IMPROVEMENTS RELATING TO FABRIC TREATMENT COMPOSITIONS

Technical Field

The present invention relates to unperfumed melamine- formaldehyde capsules and laundry treatment compositions containing them, particularly fabric softener compositions, and to their uses, particularly for delivery of a perfume benefit to fabric during a laundering process.

Background and Prior Art

Encapsulated perfume technologies are known for use in laundry products. Such technologies provide enhanced fragrance delivery over conventional free perfume oil by overcoming the issue of perfume loss during the drying process by protecting the perfume in the capsule. One type of capsule that has been used in laundry compositions has a melamine formaldehyde shell and a perfume core. Release of perfume from melamine formaldehyde capsules is friction based, the benefit becoming apparent after a rubbing process is applied to the treated fabric. However, these encapsulated perfumes have problems of their own. On storage, leakage of the encapsulated fragrance into the bulk of the product can occur. This results in a reduction of perfume performance with ageing and can also give rise to visco-stability issues as the perfume level in the bulk of the product increases.

A further problem exists, particularly in developing and emerging markets, where the use of expensive innovations

such as perfume capsules is excluded due to the high cost of such technology. A further disadvantage of many products based on perfume-containing melamine formaldehyde capsules, is that the perfume development time is high due to the need to develop a first perfume for addition to the bulk formulation and a second perfume for encapsulation.

Encapsulation of active materials such as fragrances is known in the art, see for example US Patent Nos. 2,800,457, 3,870,542, 3,516,941, 3,415,758, 3,041,288, 5,112,688,

6,329,057, and 6,261,483. Another discussion of fragrance encapsulation is found in the Kirk-Othmer Encyclopaedia.

It is known that the addition of perfume absorbers to a system can improve the stability of the fabric conditioner product. For example, EP845523 (Givaudan) discloses the addition of a liquid ester-based ingredient in a fabric conditioner that prevents the issue of viscosity problems in a perfumed fabric conditioner base. EP1533364A2 (IFF) discloses the use of a hydrophobic solvent in the core of a capsule to help reduce leaching of perfume materials.

WO 01/03825 (Givaudan) discloses a method of encapsulating flavour or fragrance compounds having a hydrogel shell and an oil core. The flavour or fragrance compound is added to an oil-containing microcapsule in its gaseous state in the presence of water such that the compound is transported into the core. A number of food and cosmetic related applications are exemplified.

WO 99/17871 (Givaudan) discloses a method of encapsulating an amphiphilic (defined in the application as being to some extent both water-soluble and lipid-soluble) flavour or fragrance compound in a hydrogel shell having an oil core. The flavour or fragrance compound is added to an oil- containing microcapsule in the presence of water such that the compound is transported into the core by aqueous diffusion. Cosmetic and food related applications are preferred and exemplified.

EP1533365 (International Flavours and Fragrances) discloses a process for imparting fragrance to and/or removing malodour from surfaces treated with surfactant containing compositions, comprising the steps of providing polymer particles having a solid infrastructure composed of ethylene-vinyl acetate copolymer an ethylcellulose polymer, a polystyrene polymer and a polymethyl methacrylate polymer. The particle may be initially empty, and is combined with surfactant containing aqueous solution and the treatment surfaces.

The compositions of the present invention comprise capsules which comprise a carrier oil core and which are substantially perfume free; the composition further comprising a non-encapsulated perfume oil. Surprisingly, a fragrance performance benefit is obtained. This is believed to be as a result of migration of the perfume into the capsules after addition of the capsules to the composition.

The compositions of the invention thus offer an inexpensive route to achieving the benefits of encapsulated perfume

technology, hitherto unavailable to certain markets for reasons of cost. The exclusion of perfume in the capsules removes a vast proportion of the cost associated with perfumed capsules. In addition, the use of the capsules of the invention offer a decreased development time for new perfume variants by eliminating the need for the development of two perfumes.

Another advantage of the present invention is an increased storage stability in comparison to equivalent compositions containing perfumed encapsulates.

Brief Description of the Invention

We have now determined that the addition of substantially perfume free capsules comprising a carrier oil core to a composition comprising free (i.e. unconfined) perfume, results in an improved perfume intensity benefit to fabrics treated with the composition, particularly when the treated fabrics are rubbed. A further advantage of improved viscostability is also seen upon storage of the compositions compared with compositions comprising pre-encapsulated perfumes .

Definition of the Invention

According to a first aspect of the present invention there is provided a process for preparing a laundry treatment composition comprising the steps of

(a) preparing a composition comprising an unconfined perfume,

(b) combining the composition of (a) with capsules comprising a shell and a carrier oil core, wherein the capsules are substantially perfume free, and

(c) allowing migration of the perfume into the capsules.

According to a second aspect of the present invention, there is provided a composition obtainable from the process of the first aspect of the invention.

According to a third aspect of the invention, there is provided a use of a composition according to the second aspect of the invention to deliver enhanced perfume intensity to fabric during a laundry treatment process, wherein the perfume intensity is apparent upon rubbing the fabric .

According to a fourth aspect of the present invention, there is provided a use of the process of the first aspect of the invention for the production of a laundry treatment composition having improved storage stability, wherein the laundry treatment composition comprises capsules and an unconfined perfume.

Detailed Description of the Invention

The Capsules

The capsules can be combined with the composition comprising the unconfined perfume at any time during the preparation of

the laundry treatment composition. The capsules can be added to the composition comprising the unconfined perfume or vice versa. For example, the unperfumed capsules may be post dosed to a pre-made composition comprising the unconfined perfume or may be combined with other ingredients such as water, during the preparation of the composition comprising the unconfined perfume.

The capsules for use in the process of the present invention comprise a shell and a carrier oil core. The shell must be permeable to the free perfume in the composition to which the capsules are added. The shell is thus comprised of materials including aminoplasts, proteins, polyurethanes, polysaccharides, gums and any other encapsulating material which may be used effectively in the present invention, such as polymethylmethacrylate.

Preferred encapsulating polymers include those formed from melamine formaldehyde or urea formaldehyde condensates, as well as similar types of aminoplasts. Most preferably the shell comprises melamine formaldehyde.

Additionally, microcapsules made via the simple or complex coacervation of gelatin are also preferred for use with the coating. Microcapsules having shell walls comprised of polyurethane, polyamide, polyolefin, polysaccaharide, protein, silicone, lipid, gums, polyacrylate, polystyrene,

and polyesters or combinations of these materials are also possible .

A representative process used for aminoplast encapsulation is disclosed in U.S. Patent No. 3,516,941 though it is recognized that many variations with regard to materials and process steps are possible. A representative process used for gelatin encapsulation is disclosed in U.S. Patent No, 2,800,457 though it is recognized that many variations with regard to materials and process steps are possible. Both of these processes are discussed in the context of fragrance encapsulation for use in consumer products in U.S. Patent Nos. 4,145,184 and 5,112,688 respectively.

Encapsulation can provide pore vacancies or interstitial openings depending on the encapsulation techniques employed. The capsules have a hollow nature. The capsules are not intended to include solid porous structures, and do not have a solid infrastructure.

Fragrance capsules known in the art and suitable for use in the present invention comprise a wall or shell comprising a three-dimensional cross-linked network of an aminoplast resin, more specifically a substituted or un-substituted acrylic acid polymer or co-polymer cross-linked with a urea- formaldehyde pre-condensate or a melamine-formaldehyde pre- condensate .

Microcapsule formation using mechanisms similar to the foregoing mechanism, using (i) melamine-formaldehyde or urea-formaldehyde pre-condensates and (ii) polymers

containing substituted vinyl monomeric units having proton- donating functional group moieties (e.g. sulfonic acid groups or carboxylic acid anhydride groups) bonded thereto is disclosed in 44068162 USB U.S. Patent 4,406,816 (2- acrylamido-2-methyl-propane sulfonic acid groups), 2062570 GBA UK published Patent Application GB 2,062,570 A (styrene sulfonic acid groups) and 2006709 GBA UK published Patent Application GB 2,006,709 A (carboxylic acid anhydride groups) .

The capsules for use in the invention have a carrier oil core. The oil must be compatible with the perfume such that the perfume can migrate into the oil core from a surrounding composition. It will be clear to a skilled person which oils are suitable for use with a certain perfume composition. The carrier oils are hydrophobic materials that are miscible in the perfume materials used in the present invention. Suitable oils are those having reasonable affinity for the fragrance chemicals. Suitable materials include, but are not limited to triglyceride oil, mono and diglycerides, mineral oil, silicone oil, diethyl phthalate, polyalpha olefins, castor oil and isopropyl myristate. Preferably, the oil is a triglyceride oil, most preferably a capric/caprylic triglyceride oil.

For liquid compositions, the capsules may be used in the form of a slurry, which preferably comprises about 40% solids. The amount of such a 40% capsule slurry to be used in a composition is up to 10 %, preferably from 0.1 to 5 %,

more preferably from 1 to 2 % by weight of the total composition .

Those with skill in the art will appreciate that the diffusion of the fragrance material into the capsules will depend on various factors including the selection of the fragrance materials, the encapsulating polymer, the surfactant level found in the product, and the physical parameters of the encapsulated particles. By physical properties it is meant such factors such as the thickness of the core, the thickness of the shell, and the relative diameter of the particles.

Particle size and average diameter of the capsules can vary from about 10 nanometers to about 1000 microns, preferably from about 50 nanometers to about 100 microns, more preferably from about 2 to about 40 microns, even more preferably from about 4 to 15 microns. A particularly preferred range is from about 5 to 10 microns, for example 6 to 7 microns. The capsule distribution can be narrow, broad or multimodal. Multimodal distributions may be composed of different types of capsule chemistries.

The capsules for use in the present invention are substantially perfume free.

The Unconfined Perfume

The compositions for use in the process of the invention comprise an unconfined perfume, by which is meant a non- encapsulated perfume. Any suitable perfume or mixture of perfumes may be used. The perfume must be compatible with the carrier oil as described above and must be able to permeate the shell of the capsule. Those with skill in the art will appreciate that the present invention may contain a single ingredient, but it is much more likely that the present invention will comprise at least eight or more fragrance chemicals, more likely to contain twelve or more and often twenty or more fragrance chemicals. The present invention also contemplates the use of complex fragrance formulations containing fifty or more fragrance chemicals, seventy five or more or even a hundred or more fragrance chemicals in a fragrance formulation. Suitable unconfined perfumes for use in the present invention include those disclosed in EP1533364A2 (IFF) .

The Fabric Treatment Composition

The fabric treatment composition, prepared by the process of the invention is suitable for use in a laundry process. Examples include a softening-in-the-wash main wash composition, a rinse treatment composition (e.g. a fabric conditioner or finisher) and a main wash composition. The compositions of the present invention are preferably rinse- added softening compositions.

The compositions obtainable by the process of the invention are preferably liquids.

The liquid compositions may have pH ranging from 2.5 (for fabric care compositions) to 12 (for fabric softening-in- the-wash compositions) .

The active ingredient in the compositions is preferably a fabric softening agent. More than one active ingredient may be included. For some applications a mixture of active ingredients may be used, for example, the main wash compositions may also include a fabric softening agent and the rinse-added fabric softening compositions may also include surface-active compounds, such as non-ionic surface- active compounds.

Any suitable fabric conditioning agent may be used in the compositions of the present invention. The conditioning agents may be cationic or non-ionic. If the fabric conditioning compound is to be employed in a main wash detergent composition the compound will typically be non- ionic. For use in the rinse phase, they will typically be cationic .

The fabric conditioning compositions of the invention may be dilute or concentrated. Dilute products typically contain up to about 8 % by weight of softening active, whereas concentrated products may contain from about 8 to about 25 % by weight active. Compositions of more than about 25 % by weight of active are defined as "super concentrated", depending on the active system, and are also intended to be

covered by the present invention. The fabric conditioning agent may, for example, be used in amounts of from 0.5% to 35%, preferably from 2% to 30% more preferably from 5% to 25% and most preferably from 8% to 20% by weight of the composition.

The preferred softening active for use in rinse conditioner compositions of the invention is a quaternary ammonium compound (QAC) . The preferred quaternary ammonium fabric conditioner for use in compositions of the present invention are the so called "ester quats".

Particularly preferred materials are the ester-linked triethanolamine (TEA) quaternary ammonium compounds comprising a mixture of mono-, di- and tri-ester linked components .

Typically, TEA-based fabric softening compounds comprise a mixture of mono, di- and tri-ester forms of the compound where the di-ester linked component comprises no more than 70% by weight of the fabric softening compound, preferably no more than 60%, e.g. no more than 55%, or even no more than 45% of the fabric softening compound and at least 10 % of the monoester linked component. A preferred hardened type of active has a typical mono:di:tri ester distribution of 18-22 mono: 58-62 di : 18-22 tri, for example 20:60:20. A soft TEA quat may have a typical mono : di : tri ester distribution of 25-45 mono: 45-60 di : 5-25 tri, for example 40:60:10.

A first group of quaternary ammonium compounds (QACs) suitable for use in the present invention is represented by formula (I) :

[ (CHz) _n (TR) ] _m

R ⁱ -N ⁺ - [ (CH ₂ ) _n (OH) ] ₃ _ _m X ^" (I)

wherein each R is independently selected from a C5-35 alkyl or alkenyl group; R ¹ represents a C1-4 alkyl, C2-4 alkenyl or a Ci-4 hydroxyalkyl group; T is generally O-CO. (i.e. an ester group bound to R via its carbon atom) , but may alternatively be CO-O (i.e. an ester group bound to R via its oxygen atom) ; n is a number selected from 1 to 4; m is a number selected from 1, 2, or 3; and X ^~ is an anionic counter-ion, such as a halide or alkyl sulphate, e.g. chloride or methylsulphate . Di-esters variants of formula I (i.e. m = 2) are preferred and typically have mono- and tri-ester analogues associated with them. Such materials are particularly suitable for use in the present invention.

Especially preferred agents are preparations which are rich in the di-esters of triethanolammonium methylsulphate, otherwise referred to as "TEA ester quats".

Commercial examples include Stepantex™ UL85, ex Stepan, Prapagen™ TQL, ex Clariant, and Tetranyl™ AHT-I, ex Kao, (both di- [hardened tallow ester] of triethanolammonium methylsulphate), AT-I (di- [tallow ester] of triethanolammonium methylsulphate), and L5/90 (di- [palm ester] of triethanolammonium methylsulphate) , both ex Kao,

and Rewoquat™ WE15 (a di-ester of triethanolammonium methylsulphate having fatty acyl residues deriving from Cio~ C20 and C16-C18 unsaturated fatty acids) , ex Witco Corporation .

Also, soft quaternary ammonium actives such as Stepantex VK90, Stepantex VT90 (both ex-Stepan) , Ceca Noramine, Prapagen TQ (ex-Clariant) , Dehyquart AU-57 (ex-Cognis) , Rewoquat WE18 (ex-Degussa) and Tetranyl L190 P, Tetranyl L190 SP and Tetranyl L190 S (all ex-Kao) are suitable.

A second group of QACs suitable for use in the invention is represented by formula (II) :

(R ¹ J ₃ N ⁺ - (CH ₂ ) _n -CH-TR ² X ^" (II)

CH ₂ TR ²

wherein each R ¹ group is independently selected from C1-4 alkyl, hydroxyalkyl or C ₂ - ₄ alkenyl groups; and wherein each

R ² group is independently selected from Cs- ₂ 8 alkyl or alkenyl groups; and wherein n, T, and X ^~ are as defined above.

Preferred materials of this second group include 1,2 bis [ tallowoyloxy] -3-trimethylammonium propane chloride, 1,2 bis [hardened tallowoyloxy] -3-trimethylammonium propane chloride, 1, 2-bis [oleoyloxy] -3-trimethylammonium propane chloride, and 1,2 bis [stearoyloxy] -3-trimethylammonium propane chloride. Such materials are described in US 4,137,180 (Lever Brothers) . Preferably, these materials also comprise an amount of the corresponding mono-ester.

A third group of QACs suitable for use in the invention is represented by formula (III) :

(R^ ₂ -N ⁺ -C (CH ₂ ) n-T-R ² ] 2 X ^" (HI)

wherein each R ¹ group is independently selected from Ci_ ₄ alkyl, or C ₂ - ₄ alkenyl groups; and wherein each R ² group is independently selected from Cs- ₂ 8 alkyl or alkenyl groups; and n, T, and X ^~ are as defined above. Preferred materials of this third group include bis (2-tallowoyloxyethyl) dimethyl ammonium chloride and hardened versions thereof.

The iodine value of the quaternary ammonium fabric conditioning material is preferably from 0 to 80, more preferably from 0 to 60, and most preferably from 0 to 45. The iodine value may be chosen as appropriate. Essentially saturated material having an iodine value of from 0 to 5, preferably from 0 to 1 may be used in the compositions of the invention. Such materials are known as "hardened" quaternary ammonium compounds.

A further preferred range of iodine values is from 20 to 60, preferably 25 to 50, more preferably from 30 to 45. A material of this type is a "soft" triethanolamine quaternary ammonium compound, preferably triethanolamine di-alkylester methylsulphate . Typical ester quat ratios of these materials are in the range of from 25 to 45% mono ester quat, from 45 to 60 % diester quat and from 5 to 20 % triester quat, preferably from 30 to 40 % mono ester quat, from 50 to 55 % diester quat and from 10 to 15 % triester quat .

Iodine value as used in the context of the present invention refers to the measurement of the degree of unsaturation present in a material by a method of nmr spectroscopy as described in Anal. Chem., 3_£, 1136 (1962) Johnson and Shoolery.

Iodine value is defined as the number of grams of iodine absorbed per lOOg of the test material. Olefinic materials absorb 1 gram of iodine per atom of olefinic hydrogen. Hence measurement can be converted to the equivalent Iodine Value. The hydrogen nmr spectrum at 360 MHz is obtained for the test material. The integral intensity, I ₃ , of the band derived from olefinic hydrogen in the alkyl chain and the integral intensity, I _m , of the band derived from terminal methyl groups in the alkyl chains are measured.

The number of olefinic hydrogens per molecule is given by:

I_ _s x 6 I _m

and the Iodine Value is given by:

I _s x 127 x 100 x 6 I _m x MMW

where MMW is the mean molecular weight of the test material.

A further type of softening compound is a non-ester quaternary ammonium material represented by formula (IV) :-

R ¹

(IV) R N R X

R ²

wherein each R ¹ group is independently selected from Ci_ ₄ alkyl, hydroxyalkyl or C2-4 alkenyl groups; R ² group is independently selected from Cs-28 alkyl or alkenyl groups, and X ^~ is as defined above.

Co-softeners may be used. When employed, they are typically present at from 0.1 to 20% and particularly at from 0.5 to 10%, based on the total weight of the composition. Preferred co-softeners include fatty esters, and fatty N- oxides. Fatty esters that may be employed include fatty monoesters, such as glycerol monostearate, fatty sugar esters, such as those disclosed WO 01/46361 (Unilever) .

The compositions of the present invention will preferably comprise a fatty complexing agent.

Especially suitable fatty complexing agents include fatty alcohols and fatty acids. Of these, fatty alcohols are most preferred.

- I i

Without being bound by theory it is believed that the fatty complexing material improves the viscosity profile of the composition by complexing with mono-ester component of the fabric conditioner material thereby providing a composition which has relatively higher levels of di-ester and tri-ester linked components. The di-ester and tri-ester linked components are more stable and do not affect initial viscosity as detrimentally as the mono-ester component.

It is also believed that the higher levels of mono-ester linked component present in compositions comprising quaternary ammonium materials based on TEA may destabilise the composition through depletion flocculation . By using the fatty complexing material to complex with the mono-ester linked component, depletion flocculation is significantly reduced.

In other words, the fatty complexing agent at the increased levels, as required by the present invention, "neutralises" the mono-ester linked component of the quaternary ammonium material. This in situ di-ester generation from mono-ester and fatty alcohol also improves the softening of the composition .

Preferred fatty acids include hardened tallow fatty acid (available under the tradename Pristerene™, ex Uniqema) . Preferred fatty alcohols include hardened tallow alcohol (available under the tradenames Stenol™ and Hydrenol™, ex Cognis and Laurex™ CS, ex Albright and Wilson) .

The fatty complexing agent is preferably present in an amount greater than 0.3 to 5% by weight based on the total weight of the composition. More preferably, the fatty component is present in an amount of from 0.4 to 4%. The weight ratio of the mono-ester component of the quaternary ammonium fabric softening material to the fatty complexing agent is preferably from 5:1 to 1:5, more preferably 4:1 to 1:4, most preferably 3:1 to 1:3, e.g. 2:1 to 1:2.

The compositions may further comprise a nonionic surfactant Typically these can be included for the purpose of stabilising the compositions. These are particularly suitable for compositions comprising hardened quaternary ammonium compounds .

Suitable nonionic surfactants include addition products of ethylene oxide and/or propylene oxide with fatty alcohols, fatty acids and fatty amines. Any of the alkoxylated materials of the particular type described hereinafter can be used as the nonionic surfactant.

Suitable surfactants are substantially water soluble surfactants of the general formula:

R-Y-(C ₂ H ₄ O) ₂ -CH ₂ -CH ₂ -OH

where R is selected from the group consisting of primary, secondary and branched chain alkyl and/or acyl hydrocarbyl groups; primary, secondary and branched chain alkenyl hydrocarbyl groups; and primary, secondary and branched chain alkenyl-substituted phenolic hydrocarbyl groups; the

hydrocarbyl groups having a chain length of from 8 to about 25, preferably 10 to 20, e.g. 14 to 18 carbon atoms.

In the general formula for the ethoxylated nonionic surfactant, Y is typically:

-O- , -C(O)O- , -C(O)N(R)- or -C(O)N(R)R-

in which R has the meaning given above or can be hydrogen; and Z is at least about 8, preferably at least about 10 or 11.

Preferably the nonionic surfactant has an HLB of from about 7 to about 20, more preferably from 10 to 18, e.g. 12 to 16. Genapol™ C200 (Clariant) based on coco chain and 20 EO groups is an example of a suitable nonoionic surfactant.

The nonionic surfactant is present in an amount from 0.01 to 10%, more preferably 0.1 to 5 by weight, based on the total weight of the composition.

The compositions of the invention may contain a non-cationic softening material, which is preferably an oily sugar derivative. An oily sugar derivative is a liquid or soft solid derivative of a cyclic polyol (CPE) or of a reduced saccharide (RSE) , said derivative resulting from 35 to 100% of the hydroxyl groups in said polyol or in said saccharide being esterified or etherified. The derivative has two or more ester or ether groups independently attached to a C8-C ₂₂ alkyl or alkenyl chain.

Advantageously, the CPE or RSE does not have any substantial crystalline character at 2O ⁰ C. Instead it is preferably in a liquid or soft solid state as herein defined at 2O ⁰ C.

The liquid or soft solid (as hereinafter defined) CPEs or RSEs suitable for use in the present invention result from 35 to 100% of the hydroxyl groups of the starting cyclic polyol or reduced saccharide being esterified or etherified with groups such that the CPEs or RSEs are in the required liquid or soft solid state. These groups typically contain unsaturation, branching or mixed chain lengths.

Typically the CPEs or RSEs have 3 or more ester or ether groups or mixtures thereof, for example 3 to 8, especially 3 to 5. It is preferred if two or more of the ester or ether groups of the CPE or RSE are independently of one another attached to a Cs to C22 alkyl or alkenyl chain. The Cs to C22 alkyl or alkenyl groups may be branched or linear carbon chains .

Preferably 35 to 85% of the hydroxyl groups, most preferably 40-80%, even more preferably 45-75%, such as 45-70% are esterified or etherified.

Preferably the CPE or RSE contains at least 35% tri or higher esters, eg at least 40%.

The CPE or RSE has at least one of the chains independently attached to the ester or ether groups having at least one unsaturated bond. This provides a cost effective way of making the CPE or RSE a liquid or a soft solid. It is

preferred if predominantly unsaturated fatty chains, derived from, for example, rape oil, cotton seed oil, soybean oil, oleic, tallow, palmitoleic, linoleic, erucic or other sources of unsaturated vegetable fatty acids, are attached to the ester/ether groups.

These chains are referred to below as the ester or ether chains (of the CPE or RSE) .

The ester or ether chains of the CPE or RSE are preferably predominantly unsaturated. Preferred CPEs or RSEs include sucrose tetratallowate, sucrose tetrarapeate, sucrose tetraoleate, sucrose tetraesters of soybean oil or cotton seed oil, cellobiose tetraoleate, sucrose trioleate, sucrose triapeate, sucrose pentaoleate, sucrose pentarapeate, sucrose hexaoleate, sucrose hexarapeate, sucrose triesters, pentaesters and hexaesters of soybean oil or cotton seed oil, glucose tiroleate, glucose tetraoleate, xylose trioleate, or sucrose tetra-, tri-, penta- or hexa- esters with any mixture of predominantly unsaturated fatty acid chains. The most preferred CPEs or RSEs are those with monosaturated fatty acid chains, i.e. where any polyunsaturation has been removed by partial hydrogenation . However some CPEs or RSEs based on polyunsaturated fatty acid chains, eg sucrose tetralinoleate, may be used provided most of the polyunsaturation has been removed by partial hydrogenation .

The most highly preferred liquid CPEs or RSEs are any of the above but where the polyunsaturation has been removed through partial hydrogenation.

Preferably 40% or more of the fatty acid chains contain an unsaturated bond, more preferably 50% or more, most preferably 60% or more. In most cases 65% to 100%, e.g. 65% to 95% contain an unsaturated bond.

CPEs are preferred for use with the present invention. Inositol is a preferred example of a cyclic polyol. Inositol derivatives are especially preferred.

In the context of the present invention, the term cyclic polyol encompasses all forms of saccharides. Indeed saccharides are especially preferred for use with this invention. Examples of preferred saccharides for the CPEs or RSEs to be derived from are monosaccharides and disaccharides .

Examples of monosaccharides include xylose, arabinose, galactose, fructose, sorbose and glucose. Glucose is especially preferred. Examples of disaccharides include maltose, lactose, cellobiose and sucrose. Sucrose is especially preferred. An example of a reduced saccharide is sorbitan .

The liquid or soft solid CPEs can be prepared by methods well known to those skilled in the art. These include acylation of the cyclic polyol or reduced saccharide with an acid chloride; trans-esterification of the cyclic polyol or reduced saccharide fatty acid esters using a variety of catalysts; acylation of the cyclic polyol or reduced saccharide with an acid anhydride and acylation of the

cyclic polyol or reduced saccharide with a fatty acid. See for instance US 4 386 213 and AU 14416/88 (both P&G) .

It is preferred if the CPE or RSE has 3 or more, preferably 4 or more ester or ether groups. If the CPE is a disaccharide it is preferred if the disaccharide has 3 or more ester or ether groups. Particularly preferred CPEs are esters with a degree of esterification of 3 to 5, for example, sucrose tri, tetra and penta esters.

Where the cyclic polyol is a reducing sugar it is advantageous if each ring of the CPE has one ether or ester group, preferably at the Ci position. Suitable examples of such compounds include methyl glucose derivatives.

Examples of suitable CPEs include esters of alkyl (poly) glucosides, in particular alkyl glucoside esters having a degree of polymerisation from 1 to 2.

The length of the unsaturated (and saturated if present) chains in the CPE or RSE is Cs-C ₂₂ , preferably Ci ₂ -C ₂₂ . It is possible to include one or more chains of Ci-Cs, however these are less preferred.

The liquid or soft solid CPEs or RSEs which are suitable for use in the present invention are characterised as materials having a solid: liquid ratio of between 50:50 and 0:100 at 20°C as determined by T2 relaxation time NMR, preferably between 43:57 and 0:100, most preferably between 40:60 and 0:100, such as, 20:80 and 0:100. The T ₂ NMR relaxation time is commonly used for characterising solid: liquid ratios in

soft solid products such as fats and margarines. For the purpose of the present invention, any component of the signal with a T ₂ of less than 100 μs is considered to be a solid component and any component with T ₂ ≥ 100 μs is considered to be a liquid component.

For the CPEs and RSEs, the prefixes (e.g. tetra and penta) only indicate the average degrees of esterification . The compounds exist as a mixture of materials ranging from the monoester to the fully esterified ester. It is the average degree of esterification which is used herein to define the CPEs and RSEs.

The HLB of the CPE or RSE is typically between 1 and 3. Where present, the CPE or RSE is preferably present in the composition in an amount of 0.5-50% by weight, based upon the total weight of the composition, more preferably 1-30% by weight, such as 2-25%, eg 2-20%.

The CPEs and RSEs for use in the compositions of the invention include sucrose tetraoleate, sucrose pentaerucate, sucrose tetraerucate and sucrose pentaoleate.

The compositions of the invention may contain a surface- active compound (surfactant) which may be chosen from soap and non-soap anionic, cationic, non-ionic, amphoteric and zwitterionic surface-active compounds and mixtures thereof. Many suitable surface-active compounds are available and are fully described in the literature, for example, in "Surface- Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.

The preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic and non-ionic compounds. The total amount of surfactant present is suitably within the range of 5 to 60 wt%, preferably from 5 to 40 wt%.

The compositions of the invention may contain anionic surfactants. Examples include alkylbenzene sulfonates, such as linear alkylbenzene sulfonate, particularly linear alkylbenzene sulfonates having an alkyl chain length of Cs- Ci ₅ . It is preferred that the level of linear alkylbenzene sulfonate is from 0 wt% to 30 wt%, more preferably 1 wt% to 25 wt%, most preferably from 2 wt% to 15 wt%.

The compositions of the invention may contain other anionic surfactants in amounts additional to the percentages quoted above. Suitable anionic surfactants are well-known to those skilled in the art. Examples include primary and secondary alkyl sulfates, particularly C8-C20 primary alkyl sulfates; alkyl ether sulfates; olefin sulfonates; alkyl xylene sulfonates; dialkyl sulfosuccinates; and fatty acid ester sulfonates. Sodium salts are generally preferred.

The compositions of the invention may also contain non-ionic surfactant. Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C8-C20 aliphatic alcohols ethoxylated with an average of from 1 to 20 moles of ethylene oxide per mole of alcohol, and more especially the C10-C15 primary and secondary aliphatic alcohols ethoxylated with an average of from 1 to 10 moles of ethylene oxide per mole of alcohol. Non-ethoxylated nonionic

surfactants include alkylpolyglycosides, glycerol monoethers, and polyhydroxyamides (glucamide) .

It is preferred that the level of non-ionic surfactant is from 0 wt% to 30 wt%, preferably from 1 wt% to 25 wt%, most preferably from 2 wt% to 15 wt%.

It is also possible to include certain mono-alkyl cationic surfactants which can be used in main-wash compositions for fabrics. Cationic surfactants that may be used include quaternary ammonium salts of the general formula RiR ₂ R ₃ R ₄ N ⁺ X ^~ wherein the R groups are long or short hydrocarbon chains, typically alkyl, hydroxyalkyl or ethoxylated alkyl groups, and X is a counter-ion (for example, compounds in which Ri is a C8-C22 alkyl group, preferably a Cs-Cio or C12-C14 alkyl group, R2 is a methyl group, and R3 and R ₄ , which may be the same or different, are methyl or hydroxyethyl groups); and cationic esters (for example, choline esters) .

Amphoteric and zwitterionic surfactants that may be used include alkyl amine oxides, betaines and sulfobetaines . In accordance with the present invention, the detergent surfactant (a) most preferably comprises an anionic sulfonate or sulfonate surfactant optionally in admixture with one or more cosurfactants selected from ethoxylated nonionic surfactants, non-ethoxylated nonionic surfactants, ethoxylated sulfate anionic surfactants, cationic surfactants, amine oxides, alkanolamides and combinations thereof .

The choice of surface-active compound (surfactant) , and the amount present, will depend on the intended use of the detergent composition. In fabric washing compositions, different surfactant systems may be chosen, as is well known to the skilled formulator, for handwashing products and for products intended for use in different types of washing machine .

The total amount of surfactant present will also depend on the intended end use and may be as high as 60 wt%, for example, in a composition for washing fabrics by hand. In compositions for machine washing of fabrics, an amount of from 5 to 40 wt% is generally appropriate. Typically the compositions will comprise at least 2 wt% surfactant e.g. 2- 60%, preferably 15-40% most preferably 25-35%.

Detergent compositions suitable for use in most automatic fabric washing machines generally contain anionic non-soap surfactant, or non-ionic surfactant, or combinations of the two in any suitable ratio, optionally together with soap.

The compositions of the invention, when used as main wash fabric washing compositions, will generally also contain one or more detergency builder. The total amount of detergency builder in the compositions will typically range from 0 to 80 wt%, preferably from 0 to 60 wt%.

Inorganic builders that may be present include sodium carbonate, if desired in combination with a crystallisation seed for calcium carbonate, as disclosed in GB 1 437 950

(Unilever) ; crystalline and amorphous aluminosilicates, for

example, zeolites as disclosed in GB 1 473 201 (Henkel) , amorphous aluminosilicates as disclosed in GB 1 473 202 (Henkel) and mixed crystalline/amorphous aluminosilicates as disclosed in GB 1 470 250 (Procter & Gamble) ; and layered silicates as disclosed in EP 164 514B (Hoechst) . Inorganic phosphate builders, for example, sodium orthophosphate, pyrophosphate and tripolyphosphate are also suitable for use with this invention.

The compositions of the invention preferably contain an alkali metal, preferably sodium, aluminosilicate builder. Sodium aluminosilicates may generally be incorporated in amounts of from 5 to 60% by weight (anhydrous basis) , preferably from 10 to 50 wt%, especially from 25 to 50 wt%.

The alkali metal aluminosilicate may be either crystalline or amorphous or mixtures thereof, having the general formula: 0.8-1.5 Na ₂ O. Al ₂ O ₃ . 0.8-6 SiO ₂

These materials contain some bound water and are required to have a calcium ion exchange capacity of at least 50 mg CaO/g. The preferred sodium aluminosilicates contain 1.5-3.5 SiO ₂ units (in the formula above) . Both the amorphous and the crystalline materials can be prepared readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature. Suitable crystalline sodium aluminosilicate ion-exchange detergency builders are described, for example, in GB 1 429 143 (Procter & Gamble) . The preferred sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof.

The zeolite may be the commercially available zeolite 4A now widely used in laundry detergent powders. In an alternative embodiment of the invention, the zeolite builder incorporated in the compositions of the invention is maximum aluminium zeolite P (zeolite MAP) as described and claimed in EP 384 070A (Unilever) . Zeolite MAP is defined as an alkali metal aluminosilicate of the zeolite P type having a silicon to aluminium ratio not exceeding 1.33, preferably within the range of from 0.90 to 1.33, and more preferably within the range of from 0.90 to 1.20.

In the case of zeolite MAP, zeolite MAP having a silicon to aluminium ratio not exceeding 1.07, more preferably about 1.00, is especially preferred. The calcium binding capacity of zeolite MAP is generally at least 150 mg CaO per g of anhydrous material.

The zeolites may be supplemented by other inorganic builders, for example, amorphous aluminosilicates, or layered silicates such as SKS-6 ex Clariant.

The zeolite may be supplemented by organic builders. Organic builders that may be present include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di and trisuccinates, carboxymethyloxy succinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyl iminodiacetates, alkyl- and alkenylmalonates and succinates; and sulfonated fatty acid salts. This list is not intended to be exhaustive.

Especially preferred organic builders are citrates, suitably used in amounts of from 1 to 30 wt%, preferably from 5 to 30 wt%, more preferably from 10 to 25 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%.

Builders, both inorganic and organic, are preferably present in alkali metal salt, especially sodium salt, form.

Builders are suitably present in total amounts of from 10 to 80 wt%, more preferably from 20 to 60 wt%. Builders may be inorganic or organic.

A built composition in accordance with the invention may most preferably comprise from 10 to 80 wt% of a detergency builder (b) selected from zeolites, phosphates, and citrates .

The laundry detergent composition will generally comprises other detergent ingredients well known in the art. These may suitably be selected from bleach ingredients, enzymes, sodium carbonate, sodium silicate, sodium sulphate, foam controllers, foam boosters, perfumes, fabric conditioners, soil release polymers, dye transfer inhibitors, photobleaches, fluorescers and coloured speckles.

Compositions according to the invention may also suitably contain a bleach system. Fabric washing compositions may desirably contain peroxy bleach compounds, for example, inorganic persalts or organic peroxyacids, capable of yielding hydrogen peroxide in aqueous solution.

Suitable peroxy bleach compounds include organic peroxides such as urea peroxide, and inorganic persalts such as the alkali metal perborates, percarbonates, perphosphates, persilicates and persulfates. Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate .

Especially preferred is sodium percarbonate having a protective coating against destabilisation by moisture. Sodium percarbonate having a protective coating comprising sodium metaborate and sodium silicate is disclosed in GB 2 123 044B (Kao) .

The peroxy bleach compound is suitably present in an amount of from 0.1 to 35 wt%, preferably from 0.5 to 25 wt%. The peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures. The bleach precursor is suitably present in an amount of from 0.1 to 8 wt%, preferably from 0.5 to 5 wt%.

Preferred bleach precursors are peroxycarboxylic acid precursors, more especially peracetic acid precursors and pernonanoic acid precursors. Especially preferred bleach precursors suitable for use in the present invention are N, N, N ' , N ' , -tetracetyl ethylenediamine (TAED) and sodium nonanoyloxybenzene sulphonate (SNOBS) . The novel quaternary ammonium and phosphonium bleach precursors disclosed in US 4 751 015 and US 4 818 426 (Lever Brothers Company) and EP 402 971A (Unilever) , and the cationic bleach precursors disclosed in EP 284 292A and EP 303 520A (Kao) are also of interest.

The bleach system can be either supplemented with or replaced by a peroxyacid, examples of such peracids can be found in US 4 686 063 and US 5 397 501 (Unilever) . A preferred example is the imido peroxycarboxylic class of peracids described in EP A 325 288, EP A 349 940, DE 382 3172 and EP 325 289. A particularly preferred example is phthalimido peroxy caproic acid (PAP) . Such peracids are suitably present at 0.1 - 12%, preferably 0.5 - 10%.

A bleach stabiliser (transition metal sequestrant) may also be present. Suitable bleach stabilisers include ethylenediamine tetra-acetate (EDTA) , diethylenetriamine pentaacetate (DTPA) , the polyphosphonates such as Dequest (Trade Mark) , ethylenediamine tetramethylene phosphonate (EDTMP) and diethylenetriamine pentamethylene phosphate

(DETPMP) and non-phosphate stabilisers such as EDDS (ethylene diamine disuccinate) . These bleach stabilisers are also useful for stain removal especially in products containing low levels of bleaching species or no bleaching species.

An especially preferred bleach system comprises a peroxy bleach compound (preferably sodium percarbonate optionally together with a bleach activator) , and a transition metal bleach catalyst as described and claimed in EP 458 397A, EP 458 398A and EP 509 787A (Unilever) .

The compositions according to the invention may also contain one or more enzyme (s) . Suitable enzymes include the proteases, amylases, cellulases, oxidases, peroxidases and lipases usable for incorporation in detergent compositions. Preferred proteolytic enzymes (proteases) are, catalytically

active protein materials which degrade or alter protein types of stains when present as in fabric stains in a hydrolysis reaction. They may be of any suitable origin, such as vegetable, animal, bacterial or yeast origin.

Proteolytic enzymes or proteases of various qualities and origins and having activity in various pH ranges of from 4-12 are available and can be used in the instant invention. Examples of suitable proteolytic enzymes are the subtilins which are obtained from particular strains of B. Subtilis B. licheniformis, such as the commercially available subtilisins Maxatase (Trade Mark), as supplied by Gist Brocades N. V., Delft, Holland, and Alcalase (Trade Mark) , as supplied by Novo Industri A/S, Copenhagen, Denmark.

Particularly suitable is a protease obtained from a strain of Bacillus having maximum activity throughout the pH range of 8-12, being commercially available, e.g. from Novo Industri A/S under the registered trade-names Esperase (Trade Mark) and Savinase (Trade-Mark) . The preparation of these and analogous enzymes is described in GB 1 243 785. Other commercial proteases are Kazusase (Trade Mark obtainable from Showa-Denko of Japan) , Optimase (Trade Mark from Miles Kali-Chemie, Hannover, West Germany) , and Superase (Trade Mark obtainable from Pfizer of U.S.A.) .

Detergency enzymes are commonly employed in granular form in amounts of from about 0.1 to about 3.0 wt%. However, any suitable physical form of enzyme may be used.

The compositions of the invention may contain alkali metal, preferably sodium, carbonate, in order to increase detergency and ease processing. Sodium carbonate may suitably be present in amounts ranging from 1 to 60 wt%, preferably from 2 to 40 wt%. However, compositions containing little or no sodium carbonate are also within the scope of the invention.

Powder flow may be improved by the incorporation of a small amount of a powder structurant, for example, a fatty acid (or fatty acid soap) , a sugar, an acrylate or acrylate/maleate copolymer, or sodium silicate. One preferred powder structurant is fatty acid soap, suitably present in an amount of from 1 to 5 wt%. The amount of sodium silicate may suitably range from 0.1 to 5 wt%.

Other materials that may be present in detergent compositions of the invention include sodium silicate; antiredeposition agents such as cellulosic polymers; soil release polymers; inorganic salts such as sodium sulfate; lather control agents or lather boosters as appropriate; proteolytic and lipolytic enzymes; dyes; coloured speckles; perfumes; foam controllers; fluorescers and decoupling polymers. This list is not intended to be exhaustive.

The detergent composition when diluted in the wash liquor (during a typical wash cycle) will typically give a pH of the wash liquor from 7 to 10.5 for a main wash detergent.

Particulate detergent compositions are suitably prepared by spray-drying a slurry of compatible heat-insensitive

ingredients, and then spraying on or post-dosing those ingredients unsuitable for processing via the slurry. The skilled detergent formulator will have no difficulty in deciding which ingredients should be included in the slurry and which should not.

Particulate detergent compositions of the invention preferably have a bulk density of at least 400 g/litre, more preferably at least 500 g/litre. Especially preferred compositions have bulk densities of at least 650 g/litre, more preferably at least 700 g/litre.

Such powders may be prepared either by post-tower densification of spray-dried powder, or by wholly non-tower methods such as dry mixing and granulation; in both cases a high-speed mixer/granulator may advantageously be used. Processes using high-speed mixer/granulators are disclosed, for example, in EP 340 013A, EP 367 339A, EP 390 251A and EP 420 317A (Unilever) .

Liquid detergent compositions can be prepared by admixing the essential and optional ingredients thereof in any desired order to provide compositions containing components in the requisite concentrations. Liquid compositions according to the present invention can also be in compact form which means it will contain a lower level of water compared to a conventional liquid detergent.

Examples

Embodiments of the invention are now illustrated with reference to the following non-limiting examples. Unless stated otherwise, all proportions are given in weight percent, by weight of the total composition.

Example 1 - Preparation of Examples El and E2 and Comparative Examples A and B

Examples El and E2 are perfumed fabric conditioners (comprising one free perfume) comprising umperfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil;

Comparative Examples A and B are equivalent fabric conditioners containing the same amount of perfume but no capsules .

Table 1:- compositions of Examples El and E2 and Comparative Examples A and B.

Component A El B E2

Stepantex UL85 (85 % active) (1) 13 .49 13.49 13 .49 13.49

Stenol C1618L (2) 0 .9 0.9 0 .9 0.9

Genapol C200 (3) 0 .33 0.33 0 .33 0.33

Perfume 1 (4) 0 .57 0.57 0 0

Perfume 2 (4) 0 0 0 .57 0.57

Non-perfumed capsules (5) 0 2 0 2

Minors (antifoam, dye and preservative) 0 .02 0.02 0 .02 0.02 (7)

Water to 100 %

(1) Hardened TEAQ; Stepan

(2) Cetearyl Alcohol (BN); Cognis

(3) Non-ionic surfactant (Alcohol Ethoxylate Type 1214-A 20) ; Clariant

(4) Supplied by IFF

(5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil) , in a slurry having approx 40 % solids

(6) Melamine formaldehyde capsules containing perfume 2

(7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

The compositions shown in Table 1 above were prepared using the following method: -

1. The TEAQ, non-ionic surfactant and cetearyl alcohol were melted together at 65°C to form a premix.

2. The water was heated with the antifoam, dye and preservative, to 65°C with pump and stirrer on.

3. The melted premix was added to the water composition of step 2 over 5 minutes, with a pump and stirrer. 4. 1 batch volume was milled when hot before cooling was initiated.

5. At 50 ⁰ C, milling was performed for 2 batch volumes.

6. At 30 ⁰ C, milling was performed for a further batch volume if required to achieve target viscosity of from 60 to 90 mPa.s.

7. The neat perfume oil and the non-perfumed capsules, where present, were post-dosed into the resulting base composition .

8. The composition was mixed with an overhead stirrer for 15 minutes.

Example 2 - Average perfume intensity on fabric conferred by Examples El and E2 and Comparative Examples A and B

Examples El and E2, in accordance with the present invention, were tested for perfume intensity performance according to the procedure outlined below. Comparative fabric conditioner compositions (Comparative Examples A and B) were also tested in the same way.

The procedure for washing the cloths was as follows :-

4Og of terry towelling fabric (20 cm x 20 cm) was washed in 1 litre of cold water (about 15°FH) for 1 minute in a tergotometer rinsing pot with agitation of 70 rpm. The cloths were removed and wrung out. This initial rinse water was disposed of. Fabric conditioner composition El, E2, A or B (0.77g) was added to a further 1 litre of cold water (about 15°FH) . The cloths were rinsed therein for 5 minutes. The cloths were then removed from the water, wrung out and spun in a top loading spin-dryer for about 30 seconds. The cloths were then line dried for 24 hours prior to perfume assessment.

Panel assessment of perfume intensity

A panel of expert trained perfume intensity panellists was used to assess perfume intensity. Each panellist assessed up to 3 pieces of treated fabric per test product in a sequential monadic test, i.e. where no direct comparison is used. The perfume intensity was scored on a scale of from 0 to 4 with discrete points at half unit intervals. A score of 0 indicated no perfume intensity whilst a score of 4 corresponded to very strong perfume intensity.

The cloths were assessed by folding in half, smelling the fabric and rating the perfume intensity. This gave the "pre-rub" score.

After each cloth had been assessed the complete set of cloths were re-assessed using a rubbing method as follows:-

The folded cloth was rubbed together in a forward and backwards motion 5 times (i.e. forward motion = 1 rub, backwards motion = 1 rub) . The cloth was then immediately re-assessed for perfume intensity by smelling the fabric. This gave the "post-rub" score.

Following the rubbing assessment, the cloths were stacked and stored on drying racks for 14 days before being reassessed for perfume intensity.

16 cloths were treated with each composition. 8 panellists each tested 2 of these cloths. An average of the resulting 16 scores was calculated for each treatment.

The data was analysed using a standard statistical software package. Significance testing was carried out using Analysis of Variance and if significant differences were found this was followed by a multiple comparison test, Tukey.

Table 2 - Average perfume intensity scores for cloths treated with compositions El, E2, A and B as described above .

It will be seen that the post-rub perfume intensity is greatly improved by the addition of the non-perfumed capsules to perfumed compositions.

Example 3 - Preparation of Examples E3, E4 and Comparative Example C

Example E3 is a perfumed fabric conditioner comprising non- perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil and one free perfume; Example E4 is a perfumed fabric conditioner composition comprising a mixture of two free perfumes and non-perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil, and

Comparative Example C is fabric conditioner containing the same amount of free perfume as Example E3 but no capsules;

Table 3:- Compositions of Examples E3, E4 and Comparative Example C.

(1) Hardened TEAQ; Stepan

(2) Cetearyl Alcohol (BN); Cognis

(3) Non-ionic surfactant (Alcohol Ethoxylate Type 1214-A 20) ; Clariant

(4) Supplied by IFF (5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil), in a slurry having approx 40 % solids

(7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

The compositions shown in Table 3 above were prepared using the following method: -

1. The TEAQ, non-ionic surfactant and cetearyl alcohol were melted together at 65°C to form a premix.

2. The water was heated with the antifoam, dye and preservative, to 65°C with pump and stirrer on. Where capsules were present in the composition, these were added to the water at this stage. 3. The melted premix was added to the water composition of step 2 over 3 minutes, with a pump and stirrer. 4. After addition of the premix was completed, the HCl was added and the resulting composition mixed for 4 minutes at 65°C 5. The composition was then allowed to start cooling with pump and stirrer on.

6. Neat perfume was added at 45°C, where required.

7. At 30 ⁰ C, the viscosity was measured and the composition milled if necessary to reach a viscosity in the range of from 60 to 90 mPa.s.

Example 4 - Average perfume intensity on fabric conferred by Examples E3 and E4 and Comparative Example C

Examples E3, E4 and Comparative Example C were tested for perfume intensity performance according to the procedure outlined above. The results are given in Table 4 below.

Table 4 - Average perfume intensity scores for cloths treated with compositions E3, E4 and C as described above.

Again, an advantage is seen in compositions to which non- perfumed capsules have been added, in accordance with the invention .

Example 5 - Preparation of Examples E5, E6 and Comparative Examples E and F

Example E5 is a perfumed fabric conditioner (with one free perfume) comprising non-perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil; Example E6 is a perfumed fabric conditioner composition containing non-perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil as well as a mixture of two free perfumes,

Comparative Example E is a fabric conditioner containing the same amount of free perfume as in Example E5 but no capsules, and

Comparative Example F is a fabric conditioner composition comprising free perfume and an encapsulated perfume.

Table 5:- Compositions of Examples E5, E6 and Comparative Examples E and F.

(1) Hardened TEAQ; Stepan

(2) Cetearyl Alcohol (BN); Cognis

(3) Non-ionic surfactant (Alcohol Ethoxylate Type 1214 -A 20) ; Clariant

(4) Supplied by IFF (5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil) , in a slurry having approx 40 % solids (6) Melamine formaldehyde capsules containing perfume 4, in a slurry having approx 40 % solids and 28 % perfume (7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

- A l -

The compositions shown in Table 5 above were prepared using the following method: -

1. The TEAQ, non-ionic surfactant and cetearyl alcohol were melted together at 65°C to form a premix.

2. The water was heated with the antifoam, dye and preservative, to 65°C with pump and stirrer on. Where capsules were present in the composition, these were added to the water at this stage. Neat perfume 4 was also added into the water at this stage (for Example E6) .

3. The melted premix was added to the water composition of step 2 over 3 minutes, with a pump and stirrer.

4. After addition of the premix was completed, the HCl was added and the resulting composition mixed for 4 minutes at 65°C.

5. The composition was then allowed to start cooling with pump and stirrer on.

6. Neat perfume 3 was added at 45°C to all the compositions.

7. At 30 ⁰ C, the viscosity was measured and the composition milled if necessary to reach a viscosity in the range of from 60 to 90 mPa.s.

Example 6: Effect of ageing of Examples E5, E6 and Comparative Examples E and F on perfume intensity performance

Examples E5, E6 and Comparative Examples E and F were tested for perfume intensity performance according to the procedure outlined above. The results are given in Table 6 below.

Table 6: Average perfume intensity scores for Examples E5, E6 and Comparative Examples E and F before and after ageing at 37°C for 4, 8 and 12 weeks

It will be seen that an advantage of the inclusion of non- perfumed capsules containing triglyceride oil in a fabric conditioner composition is their propensity to maintain the fresh performance over time when stored at elevated temperature. Equivalent perfumed capsules lose their perfume performance gradually when stored at high temperatures as a consequence of perfume leakage from the capsules .

Although the initial performance of the fresh products containing the unperfumed triglyceride capsules is significantly lower than equivalent perfumed capsules, once the products have been aged for up to 8 weeks at 37 ⁰ C there is no difference in the post rub perfume intensity performance of the triglyceride capsules.

This shows that a higher level of neat perfume in the product as in Example 6, i.e. higher total perfume (comparative to total perfume in Example F) , leads to higher pre-rub scores.

Example 7 - Preparation of Examples E7, E8 and Comparative Example G

Example E7 is a perfumed fabric conditioner comprising non- perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil and one unconfined perfume; Example E8 is a perfumed fabric conditioner comprising a mixture of 2 free perfumes and non-perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil; and

Comparative Example G contains free perfume and no capsules

Table 7:- Compositions of Examples E7, E8 and Comparative Example G.

(1) Hardened TEAQ; Stepan

(2) Cetearyl Alcohol (BN); Cognis

(3) Non-ionic surfactant (Alcohol Ethoxylate Type 1214-A 20) ; Clariant

(4) Supplied by IFF

(5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil) , in a slurry having approx 40 % solids

(7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

The compositions shown in Table 7 above were prepared as follows : -

1. The TEAQ, non-ionic surfactant and cetearyl alcohol were melted together at 65°C to form a premix.

2. The water was heated with the antifoam, dye and preservative, to 65°C with pump and stirrer on. Where capsules were present in the composition, these were added to the water at this stage. Neat perfume 4 was also added into the water at this stage (for Example E8) .

3. The melted premix was added to the water composition of step 2 over 3 minutes, with a pump and stirrer.

4. After addition of the premix was completed, the HCl was added and the resulting composition mixed for 4 minutes at 65°C.

5. The composition was then allowed to start cooling with pump and stirrer on.

6. Neat perfume 3 was added at 45°C to all the compositions .

7. At 30 ⁰ C, the viscosity was measured and the composition milled if necessary to reach a viscosity in the range of from 60 to 90 mPa.s.

Example 8: Effect of ageing of Examples E7, E8 and Comparative Example G on perfume intensity performance

Examples E7, E8 and Comparative Example G were aged at 20°C for 9 weeks and then tested for perfume intensity performance according to the procedure outlined above (i.e. performed on fabrics 24 hours post-treatment with the fabric conditioner compositions) . The same treated cloths were then stored for a further 12 days before being re-assessed for perfume intensity before and after rubbing.

The results are given in Table 8 below.

Table 8 - Average perfume intensity scores for Examples E7, E8 and Comparative Example G before and after ageing for 9 weeks at 20°C and then a further 12 days.

As can be seen, the perfume benefit on the fabric treated with compositions in accordance with the invention remains consistently higher than on fabric treated with capsule-free compositions .

Example 9: Addition of Non-perfumed triglyceride capsules to commercially available fabric softener (Example E9)

A commercially available fabric softener (Comfort Blue concentrate) was purchased from a shop. This was designated as Comparative Example H.

Non-perfumed triglyceride capsules were added to the Comfort Blue concentrate as follows :-

A 1.79 % slurry (by weight) containing non-perfumed capsules with triglyceride oil was prepared and post-dosed into the Comfort Blue concentrate and mixed with an overhead stirrer for 20 minutes. The resulting composition was designated Example E9.

Example 10 - Perfume intensity on fabric conferred by Example E9 and Comparative Example H

Test fabrics were washed within approximately 2 hours of the capsules being added to the shop-bought fabric conditioner and the perfume assessment (described above) carried out 24 hours after the wash. The same samples were then tested after having been stored at ambient temperature for 10 weeks and the perfume intensity assessed 24 hours after the wash and again after a further 13 days.

Table 9: Average perfume intensity scores for Examples E9 and Comparative Example H before and after ageing

It will be seen that there is a boost in post-rub perfume intensity on rubbing of the cloth treated with the fabric conditioner containing the non-perfumed capsules. In both cases there was a boost in performance post-rub and the intensity was significantly higher than the control that did not contain any capsules.

Example 11: Preparation of Example ElO and Comparative Example I

Example ElO is a perfumed fabric conditioner comprising non- perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil one unconfined perfume; Comparative Example I is a perfumed fabric conditioner comprising conventional perfumed capsules.

Table 10:- Compositions of Examples ElO and Comparative Example I .

(1) Hardened TEAQ; Stepan (2) Cetearyl Alcohol (BN); Cognis (4) Supplied by IFF

(5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil), in a slurry having approx 40 % solids

(6) Melamine formaldehyde capsules containing perfume 4, in a slurry having approx 40 % solids and 28% perfume

(7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

1. The TEAQ and cetearyl alcohol were melted together at 65°C to form a premix.

2. The water was heated with the antifoam, dye and preservative to 65°C with pump and stirrer on. Where capsules were present in the composition, these were added to the water at this stage.

3. The melted premix was added to the water composition of step 2 over 3 minutes, with a pump and stirrer.

4. After addition of the premix was completed, the HCl was added and the resulting composition mixed for 4 minutes at 65°C

5. The composition was then allowed to start cooling with pump and stirrer on.

6. Neat perfume 3 was added at 45°C to all the compositions . 7. At 30 ⁰ C, the viscosity was measured and the composition milled if necessary to reach a viscosity in the range of from 60 to 90 mPa.s.

Example 12 - Effect on viscostability of Examples ElO and Comparative Example I

Table 11: Viscosity (mPa.s) of compositions Example ElO and Comparative Example I upon ageing at 37°C for up to 161 days

Viscosity as measured using a Haake VT550, with an MV cup and MVl rotor operating at 106s-l.

It will be seen that a fabric conditioner product containing unperfumed triglyceride oil capsules in accordance with the invention has an increased shelf life compared with fabric conditioner compositions containing perfume capsules.

Example 13 - Preparation of Examples Ell and Comparative Examples J, K and L

Example Ell is a perfumed fabric conditioner comprising non- perfumed melamine formaldehyde capsules containing capric/caprylic triglyceride oil and one unconfined perfume in accordance with the invention;

Comparative Example J is a perfumed fabric conditioner further comprising conventional perfumed capsules; Comparative Example K is a perfumed fabric conditioner further comprising conventional perfumed capsules; and Comparative Example L is a perfumed fabric conditioner, which does not contain any capsules.

These compositions were prepared using the same method as given above .

Table 12:- Compositions of Example Ell and Comparative Examples J, K and L.

Component J K L Ell

Stepantex UL85 (85 % active) (D 11 .93 11.93 11 .93 11 .93

Stenol C1618L (2) 1 13 1.13 1 .13 1. 13

Perfume 3 (4) 0 .5 0.75 0 .5 0 .5

Non-perfumed capsules (5) 1. 79

Perfumed capsules (6) 1 79 1.08

Minors (antifoam, dye and 0 02 0.02 0 .02 0. 02 preservative) (7)

Water to 100 %

(1) Hardened TEAQ; Stepan

(2) Cetearyl Alcohol (BN); Cognis

(4) Supplied by IFF

(5) Melamine formaldehyde capsules containing Neobee M5 (a capric/caprylic triglyceride oil) , in a slurry having approx 40 % solids

(6) Melamine formaldehyde capsules containing perfume 4

(7) The preservative used was Proxel GXL, 20 % active, ex Arch Chemicals, the antifoam used was 20 % active silicone antifoam

Example 14 - Effect of storage on the stability of the quaternary ammonium active contained in Example Ell and Comparative Examples J, K and L

Example Ell and Comparative Examples J, K and L were stored at 37°C for 140 days. The free fatty acid level in the compositions was determined as a measure of the extent of hydrolysis of the quaternary softening active at 112 days and 140 days. The data for the free fatty acid when viscous was calculated by fitting a quadratic to the level of free fatty acid with time on store.

The first 2 data columns in Table 13 show the actual data as measured; the 3rd column of data is the calculated level of free fatty acid when the product actually went viscous.

Table 13:- Free fatty acid levels (wt % of free fatty acid as wt % of total solids) of compositions Example Ell and Comparative Examples J, K and L after storage at 112 days and 140 days.

Composition Free fatty Free fatty Free fatty acid (%) at acid (%) at acid (%) when

112 days 140 days viscous

J 28.9 38.1 22.8

K 25.2 35.4 25

L 25.9 34.8 28.4

Ell 26.7 39.1 28.7

It will be seen that Example Ell, in accordance with the invention can tolerate a higher level of free fatty acid in the formulation before going viscous in comparison with the perfumed capsule systems and the non-capsuled system.