Title of Invention

AQUEOUS LIQUID FABRIC CONDITIONING COMPOSITION

Abstract

An aqueous, liquid fabric conditioning composition comprising: (i) a.quaternary ammonium cationic softening compound in an amount of 1.5 to 60% by wt..; (ii) a perfume having a ClogP of 2 or! more; and (iii) an oily perfume carrier comprising a mineral oil in an amount of 0.1 to 15% by wt. having a ClogP of 3.5 or more; where the composition comprises an emulsion wherein 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements.

Full Text

FORM 2 THE PATENTS ACT, 1970 (39 OF 1970) COMPLETE SPECIFICATION (See Section 10 ; rule 13) 1. TITLE OF INVENTION AQUEOUS LIQUID FABRIC CONDITIONING COMPOSITION 2. HINDUSTAN.-LEVER LIMITED, of Hindustan Lever House, 165/166, Backbay Pveclamation,. Mumbai - 400 020, Maharashtra, India, a company incorporated under the Ind.ian Companies-Act, 1913. The following specification particularly describes and ascertains the nature of this invention and the manner in which it is to be performed. Field of the Invention The present invention relates to fabric conditioning cOmpositions, and in particular, relates to fabric conditioning compositions comprising emulsions having emulsion, droplets with a mean diameter within a certain size range. Background of the Invention Rinse added fabric conditioning compositions are well known. Typically, such compositions comprise aqueous lamellar phase dispersions which have fabric softening properties. One of the problems frequently associated with conventional fabric conditioning compositions is that perfume is lost upon storage of the product or is not delivered to fabric in sufficient quantities. Delivery of insufficient perfume to fabrics is a problem particularly encountered with dilute fabric conditioning compositions, that is compositions containing less than 7.5% by Weight of a quaternary ammonium softening material. In order-to overcome this, more perfume ingredient can be. incorporated into the dilute composition. However, this leads to instability of the composition. The problem of instability is especially noticeable when the product is stored at high temperatures. Instability can manifest itself as a thickening of the product to the point where it is no longer pourable, floceulation of particles within the product or a lack of homogeneity exhibited by surface cracking of the product. It is desirable, that in addition to softening, fabric conditioning compositions have stability upon storage at high temperature and good perfume characteristics such as longevity of fragrance and delivery of perfume to fabric to be treated. WO 97/16516 describes a fabric softening composition comprising hydrophobic particles having a preferred mean diameter of from about 3 to about 15 microns in which the hydrophobic particles comprise perfume surrounded by a cationic softener and nonionic surfactant. A process for forming the composition is described and includes a homogenizing stage so as to provide dispersed small hydrophobic particles of perfume held in suspension by the surfactant activity of the cationic softener and nonionic surfactant. There is no disclosure of compositions comprising a perfume carrier where the carrier and the perfume have hydrophpbicities selected for compatibility with each-other such that particles comprising the perfume partitioned into the perfume carrier are present. US.5288417 relates to a process for making an aqueous dispersion of a fabric softening composition and describes fabric conditioning active mean" particle sizes of about 0:7 to 10 microns. It-does not relate to emulsion-based compositions and has no disclosure or teaching of the use of perfumes in combination with perfume carriers having a hydrophobicity compatible with the perfume. Co-pending application, GB 0021766.1, discloses a composition comprising a aqueous lamellar phase dispersion '* ' of fabric conditioning particles having a mean particle diameter or from 0.3 to 7 microns. EP-B-0458599 discloses a fabric treatment composition comprising lamellar droplets of a fabric softening material in combination with an emulsion component. A deflocculating polymer having a hydrophilic backbone and one or more hydrophobic side chains is also present in the composition EP-A-0746603 discloses a fabric softening composition comprising a quaternary ammonium softening compound and 0.1 to 10 wt% of a perfume/carrier substance mix having a slip point of less than 37°C. Co-pending application PCT/EP00/04223, published as WO-A1-00/71806, discloses a cationic fabric softening agent and an emulsified silicone. The median droplet size of the silicone in the emulsion is 0.2 urn to 25 µm. Cationic and nonionic emulsifiers are disclosed. Co-pending application GB9930436. 2, published as WO-AL-01/46360, discloses compositions comprising an oily sugar stabiliser, a quaternary ammonium softening compound, a perfume and a nonionic surfactant. There is no reference to emulsions or particle sizes. WO-AL-95/22594 discloses a fabric softening composition comprising a quaternary ammonium fabric softening agent and from 0.1 wt% to 10 wt% of a perfume/carrier substance mix having a slip point below 45°C. Although reference is made to the ester-linked quaternary ammonium compounds being present in an amount of at least 1% by weight of the composition, especially interesting are said to be concentrated compositions which comprise between 10 and 30% by weight of ester-linked quaternary ammonium compound. Furthermore, all of the examples relate to highly concentrated compositions containing 14.5 wt% or even 20 wt% of the ester-linked quaternary ammonium compound. There is no enabling disclosure of improving stability and perfume delivery at low concentrations of the quaternary ammonium material. In addition, the only perfume carriers disclosed in the examples are tallow oil and palm oil. There is no disclosure of either mineral oils or the combination of ester oils with a fatty alcohol. Objects of the Invention The present invention seeks to address one or more of the above-mentioned problems, and, to give one or more of the above-mentioned benefits desired by consumers. Surprisingly, we have found that a fabric conditioning composition comprising an aqueous emulsion formed from hydrophobic ingredients where the emulsion has droplets within a certain size range exhibit good physical stability upon storage at high temperature, and excellent perfume characteristics. Summary of the Invention According to the present invention there is provided: an aqueous, liquid fabric conditioning composition comprising: (i) from 2.1 to 7% of a quaternary ammonium cationic softening compound; and (ii) a perfume having a ClogP of 2 or more; and (iii) an oily perfume carrier having a ClogP of 3.5 or more;. where the composition comprises an emulsion in which 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. The invention further provides: an aqueous, liquid fabric conditioning composition comprising: (i) a quaternary ammonium cationic softening compound; and (ii) a perfume having a ClogP of 2 or more; and (iii) an oily perfume carrier comprising a mineral oil having a ClogP of 3.5 or more; where the composition 'comprises an emulsion in which 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. The invention additionally provides: an aqueous, liquid fabric; conditioning composition comprising: (i) a quaternary ammonium cationic softening compound; and (ii) a perfume having a ClogP of 2 or more; and (iii) an oily perfume carrier comprising an ester oil having a ClogP of 3.5 or more; and (iv) a fatty alcohol where the composition comprises an emulsion in which 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. In the context of the present invention, the term "comprising" embraces "consisting of" and "including but not limited to". Thus, the. ingredients or steps following the term "comprising" are not exhaustive. Detailed Description of the Invention The present invention is concerned with aqueous fabric conditioning compositions which comprise emulsions. In the context of the present invention, the term 'emulsion' means a liquid product which, at ambient temperature, is opaque, metastable, comprises droplets, or groups of droplets, of one immiscible liquid suspended in another liquid and which shows none of the signatures of a lamellar phase dispersion as evaluated by low angle x-ray diffraction and polarising light microscopy. The term emulsion does not include conventional micro-emulsions which are clear and isotropic and which are thermodynamically stable across a specified temperature range. Furthermore, it does not include conventional fabric conditioning compositions which consist entirely of aqueous lamellar phase dispersions. Aqueous lamellar phase dispersions consist of a suspension of a lamellar liquid crystalline phase in a liquid, in which the molecular packing of the suspended material results in a structure which exhibits long range order. • The compositions of the present invention may comprise a mixture of emulsion droplets and dispersions. These compositions are entirely different from conventional aqueous lamellar dispersions which are free of an emulsion component. For instance, unlike pure dispersions, mixed emulsion/dispersion compositions do not necessarily exhibit long range order. In the context of the present invention, "long range order" means positional and orientational order of the structure in at least one direction. For an explanation of positional and orientational order, see "Introduction to Liquid Crystals", Chemistry and Physics, P.J. Collings and M Hird, printed 1997, reprinted 1998, p1. Long range order can be verified by detection of Bragg peaks using low angle x-ray diffraction or by observing the composition in a polarising light microscope. In the present invention, it is believed that the hydrophobic perfume partitions into the oily perfume carrier and thus forms perfume carrier/perfume emulsion droplets. Without being bound by theory, it is believed that this is because in a mixed emulsion/dispersion system, it will be thermodynamically preferable for the specified hydrophobic perfume components to partition into the hydrophobic oily perfume carrier (forming emulsion droplets of perfume carrier/perfume) rather than into the dispersion phase. In the rinse cycle of a wash, co-deposition of the mixture of the perfume carrier and perfume improves the efficiency of perfume delivery to and perfume retention on the fabric being treated. Therefore, the fabric conditioning compositions of the present invention comprising an emulsion or a mixture of emulsion and dispersion components (rather than a pure dispersion) are highly desirable because the emulsion (component) provides benefits, particularly perfume delivery benefits and good lubrication of fabric treated with the competition. Emulsion Droplet Sizes In the composition, 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser, according to the method below. More preferably, 80% or more by weight of the droplets have a mean diameter of from 0.5 to 50 microns, most preferably from 0.6 to 35 microns, e.g. 0.6 to 30 microns, or even 0.6 to 25 microns. Without wishing to be bound by theory, it is believed that the droplets, 80% or more by weight of which have a diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser, are agglomerations of minute particles of the oily perfume carrier and perfume which comprise both individual oily emulsion particles/droplets and droplets which consist of flocs of flocculated oily emulsion particles/droplets. Thus, in the context of the present invention, the term droplet includes both individual oily emulsion particle/droplets as well as flocs of flocculated oily emulsion particles/droplets. The nature of the emulsion droplets being measured will, of course, be apparent to the person skilled in the art using a Malvern particle size analyser and following the method of measuring droplet size, as set out below and correlating to measured droplet sizes with observations using a phase-contrast light microscope. Method of Measuring Droplet Size The emulsion droplet size is measured using a Malvern particle size analyser using a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. D[0,1] and D[0,9] readings denote droplet sizes which 10% by weight and 90% by weight respectively of the droplets are below. The particle size analyser is a Malvern Mastersizer X. A presentation code of 2LAD is used to reflect the average refractive index difference between oily droplets and water and between dispersed cationic softening compound lamellar phase particles and water. Without wishing to be bound by theory, it is believed that the results obtained will be dependent at least partly on the lens selected since each lens will have maxima and minima measurement range and thus if particles outside of this range are present they may not be measured. Therefore, to ensure that the droplet mean diameter is within the mean diameter range of the invention, as measured using a 45 mm lens, it must be ensured that the emulsion does not comprise flocs of flocculated particles above the measurement capabilities of a 45 mm lens. Accordingly, a 1000 mm lens is used to confirm the D[0,9] measurement, using the 45 mm lens, so as to ensure that no large flocs (not registered using the 45 mm lens) are present in the emulsion. ClogP Measurements The hydrophobicity of the perfume and oily perfume carrier are measured by ClogP. ClogP' is calculated using the "ClogP" program; (calculation of hydrophobicities as logP (oil/water)) version 4.01, available from Daylight Chemical Information Systems Inc of Irvine California, USA. Quaternary Ammonium Cationic Fabric Softening Compound The fabric conditioning composition of the present invention comprises one or more quaternary ammonium cationic fabric softening compounds. It is preferred that the fabric softening compound(s) used is/are selected from those which are typically included in rinse-added fabric softening compositions. The quaternary ammonium fabric softening compounds may have at least one ester group. The cationic softening compounds may comprise quaternary ammonium compounds having two C8_C28 alkyl or alkenyl chains being directly attached to the nitrogen of the quaternary ammonium group. As a suitable source for the hydrocarbyl chains, fatty compounds based on tallow and/or palm chains are particularly preferred although fatty compounds based on other sources for the hydrocarbyl chain, especially vegetable sources, are also suitable. In examples 8 to 10, pre-washed terry towelling was agitated for 1 minute in a 1 litre Terg-o-tometer pot containing 10° FH water and a 1% solution of anionic surfactant (sodium dodecylbenzene sulphonate, ex Aldrich) to simulate anionic carryover. The cloth was removed and excess water was squeezed out. 1.8 ml of the treatment composition (examples 8 to 10) was added to the Tergo-tometer. The cloth was then returned to the Terg-o-tometer and agitated for a further 5 minutes, after which time the cloth was removed, spun dried for 30 seconds and line dried overnight. The treated cloths were assessed by an expert panel of 12 panellists for perfume intensity on dry fabric 24 hours after it had been treated with the compositions. For all examples, perfume intensity was scored on a comparative numbering system ranging from 0, denoting undetectable, to 5, denoting exceptionally strong perfume. aroma; Results were analysed using a general linear means statistical analysis procedure including normalisation against a standard. The perfume delivery scores are given in tables 3 and 4, below. Table 3; perfume delivery in absence of anionic carryover Example 1 2 3 4 5 A B C Droplet size range (microns) 0.64 to 35 0.62 to 18 0.61 to 20 0.72 to 22 0.83 to 31 0.77 to 66 0.77 to 66 0.77 to 70 Perfume Score 1.30 1.30 1.35 1.55 1.57 0.85 1.10 1.10 80% or more by weight of droplets are within this range, based on D[0, 1] readings using a 45 mm lens and D[0,9] readings using 45 mm and 10,00 mm lenses, taken using a Malvern particle size analyser. "Table 4; perfume delivery with anionic carryover Example 8 9 10 Droplet size ■" ,- • " Perfume Score 1.24 1.48 1.54 See note '1', table 3 In examples 6 and 7 and D to F, 28g of underfumed detergent powder (comprising 22 wt% anionic active ingredient) was predissolved in 7 litres of 10° FH water. 1 Kg of pre-washed terry-towelling was added to the solution and allowed to soak-for 10 minutes. The cloths were then squeezed out by ' hand and rinsed 3 times in 14 litres of water 52 g of the composition selected from examples 6, 7, D, E or F was pre- dispersed in the final rinse water and the cl.oths allowed to soak in the water for 10 minutes. The cloths were then removed and line dried overnight. The treated cloths were assessed for perfume intensity after 24 hours by an expert panel of 8 panellists. The method of measuring perfume intensity was as described above. The results are given in table 5. Table-5 See note '1', table 3 The results in tables 3 and 4 show that for compositions comprising emulsions with at Least 80% of the droplets having a mean diameter within the range specified by the invention, perfume delivery is significantly better than for compositions comprising emulsions with droplets having mean diameters outside of the range of the invention. Storage Stability of the Compositions The compositions of example's 6, 7, D, E and F were stored in sealed Containers at 45°C. The viscosity of each composition was measured after 4 weeks using a Haake RV20 rotoviscometer -1 MV1 cup and bob at a shear rate of 20s at 20°C in order to ascertain long range storage stability of the composition. The results are given in table 6, below. Table 6 .. Measured after 4 weeks storage at 45°C. 3 •• • ..,. ••.-. Measured by sieving through a metal sieve. The flocs are solids Over 1mm in diameter remaining after sieving. Measured visually by a panel of 10 people with the results being averaged and given on a scale of from 0 to 5 where 0 denotes homogeneous and 5 denotes marked surface cracking of the product. The results in table 6 demonstrate that the compositions according to the invention provide long term viscosity ' stability without any loss of homogeneity and with little ••■•■ . -. . . ■ ■ ■•*& -'• .•■'•" . formation of flocs. By contrast, Examples D and F thickened - ■ ■ * unacceptably and suffered high levels of flocculation at high temperature and Example E did not remain homogeneous and also produced significantly higher levels of flocs. We claim: An aqueous, liquid fabric conditioning composition comprising: '(i) a.quaternary ammonium cationic softening compound in an amount of 1.5 to 60% by wt..; (ii) a perfume having a ClogP of 2 or! more; and (iii) an oily perfume carrier comprising a mineral oil in an amount of 0.1 to 15% by wt. having a ClogP of 3.5 or more; where the composition comprises an emulsion wherein 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. 2.., A composition as claimed in claim 1 further comprising fatty alcohol for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. 3. A composition as claimed in any one of claims 1 to 2, wherein the perfume/perfume carrier emulsion droplet is present at a level from 0.5 to 15% by weight based on the total weight of the composition. 4. A composition as claimed in any one of claims 1 to 3, wherein the weight ratio of the perfume/perfume carrier emulsion droplets to quaternary ammonium fabric softening cdmpound is. from 5:1 to 1:25. 5. A composition as claimed in any one of claims 1 to 4, Wherein the weight ratio of perfume to oily perfume carrier is from 1:5:0 to 2:1. 6. A composition as claimed in any one of claims 1 to 5 wherein the quaternary ammonium cationic softening compound is present in an amount from 2.2 to 6% by weight, based on the total weight ot the composition. 7. A composition as claimed in any one of claims 1 to 6 wherein 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.6 to 35 microns, as measured using a Malvern. particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. 8. A composition as claimed in any one of claims 1 to 7 wherein the quaternary ammonium cationic softening compound is represented by formula (I): wherein each R1 group is independently selected from > C1-4 alkyl or hydroxyalkyl or C2-4 alkehyl groups; and wherein each R2 group is independently selected from ! C8-28 alkyl or alkenyl groups; where R1 and R2 are C8-28 alkyl or alkenyl groups; R3 and R4 are C1-4 alkyl or C2-4 alkenyl groups and X is any anion compatible with the cationic surfactant, such as halides or alkyl. sulphates, e.g. chloride, methyl sulphate or ethyl sulphate 10. A method of forming an aqueous, liquid fabric conditioning composition comprising the steps of: (i) co-melting a quaternary ammonium cationic softening compound and a perfume carrier having a ClogP of 3,5 or more; (ii) adding the mixture formed in step (i) to water with milling; (iii) adding perfume haying a ClogP of 2 or more to the mixture formed in step (ii); (iv) subjecting the mixture to further milling. so as to form a composition comprising an emulsion wherein 80% or more by weight of the droplets in the emulsion have a mean diameter of from 0.4 to 60 microns, as measured using a Malvern particle size analyser with a 45 mm lens for D[0,1] measurements and both a 45 mm and a 1000 mm lens for D[0,9] measurements. Dated this 10th day of April 2003 DR. SANCHITA GANGULI Of S. MAJUMDAR & CO. Applicants' Agent

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401-mumnp-2003-claims(granted)-(10-4-2003).doc

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401-MUMNP-2003-CORRESPONDENCE(8-2-2012).pdf

401-mumnp-2003-correspondence(ipo)-(22-3-2007).pdf

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401-mumnp-2003-form 2(granted)-(10-4-2003).doc

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