepared according to any suitable method.

In a first preferred method for spray is to disperse the silica colloid into water which already contains the minor ingredients like dye and preservative and surfactants, if present, and add silicone emulsion or microemulsion followed
by perfume.

WO 2006/097227 PCT/EP2006/002116

Product Form
In its undiluted state at ambient temperature the product preferably comprises a liquid, preferably an aqueous liquid.
Product Use
The composition can conveniently be delivered from a spray during the domestic ironing operation. Compositions other than those containing silicone resin nanoparticles may be
delivered via a spray through a steam iron or steam generator iron.
Summary of Drawings

Figures la and lb represent a standard Wrinkle Recovery Tester Instrument Model 155 commercially available from James H Heal & Co. Ltd.,
Figure 2 represents images of the existing AATCC 128 Scale,
Figure 3 represents images of the new U Scale and
Figure 4 is a plot showing the comparison of the AATCC scale with the new U Scale.
Evaluation of in-wear wrinkling
It has been discovered that the traditional Crease or Wrinkle Recovery Angle (CRA) approach for characterising anti-wrinkle compositions of inventions, that is AATCC66-1990 (see EP 1096060 (Al)) is largely irrelevant to in-wear wrinkle assessment. In in-wear wrinkling the sharpness of the fold and deformation matters and this is not measured by CRA.

WO 2006/097227 PCT/EP2006/002116

There are many textile industry standard methods (Association of American Textile Chemists and Colourists - AATCC) described for generating and measuring wrinkling on fabric.
The AATCC 128 Wrinkle Recovery Test is that most widely used to determine the wrinkle recovery of garments and is referenced widely in the external literature. A test fabric is wrinkled under standard conditions of load, time and
environmental conditions using a standard Wrinkle Recovery Tester model 155 device supplied by James H Heal & Co Ltd (Figure 1). The level of recovery from a wrinkled state is ranked visually with reference to a standard 3D replica scale, WR1-WR5, where WR1 = no recovery from creasing and WR5 = full
recovery using a defined illumination set-up. Figure 2 shows this 3D AATCC 128 wrinkle scale.
However, the existing 3D AATCC 128 scale is not ideal when testing fabrics for in-wear wrinkling for the following reasons.
The existing AATCC 128 3D standards cannot allow a panellist to distinguish fine differences in intensity of wrinkling. For example in in-wear wrinkling the range of wrinkle falls around 2.5 to 3.5 but the 128 scale covers the broad brush scale of 1 to 5 missing details in the 2.5-3.5 range of interest.
Hence there is a need for a more relevant scale to assess the intensity of wrinkling with good discrimination.
The new scale, called U scale hereafter, emerged from images of woven cotton poplin monitors wrinkled, using the Wrinkle Recovery Tester model 155, to severity between 0 = not

WO 2006/097227 PCT/EP2006/002116

wrinkled (flat) and 10 = severely wrinkled as shown in Figure 3. This scale therefore covers a wider spectrum of wrinkles in the middle range allowing panellists to discriminate fine details in a systematic manner.
Compared to AATCC128 scale, which manifests a rather flat insensitive region around a score of 3, the new U scale allows discrimination between the intensity of wrinkling around this region. Figure 4 shows the comparison between the two scales graphically.
Methodology
1. Monitor Preparation
The test solution is prepared with the desired strength or the desired %owf and stabilised overnight on a roller bank.
The monitor is then weighed (Wl) , soaked in the test solution and compressed between the rollers of the Werner Mathis AG padder so that it weighs double its original weight.
The monitor is left to dry at controlled temperature and RH (20°C/65%RH) for 24 hours and then re-weighed (W2) .
The weight of additive on the monitor is (W2 - Wl) from which the %owf can be calculated.
The dry monitor is ironed flat using the Philips Azur 4000 iron on the hottest setting and with highest steam setting and left to condition for a further 24 hours at controlled T and RH (20°C/65%RH).
Six such test monitors per treatment are prepared.

WO 2006/097227 PCT/EP2006/002116

In each test there are control monitors for comparison with the composition treated monitors. These control monitors are treated with demineralised water instead of the compositions and prepared in the same way
2. Wrinkling
To generate wrinkled state the monitors are loaded onto a Wrinkle Recovery Tester model 155 so that the warp direction is vertical. The fabric is then compressed (wrinkled) using no additional weight for 8 minutes.
After wrinkling the monitors are hung up for 24 hours at 20°C/65%RH.
3. Monitor Assessment
A digital photograph image is taken of each monitor using a Nokia Digital Camera under identical lighting conditions. The standard lighting conditions are achieved using a Verivide Crease Imaging Cabinet.
The images are then loaded into a panelling programme and each image is presented to the panellist to score against images of the scale being used - either AATCC128 or U Scale.
Six trained panellists score all monitors for wrinkle intensity against the scale.

In each test six untreated control monitors are also prepared
and wrinkled in exactly the same way as the treated monitors as described above to enable comparison with the compositions.

WO 2006/097227 PCT/EP2006/002116

The invention will now be illustrated by the following non-limiting examples. Further modifications will be apparent to the person skilled in the art. Samples of the invention are represented by a number. Comparative samples are represented by a letter. All values are percentage by weight of the active ingredient unless stated otherwise.
Examples
Tables 1 and 2 identify the nature of the lubricant and particulate phases used.
Table 1. The physical properties of silicone emulsions (lubricants) tested.

WO 2006/097227 PCT/EP2006/002116

chemistry emulsifier droplet size/nm oilviscosity/mPas s
DC2-8663(DowCorning) linearaminosilicone Nonionic 50 3500
DC2-8177(DowCorning) linear aminosilicone Nonionic 50 12000
DC1652(DowCorning) linear pdms Nonionic 700 350
HMW2220 (Dow Corning) linear pdms -extremely-high MW polymer Nonionic 500 1.2 M
DC1716(DowCorning) PDMS micro emulsion Cationic unknown unknown
CT208E (Wacker) linearaminosi1icone Nonionic unknown unknown
Table 2. Physical properties of some of the colloidal silica dispersions tested.

WO 2006/097227 PCT/EP2006/002116

Trade name charge particle size/ nm Silicacontent/wt%
Ciba 820 (Ciba) ( + ) 22 11
Ludox CL-P silica (Grace) (+) 22 30
Ludox TM40 (Grace) (-) 22 50
Ciba 911 (Ciba) ( + ) 22 ?
Ciba 1143 (Ciba) (-) ? ?
Ludox SP532-10519 (Grace Davison) ( + ) 50 40
Table 3 shows the effect of lubrication treatment on its own. Using silicone oils or most other lubricants provide little or no in-wear wrinkle benefit as the comparison with water controls demonstrates.
Table 3. AATCC128 wrinkle score for different %owf of silicone samples. The HIGHER the score the less the monitors are wrinkled.

silicone emulsions 0.07% owf 0.25% owf 0.5% owf water control
DC2-8663 3.91 3.74 3.66 3.73
DC2-8177 3.28 2.73 2.7 3.11
DC1652 3.47 3.38 3.48 3.49
HMW2220 3.01 2.9 2.07 3.3
DC1716 2.91 2.6 2.58 3.42
CT208E 3.48 3.29 2.65 4.04

WO 2006/097227 PCT/EP2006/002116

Tables 4 and 5 and 6 show that silica particles on their own (stiffener or friction enhancer alone) offer improved in-wear wrinkle benefit. However on their own the fabric feel and handle is too harsh.
Table 4. U Scale wrinkle score for different %owf of silica sample Ludox W50 after lhr. The LOWER the score the less the monitors are wrinkled.

Test 0.50% owf 1.00% owf 2.00% owf water control
Test 1 2.62 2.50 2.58 3.58
Test 2 — 3.53 - 4.3
Test 2 2.03 — - 2.45
Table 5. AATCC128 wrinkle score for different %owf of silica sample C820 after 24hrs. The HIGHER the score the less the monitors are wrinkled.

0.20% owf 0.40% owf 0.79% owf 1.57% owf water control
3.21 3.21 3.55 3.51 2.89
Table 6. U Scale wrinkle score for different %owf of silica sample C820 after 24hrs. The LOWER the score the less the monitors are wrinkled.

0.20% owf 0.40% owf water control
2.50 - 2.70
3.11 - 3.40
2.06 - 2.52
— 2.26 3.30

WO 2006/097227 PCT/EP2006/002116

The particulate phase and lubricant phase combinations of the invention in Table 7 show synergy in in-wear wrinkle resistance at certain ratios.
Table 7. U Scale scores for different owf % of a blend of
Ludox W50 lubricants at different silica:silicone ratios after lhr. The LOWER the score the less the monitors are wrinkled.

lubricant OWF % 1:1 2:1 1:2 water control
DC21310 0.5 2.93 2.13 2.68 2.45
DC21310 1.0 3.48 3.13 3.46 4.30
SPE 0.5 3.63 2.15 3.07 2.46
Silicone DC21310 PDMS (ex DOW CORNING is a polydimethylsiloxane provided as an anionic macro-emulsion having a viscosity before emulsification of 60,000cSt). SPE is sucrose poly ester based on palm kernel oil.
The monitors were tested by a panel for softness and handle.
Silica/silicone and silica/SPE treated monitor at 0.5% level in Table 7 showed good softness. Ease of ironing of the silica + silica blend was comparable to that of Comfort commercial fabric conditioner but compositions using silica alone showed unacceptable iron glide.

Another class of lubricant-particle blends belong to the MQ silicone resin class from Dow Corning shown in Table 8. The intensity of wrinkling is reduced compared to untreated after 1 hr and 24hrs at the preferred deposition levels.

WO 2006/097227

PCT/EP2006/002116

Table 8. U scale wrinkle scores after 1 hr and 24hrs for o/w emulsion of silicone oil/silicone resin blends using cationic emulsifier.

Ratio of PDMS/silicone resin blend (cationic emulsifier)
% owf 40/60 30/70 20/80 Untreated
1hr score 24hr score 1hr score 24hr score 1hr score 24hr score 1hr score 24hr score
0.1 3.71 2.97 3.17 2.61 3.25 2.49 3.60 2.88
0.25 3.08 2.49 2.78 2.29 2.40 1.93 3.60 2.88
Table 9. U scale wrinkle scores after 1 hr and 24hrs for o/w emulsion of silicone oil/silicone resin blends using nonionic
emulsifier.

Ratio of PDMS/silicone resin blend (non-ionic emulsifier)
% owf 40/60 30/70 20/80 Untreated
1hr score 24hr score 1hr score 24hr score 1hr score 24hr score 1hr score 24hr score
0.1 2.67 1.67 2.15 2.08 2.75 2.38 3.58 2.89
0.25 1.83 2.14 2.92 2.25 3.58 2.38 4.00 2.89
In Tables 8 and 9 the emulsion internal phase composition is the same for all samples, only the surfactant used for emulsification is different.
Table 10 shows the percentage D5, PDMS/resin blend and water in the emulsion compositions. The PDMS/resin blend is
dissolved in D5 (a low molecular weight silicone oil solvent) and then emulsified in water.
Table 10. Composition of water and oil phases of the emulsions (surfactants not included).

Ingredient w% in composition
Water 50
■ D5 25
PDMS/resin blend 25

WO 2006/097227 PCT/EP2006/002116

Siloxane resin consisting of monovalent trisiloxy (M) groups having formula R3Si01/2 and tetravalent siloxy (Q) groups
having formula Si04/2 and the polymer is amino functionalised
PDMS with some degree of OH termination of viscosity 4000 mPa s.
Table 11 provides the particle size distribution for the resin blend emulsions used in Tables 8 and 9.
Table 11. Emulsion droplet size of the Dow Corning PDMS/resin
polymer blends.

PDMS/MQ blend Surfactant size/ nm
ratio Type
40/60 Nonionic 139
30/70 Nonionic 129
20/80 Nonionic 161
40/60 Cationic 116
30/70 Cationic 154
20/80 Cationic 139
The silicon resin blend treated monitors showed better softness and handle compared to silica at equal add-on levels.Their ease of ironing was also improved compared to the silica.

WO 2006/097227

PCT/EP2006/002116

CLAIMS:
1. An ironing aid fabric treatment composition comprising:
a) a nanoparticle dispersion comprising particles having an average particle size in the range 5 to 500 nm,
b) a lubricant phase comprising a lubricant selected from silicone oil, sucrose polyester oil and mixtures thereof, and
c) water
wherein the weight ratio of a) : b) is in the range 4 : 1 to 1: 4.
with the proviso that when the colloidal nanoparticle dispersion comprises a silicone resin the composition is not delivered through an iron.
2. An ironing aid fabric treatment composition as claimed in
Claim 1 in which all the particles of the nanoparticle
dispersion have a particle size less than 500 nm.
3. An ironing aid fabric treatment composition as claimed in
Claim 2 in which all the particles of the nanoparticle
dispersion have a particle size less than 100 nm.
4. An ironing aid fabric treatment composition as claimed in any preceding claim in which the particles of the nanoparticle dispersion have an average particle size in the range 15 to 50 nm.
5. An ironing aid fabric treatment composition as claimed in any preceding claim in which the nanoparticles are selected from silica, titania, alumina, zinc oxide and silicone resin.

WO 2006/097227 PCT/EP2006/002116

6. An ironing aid fabric treatment composition as claimed in
Claim 5 in which the nanoparticle dispersion is a cationic,
anionic or neutral colloidal dispersion of silica.
7. An ironing aid fabric treatment composition as claimed in
Claim 5 in which the particles of the colloidal nanoparticle
dispersion comprise silicone resin.
8. An ironing aid fabric treatment composition as claimed in
any preceding claim in which the silicone oil comprises
polydimethyl siloxane.
9. An ironing aid fabric treatment composition as claimed in any preceding claim in which the weight ratio of a) : b) is in the range 3 : 1 to 1 : 3.
10. An ironing aid fabric treatment composition as claimed in
Claim 9 in which the weight ratio of a) : b) is in the range 2
: 1 to 1 : 2.
11. An ironing aid fabric treatment composition as claimed in
any preceding claim which comprises:
0.1 to 50 weight percent of component a),
0.1 to 50 weight percent of component b)
up to 99.8 weight percent water.
12. An ironing aid fabric treatment composition as claimed in
Claim 10 which comprises:
0.5 to 20 weight percent component a),
0.5 to 20 weight percent component b),
0.1 to 15 weight percent surfactant,
0.1 to 5 weight percent perfume, and

WO 2006/097227 PCT/EP2006/002116

up to 70 percent deionised water.
13. An ironing aid fabric treatment product comprising a reservoir containing a composition as claimed in any preceding claim and a spray dispensing valve.
14. A cartridge for insertion into a steam iron comprising a reservoir containing a formulation as claimed in any one of Claims 1 to 12, with the proviso that the colloidal nanoparticle dispersion does not comprise a silicone resin.
15. A method of treating a fabric which comprises applying to
the fabric an iron aid fabric treatment composition
comprising:
a) a colloidal nanoparticle dispersion comprising particles having an average particle size in the range 1 to 500nm,
b) a lubricant phase,
c) water
wherein the ratio of a) : b) is in the range 4 : 1 to 1 : 4, and
simultaneously with said application or thereafter, ironing said fabric under elevated temperature and pressure, with the proviso that when-the colloidal nanoparticle dispersion comprises a silicone resin the fabric treatment composition is not delivered through an iron.
16. A method as claimed in Claim 15 in which the composition
is applied in an amount to deposit from 0.25 to 2 percent by
weight of the total of the particulate phase and lubricant phase.

WO 2006/097227 PCT/EP2006/002116

17. A method as claimed in Claim 16 in which the composition is applied in an amount to deposit from 0.5 to 1 percent by weight of the total of the particulate phase and lubricant phase.
18. A method as claimed in any one of Claims 15 to 17 in
which the composition is as defined in any one of Claims 1 to 12.
19. A method as claimed in any one of Claims 14 to 18 in
which the composition is applied from a steam iron, with the
proviso the composition does not comprise a nanoparticle dispersion comprising silicone resin particles.
20. A method as claimed in any one of Claims 14 to 18 in
which the composition is applied by spraying prior to ironing.
21. The use of a composition as claimed in any one of Claims
1 to 13 to treat fabric to provide anti-wrinkle benefit.