PROCESS TO MANUFACTURE AN EXTERNALLY STRUCTURED ISOTROPIC AQUEOUS DETERGENT LIQUID

Abstract

The present invention relates to a process of incorporating charged microcapsules into a structured aqueous liquid detergent comprising: total surfactant in the range 3 weight % to 70 weight %, wherein the total surfactant comprises at least 5 weight anionic surfactant; at least 0.05% activated citrus fibre external structurant and at least 0.001 weight % microcapsules, the process comprising the step of combining two premixes A and B to form the liquid detergent; wherein Premix B comprises the structured aqueous concentrated liquid detergent formulation in the absence of the microcapsules; and Premix A comprises an aqueous dispersion of the charged microcapsules characterised in that Premix A comprises a slurry of charged microcapsules diluted with at least an equal weight of water; and wherein the structured aqueous concentrated liquid detergent comprises less than 5% agglomerated groups of microcapsules, based on the total number of groups of microcapsules, wherein an agglomerated group of microcapsules comprises more than five microcapsules grouped together.

Claims

1. A process of manufacturing a structured isotropic aqueous detergent liquid, incorporating microcapsules, the detergent liquid comprising: i) total surfactant in the range 3 weight % to 70 weight %, and wherein the total surfactant comprises at least 5 weight % anionic surfactant; and ii) at least 0.05% activated citrus fibre external structurant; iii) at least 0.001 weight % microcapsules; the process comprising a step of combining two premixes A and B; wherein: a) Premix A comprises an aqueous dispersion of microcapsules; and b) Premix B comprises the structured aqueous concentrated liquid detergent formulation in the absence of microcapsules, characterised in that: Premix A comprises: a slurry of microcapsules diluted with at least at an equal weight of water; and wherein at least 90 weight % of the microcapsules comprise a particle size in the range 1 to 100 microns, preferably from 5 to 30 microns; and wherein Premix A is agitated with stirring to disperse the microcapsules prior to the addition of Premix A to Premix B; and wherein: the structured isotropic aqueous liquid detergent comprises less than 5% agglomerated groups of microcapsules, based on the total number of groups of microcapsules, wherein an agglomerated group of microcapsules comprises more than five microcapsules grouped together.

2. A process according to claim 1 wherein the water comprises demineralised water.

3. A process according to claim 1 wherein the microcapsules are charged.

4. A process according to any of the preceding claims wherein the aqueous dispersion of microcapsules in water are added to the structured aqueous concentrated liquid detergent before the addition of all other components of the liquid detergent.

5. A process according to any of the preceding claims wherein the aqueous dispersion of microcapsules in water are added to the structured aqueous concentrated liquid detergent after addition of all other components of the liquid detergent.

6. A process according to claim 5 wherein the aqueous dispersion of microcapsules comprises a 1:1 ratio by weight of microcapsule slurry to water.

7. A process according to claim 5 wherein the aqueous dispersion of microcapsules comprises a 1:3 ratio of microcapsule slurry to water.

8. A process according to any of claims 1 to 7 wherein Premix B is milled with an energy input of from 1.2 to 5.0 KJ/kg prior to mixing with Premix A to form the structured aqueous concentrated liquid detergent.

9. A process according to any of claims 1 to 7 wherein Premix A is combined with Premix B and the two Premixes milled with an energy input of from 1.2 to 5.0 KJ/kg to form the structured aqueous concentrated liquid detergent.

10. A process according to any of claims 1 to 9 wherein the microcapsules comprise an anionic charge.

11. A process according to any of claims 1 to 9 wherein the microcapsules comprise a cationic charge.

12. A process according to any of claims 1 to 9 in which the microcapsules comprise a shell comprising a material selected from the group consisting of: (poly)urea, (poly)urethane, polysaccharide, starch, aminoplasts or a melamine formaldehyde shell.

13. A process according to any of the preceding claims wherein the microcapsules further comprise a deposition aid.

14. A process according to any of claims 1 to 13 wherein the total surfactant is in the range 10 to 40 weight %, most preferably the total surfactant is in the range 20 to 30 weight %.

15. A process according to any preceding claim in which the microcapsules are perfume encapsulates.

Description

EXAMPLES

[0155] The invention will now be further described with reference to the following non-limiting examples and accompanying drawings in which:

[0156] FIG. 1is a photograph of a detergent liquid formulation from experiment 1B viewed through a microscope in which microcapsules have been added to the formulation as a concentrated slurry at the end of the formulation process that is, after the milling stage and illustrates agglomeration of the microcapsules.

[0157] FIG. 2is a photograph of a detergent liquid formulation from experiment 10 viewed through a microscope in which a dispersion of microcapsules has been formed and added to the formulation at the end of the formulation process, after the milling step and illustrates no agglomeration of the microcapsules.

[0158] FIG. 3is a photograph of a detergent liquid formulation from experiment 1A viewed through a microscope in which a dispersion of microcapsules has been formed in batch water and added to the formulation at the start of the formulation process and illustrates no agglomeration of the microcapsules.

[0159] FIG. 4is a photograph of a detergent liquid formulation from experiment 2A comprising Type 2 (Dual) encapsulates and illustrates no agglomeration of the microcapsules when added at the start of the formulation process with batch water.

[0160] FIG. 5a photograph of a detergent liquid formulation from experiment 2B comprising Type 2 (Dual) encapsulates and illustrates agglomeration of the microcapsules when added neat to the formulation after the milling stage.

[0161] FIG. 6a photograph of a detergent liquid formulation from experiment 2C comprising Type 2 (Dual) encapsulates and illustrates minimal agglomeration when the microcapsules are pre-dispersed in 50:50 mixture of slurry:water.

[0162] FIG. 7is a photograph of a detergent liquid formulation from experiment 3A comprising cationic encapsulates and illustrates no agglomeration of the microcapsules when same are added up-front with batch water.

[0163] FIG. 8is a photograph of a detergent liquid formulation from experiment 3B comprising cationic encapsulates and illustrates no agglomeration of the microcapsules when added as a 50:50 pre-dispersion with water and when added at the end of the formulation process.

[0164] FIG. 9is a photograph of a detergent liquid formulation from experiment 4A comprising HPC encapsulates and illustrates no agglomeration of the HPC microcapsules when added upfront at the start of the formulation process with batch water.

[0165] FIG. 10is a photograph of a detergent liquid formulation from experiment 4B comprising HPC encapsulates and illustrates no agglomeration of the HPC microcapsules when pre-dispersed in 50:50 slurry:water mixture and post-dosed into the formulation.

[0166] FIG. 11is a photograph of a detergent liquid formulation from experiment 5A comprising non-coated encapsulates and illustrates no agglomeration of microcapsules when added up-front in batch water.

[0167] FIG. 12is a photograph of a detergent liquid formulation from experiment 5B comprising non-coated encapsulates and illustrates agglomeration of the microcapsules when pre-dispersed in 50:50 slurry:water mixture.

[0168] FIG. 13is a photograph of a detergent liquid formulation from experiment 5C comprising non-coated encapsulates and illustrates no agglomeration of the microcapsules when pre-dispersed in a 1:3 slurry:water mixture and then post-dosed into the formulation.

ABBREVIATIONS

[0169] The following abbreviated names used in the examples have the following meanings: [0170] ACF is high pressure homogenizer (HPH) activated citrus fibre (2 weight % premix). [0171] Water is Demineralised water. [0172] Glycerol is hydrotrope. [0173] MPG is Monopropylene Glycol (hydrotrope). [0174] Neodol NI is a nonionic surfactant (NI) ex Shell [0175] NaOH is 50% sodium hydroxide base. [0176] LAS acid is linear alkyl benzene sulphonic acid anionic surfactant. [0177] MEA is Monoethanolamine base [0178] TEA is Triethanolamine base [0179] Prifac 5908 is saturated fatty acid (soap) ex Croda [0180] SLES (3EO) is SLES 3EO anionic surfactant. [0181] Dequest 2066 is Diethylenetriamine penta(methylene phosphonic acid (or Heptasodium DTPMP) sequestrant ex Thermphos. [0182] Dequest 2010 is HEDP (1-Hydroxyethylidene-1,1,-diphosphonic acid) sequestrant ex Thermphos [0183] EPEI is ethoxylated polyethyleneimine PE1600E020 Sokalan HP20 ex BASF [0184] HPH High pressure homogenizer [0185] Neolone MIT 950 is antimicrobial preservative, methylisothiazolin-3-one in water ex Dow chemical [0186] Perfume encaps is encapsulated perfume, for example, Oasis Cap Det B72 ex Givaudan. [0187] Polynesie is a fragrance oil [0188] Preservative is Proxel GXL antimicrobial preservative, 20% solution of 1,2 benzisothiazolin-3-one in dipropylene glycol and water ex Arch Chemicals. [0189] Perfume is free oil perfume [0190] Laponite EL is water swellable synthetic hectorite clay ex Rockwood [0191] Laponite RD is water swellable synthetic hectorite clay ex Rockwood [0192] Micro is ISP white microbeads (visual cues). [0193] Viscolam CK57 is a cross-linked thickening polymer ex Lamberti [0194] Tinopal 5BMGX is a fluorescer ex BASF [0195] Kleen is an encapsulated fragrance [0196] Xpect1000L is pectate lyase ex Novozymes [0197] Protease is Relase Ultra 16L EX ex Novozymes [0198] L blend is a blend of 3 parts Stainzyme (amylase) to 1 part Mannaway (mannanase) ex Novozymes [0199] Savinase is Ultra 16Lan enzyme Ex Novozymes [0200] Liquitint a dye [0201] NI non-ionic

[0202] Experimental

[0203] Five experiments were performed to investigate how different types of microcapsules in the form of encapsulated perfumes (or encaps) behave in a liquid detergent formulation depending on the order of addition of the encapsulated perfumes with respect to other reagents.

[0204] The experiments involved two different formulations and five different types of encapsulated perfumes. The encapsulated perfumes were added at two different times during the preparation of the detergent formulation, namely, at the start of the formulation process that is, up-front addition of the microcapsules, or at the end of the formulation process, referred to as post-dosed addition of the microcapsules. In addition, the microcapsules were added as a concentrated slurry or as a pre-dispersed solution as described in premix A.

[0205] The five different experiments were therefore: [0206] Experiment 1: Formulation 1 with encapsulated perfume of type 1. [0207] Experiment 2: Formulation 1 with encapsulated perfume of type 2. [0208] Experiment 3: Formulation 2 with encapsulated perfume of type 3. [0209] Experiment 4: Formulation 2 with encapsulated perfume of type 4. [0210] Experiment 5: Formulation 2 with encapsulated perfume of type 5.

Form of the Five Different Microcapsules Used in Experiments 1 to 5:

[0211] 1. Encapsulated perfume of type 1a slurry of an uncharged/non-ionic melamine formaldehyde resin polymer shell incorporated with a xyloglucan (XG) (non-ionic polysaccharide) deposition aid. [0212] 2. Encapsulated perfume of type 2a slurry comprising Type 2 dual encaps, that is, a mixture of 2 different encapsulated microcapsules, a first encap, Encap A comprising a melamine formaldehyde resin polymer shell which has incorporated within, an xyloglucan (XG) (a non-ionic polysaccharide) deposition aid; and Encap B comprising a melamine formaldehyde resin polymer shell, modified to be porous or leaky in a wash, with no deposition aid. [0213] 3. Encapsulated perfume of type 3an encapsulated microcapsule slurry comprising a melamine formaldehyde resin polymer shell which has incorporated within, a cationic guar gum deposition aid, ex Firmenich. [0214] 4. Encapsulated perfume of type 4an encapsulated microcapsule slurry comprising a melamine formaldehyde resin polymer shell which has incorporated within, Hydroxy propyl cellulose (HPC), a non-ionic polysaccharide substantive to cellulose and polyester.

[0215] 5. Encapsulated perfume of type 5an encapsulated microcapsule slurry comprising a melamine formaldehyde resin polymer shell which does not have any deposition aids grafted into the shell (classed as a bare or non-coated encap).

Premix APreparation of Dispersed Microcapsules (Encapsulated Perfumes).

[0216] The microcapsules used in the experiments encapsulate a fragrance and comprise a melamine formaldehyde shell, with either an outer cationic charge or an outer anionic charge. The microcapsules are supplied as a concentrated slurry in water. In accordance with the present invention the microcapsules were further diluted with an equivalent or greater weight of water and agitated with stirring for 5 minutes to form a diluted or pre-dispersed slurry (where a 50:50 dilution was not sufficient to disperse the microcapsule encap, a premix of 1:3 slurry:water was used). The slurry of microcapsules was either diluted with demineralised water or with demineralised water and batch water supplied with other components to achieve the required final weight of water in the formulation.

[0217] Premix BPreparation of Activated Citrus Fibre

[0218] An activated 2 Kg citrus fibre premix was prepared which involved the preparation of a citrus powder/water premix comprising citrus fibre powder (Herbacel AQ plus N Citrus Fibre (ex: Herbafoods)), for example 2 weight %, as the external structurant as set out in Table 1.

TABLE-US-00001 TABLE 1 Material % As supplied Weight (g) De-mineralised water 97.92 1958.4 Proxel GXL 0.08 1.6 Herbacel AQ + type N 2 40

[0219] The citrus pulp was added slowly to a mixture of de-mineralised water and preservative, Proxel GXL and the reactants stirred with agitator with overhead drive operated at 200 rpm for 15 minutes ensuring that clumping did not occur. This allowed the fibres to hydrate sufficiently prior to activation. The citrus pulp powder/water premix was then processed using a high pressure homogenizer (HPH) (200) to activate the citrus pulp fibres. That is, the solubilised citrus pulp powder was homogenized at around 500 barg and at a flow rate of 11 kg/hour using an APV2000 laboratory high pressure homogenizer available from SPX.

Preparation of Generic Formulation Mixture.

[0220] Separately, a formulation was prepared in which clay for example 0.1 weight % was mixed together with de-mineralised water as required with stirring at 300 rpm for 15 minutes. The stirring rate of the clay formulation was then reduced to 250 rpm before adding activated citrus pulp premix. The citrus pulp and clay mixtures were then mixed together for 5 minutes.

[0221] As appropriate, sufficiently fresh activated citrus fibre/clay premix was added to the mixer to provide the required level of activated citrus fibre in the finished detergent formulation prior to milling.

[0222] Demineralised water (as defined in Table 2), clay and citrus pulp (premix B), were combined with stirring, the stirring rate of the citrus fibre and clay premix was set to 200 rpm and the remaining formulation components as defined in Table 2 were added except for encapsulated fragrance microcapsules (Premix A).

[0223] In experiments where the encapsulated fragrance microcapsules (encaps) were added up-front, that is, at the start of the preparation of the detergent formulation mixture, the microcapsules were added in concentrated slurry format directly to the formulation batch before addition of the citrus pulp and clay. The formulation (which may or may not include encapsulated fragrance microcapsules, depending on the experimental encap order of addition) was then mixed for 15 to 20 minutes. The formulation was then passed through an in-line high shear rotar stator mixer operating at between 1.2 and 5.0 kJ/Kg energy. A specific energy of between 1.2 and 5.0 kJ/Kg provides a suitable operating window for consistent structurant dispersal of the detergent components.

[0224] The components in the detergent formulation were added in the order set out in Table 2 in which as 100% defines the amount of reagent required in final the formulation based on 100% reagent supplied.

TABLE-US-00002 TABLE 2 AS 100% WEIGHT REAGENT ACTIVE (g) Demineralised (batch) water** 58.451 490.18 Non-clay microcapsules in the form of 0.300 3.00 encapsulated fragrance 2% Citrus Pulp 0.100 50.00 Laponite Clay powder 0.200 2.00 Fluorescer (brightening agent) 0.080 1.18 Tinopal 5BM-GX MPG (hydrotrope) 2.000 20.00 Glycerol(hydrotrope) 5.000 50.00 NaOH (neutralizer) 1.200 25.53 TEA (neutralizer, buffer, hydrotrope) 1.690 17.07 Neodol 25_79 (non-ionic surfactant) 13.720 137.20 LAS acid (anionic surfactant) 9.150 94.23 Prifac 5908/Palmera B1231(fatty acid) 1.500 15.00 SLES 3EO (anionic surfactant) 4.570 65.29 Dequest 2066 (sequestrant) 0.340 10.63 Proxel GXL (preservative) 0.02 1.00 Neolone MIT 950(preservative) 0.0095 1.00 Perfume fragrance 0.92 9.20 Enzymes 0.75 7.50 Total 100% 5000.00 **Amount includes water derived from reagents in the formulation.

[0225] Experiment 1

[0226] Formulation (1) (as a 30% active formulation)a first formulation was prepared comprising the components in Table 2 above using an encapsulated fragrance of type 1. The type 1 encapsulated fragrance comprised a melamine formaldehyde shell with a Xyloglucan outer coating deposition aid. The type 1 encapsulated fragrance was added to the detergent formulation as follows:

[0227] Experiment 1A: encapsulated fragrance added upfront to the demineralised (batch) water;

[0228] Experiment 1B: encapsulated fragrance post-dosed at the end of the preparation after milling of the detergent formulation as a concentrated slurry; or

[0229] Experiment 1C: encapsulated fragrance post-dosed at the end of the preparation of the detergent formulation after milling as a pre-dispersed 50:50 premix (A) in demineralised/batch water.

[0230] The resulting formulations were then observed under a microscope in order to investigate and assess the agglomeration of the encapsulated fragrance (encaps).

[0231] The results from experiments 1A, 1B and 10 demonstrated that for encapsulated fragrance with a xyloglucan outer coating deposition aid, if added in a concentrated format after the formulation has been milled, the encapsulated fragrance agglomerated, as depicted in FIG. 1. However, addition of the encapsulated fragrance in either the demineralised (batch) water (Experiment 1A, FIG. 3), or pre-dispersed and post-dosed at the end of the preparation of the detergent formulation after milling (Experiment 10, FIG. 2), did not lead to agglomeration of the encapsulated fragrance microcapsules.

[0232] Therefore, Experiments 1A, 1B and 10 demonstrate that pre-dispersal of the encapsulated fragrance in water enables the encapsulated fragrance to be added at the start or the end of the batch process.

[0233] Experiment 2

[0234] For Experiment 2, Experiment 1 was repeated using the formulation detailed in Table 2.

[0235] The encapsulated fragrance was replaced however with an alternative encapsulated fragrance namely, an encapsulated perfume slurry comprising Type 2 dual encaps, that is, a mixture of 2 different encapsulated microcapsules, a first encap, Encap A comprising a melamine formaldehyde resin polymer shell which has incorporated within, a xyloglucan (XG) (a non-ionic polysaccharide) deposition aid; and Encap B comprising a melamine formaldehyde resin polymer shell, modified to be porous or leaky in a wash, with no deposition aid.

[0236] The Type 2 encapsulated fragrance was added to the detergent formulation as follows:

[0237] Experiment 2A: encapsulated fragrance added up-front in demineralised (batch) water;

[0238] Experiment 2B: encapsulated fragrance post-dosed at the end of the preparation of the detergent formulation as a concentrated slurry; or

[0239] Experiment 2C: encapsulated fragrance post-dosed at the end of the preparation of the detergent formulation as a pre-dispersed 50:50 premix (A) in demineralised (batch) water.

[0240] The resulting formulations were then observed under a microscope in order to investigate and assess the agglomeration of the encapsulated fragrance (encaps).

[0241] The results from experiments 2A, 2B and 2C again demonstrated that for the Type 2 encapsulated fragrance with and without a xyloglucan outer coating deposition aid, if added in a concentrated format after the formulation has been milled, the encapsulated fragrance agglomerates, as depicted in FIG. 5 (Experiment 2B). However, addition of the encapsulated fragrance in either the demineralised (batch) water (Experiment 2A, FIG. 4), or pre-dispersed in water and post dosed at the end of the preparation of the detergent formulation after milling (Experiment 2C, FIG. 6), does not lead to unacceptable levels of agglomeration of the encapsulated fragrance microcapsules. Therefore, Experiments 2A, 2B and 2C also demonstrate that pre-dispersal of encapsulated fragrance in water enables the encapsulated fragrance to be added at the start or the end of the formulation process.

[0242] Experiment 3

[0243] For experiments 3 to 6 a second formulation, Formulation (2), (as a 23% active formulation) was prepared comprising the components in Table 3 below but using three different encapsulated fragrances described as types 3 to 5 respectively.

TABLE-US-00003 TABLE 3 Example of 1 Kg batch of Formulation 2 WEIGHT REAGENT AS 100% ACTIVE (g) Demineralised (batch) water 58.4 480 Non-clay microcapsules in the form of 0.4 13.7 encapsulated fragrance, type 3, 4 or 5 2% Citrus Pulp 0.1 50 Laponite Clay powder 0.2 2 Fluorescer (brightening agent) 0.08 1.18 Tinopal 5BM-GX MPG (hydrotrope) 2 20 Glycerol(hydrotrope) 5 50 NaOH (neutralizer) 1.2 25.5 TEA (neutralizer, buffer, hydrotrope) 1.69 17.1 Neodol 25_79 (non-ionic surfactant) 13.72 137.2 LAS acid (anionic surfactant) 9.15 94.2 Prifac 5908/ 1.5 15 Palmera B1231 (fatty acid) SLES 3EO (anionic surfactant) 4.57 65.3 Dequest 2066 (sequestrant) 0.34 10.63 Proxel GXL (preservative) 0.02 1.0 Neolone MIT 950 (preservative) 0.0095 1.0 Perfume fragrance 0.86 8.6 Enzymes 0.75 7.5 Total 100 1000

[0244] For experiment 3, a type 3 encapsulated microcapsule slurry fragrance was used which comprised a melamine formaldehyde resin polymer shell which had incorporated within, a cationic guar gum deposition aid, ex Firmenich.

[0245] The type 3 encapsulated fragrance was added to the detergent formulation as follows:

[0246] Experiment 3A: encapsulated fragrance added up-front in demineralised (batch) water;

[0247] Experiment 3B: encapsulated fragrance post-dosed at the end of the preparation of the detergent formulation as a pre-dispersed 50:50 premix (A) in demineralised (batch) water.

[0248] The resulting formulations were then observed under a microscope in order to investigate and assess the agglomeration of the encapsulated fragrance (encaps).

[0249] The results from experiments 3A and 3B demonstrated that for a cationic coated encapsulated fragrance addition of the encaps either to the demineralised (batch) water (Experiment 3A, FIG. 7), or pre-dispersed and post-dosed at the end of the preparation of the detergent formulation after milling (Experiment 3B, FIG. 8), does not lead to agglomeration of the encapsulated fragrance microcapsules.

[0250] Therefore, Experiments 3A and 3B also demonstrate that pre-dispersal of the encapsulated fragrance in water enables the encapsulated fragrance to be added at the start or the end of the formulation process.

[0251] Experiment 4

[0252] For Experiment 4, Experiment 3 was repeated using the formulation detailed in Table 3 except that the encapsulated fragrance was replaced with type 4 encapsulated fragrance microcapsule slurry comprising a melamine formaldehyde resin polymer shell which had incorporated within, hydroxypropyl cellulose (HPC), a non-ionic polysaccharide deposition aid or coating substantive to cellulose and polyester.

[0253] The type 4 encapsulated fragrance microcapsules were added to the detergent formulation as follows:

[0254] Experiment 4A: encapsulated fragrance added up-front in demineralised (batch) water;

[0255] Experiment 4B: encapsulated fragrance post-dosed as a 50:50 premix A.

[0256] The resulting formulations were then observed under a microscope in order to investigate and assess the agglomeration of the encapsulated fragrance (encaps), Experiment 4A, FIG. 9 and Experiment 4B, FIG. 10 respectively.

[0257] The results from experiments 4A, and 4B demonstrated that for the type 4 encapsulated fragrance with a HPC (hydroxylpropyl cellulose) deposition aid or coating, this encapsulated fragrance did not lead to agglomeration of the encapsulated fragrance microcapsules either when added with the demineralised (batch) water or when post-dosed as a 50:50 premix A.

[0258] Experiment 5

[0259] For Experiment 5, Experiment 3 was repeated using the formulation detailed in Table 3 using an alternative type 5 encapsulated fragrance microcapsule slurry comprising a melamine formaldehyde resin polymer shell without any deposition aids grafted into the shell (classed as a bare or non-coated encapsulate).

[0260] The type 5 encapsulated fragrance was added to the detergent formulation as follows:

[0261] Experiment 5A: encapsulated fragrance added up-front in demineralised (batch) water;

[0262] Experiment 5B: encapsulated fragrance post-dosed as a 50:50 premix A.

[0263] Experiment 5C: encapsulated fragrance post-dosed as a pre-dispersed 1:3 slurry:water ratio premix.

[0264] The resulting formulations were then observed under a microscope in order to investigate and assess the agglomeration of the encapsulated fragrance (encaps), Experiment 5A FIG. 11, Experiment 5B, FIG. 12 and Experiment 5C, FIG. 13 respectively.

[0265] The results from experiments 5A, and 5B demonstrated that for the type 5 encapsulated fragrance with no deposition aid or coating, this encapsulated fragrance does not lead to agglomeration of the encapsulated fragrance microcapsules either when added with the demineralised (batch) water or when post dosed as a pre-dispersed 1:3 slurry:water ratio premix after milling.

[0266] Therefore, in summary, the results of the five groups of experiments show that that if microcapsules with encapsulated perfumes are dispersed either in aqueous media such as for example, demineralised (batch) water, or alternatively, in a ratio of least 1:3 encapsulated microcapsule to aqueous solution, the encapsulated perfume may be added up-front with formulation demineralised (batch) water or post-dosed to the formulation, without agglomeration of the microcapsules. That is, it is possible to avoid the agglomeration of microcapsules normally observed on post-addition of a concentrated slurry of microcapsules.

[0267] Microscope Images and Analysis

[0268] As indicated above photographs were taken of each liquid detergent formulation prepared with microcapsules treated and added to the liquid detergent at different points in the preparation of the formulation.

[0269] The photographic images seen in FIGS. 1 to 13 were acquired using a BX51 Olympus microscope fitted with a Marzhauser motorised stage, fitted with a Zeiss HRc

[0270] Axiocam camera controlled by Zeiss Axiovision software.

[0271] For each detergent liquid formulation, a sample of the detergent was isolated and contained within a cavity slide which in turn was sealed with a coverslip. The images of the liquid detergent formulations were recorded in transmission DIC mode at times twenty 20 magnification producing images with a lateral resolution of 0.65 um and a field of view of 446335 um.

[0272] Summary of Results

TABLE-US-00004 TABLE 4 Exper- Encap iment Order of Observation Figure Number Description addition after Milling Number 1A Neat XG encaps Upfront No agglomeration 3 2A Neat Dual encaps Upfront No agglomeration 4 3A Neat Cationic Upfront No agglomeration 7 encaps 4A Neat HPC encaps Upfront No agglomeration 9 5A Neat Non coated Upfront No agglomeration 11 encaps 1B Neat XG encaps Post dosed Agglomeration 1 1C Pre-dispersed Post dosed No agglomeration 2 (50:50) XG encaps 2B Neat Dual encaps Post dosed Agglomeration 5 2C Pre-dispersed Post dosed No agglomeration 6 (50:50) Dual encaps 3B Pre-dispersed Post dosed No agglomeration 8 (50:50) Cationic encaps 4B Pre-dispersed Post dosed No agglomeration 10 (50:50) HPC encaps 5B Pre-dispersed Post dosed Agglomeration 12 (50:50) Non-coated encaps 5C Pre-dispersed (1:3) Post dosed No agglomeration 13 Non-coated encaps

[0273] Therefore it may be seen in Table 4 above that agglomeration of microcapsules (such as perfume containing microcapsules) occurs when concentrated microcapsules are added as a final reagent in the preparation of a liquid detergent.

[0274] The present inventors have therefore found that agglomeration of microcapsules may be overcome by pre-dispersion of the microcapsules in water prior to addition of the microcapsules to the liquid detergent formulation. The microcapsules may be dispersed in for example, de-mineralized water or alternatively in demineralised water and/or batch water used to formulate the detergent.

[0275] However, of interest is the fact that once the microcapsules have been pre-dispersed, it is possible to add the microcapsules at different stages in the preparation of the detergent formulation without encountering agglomeration. In contrast however, if the microcapsules are not pre-dispersed prior to addition to the formulation and the microcapsules are instead added in undiluted concentrated form, agglomeration occurs.

[0276] The ability to add microcapsules at different points during the formulation of the detergent liquid provides increased flexibility of the formulation process. In addition, the lack of agglomeration avoids the need for increased agitation of the formulation to ensure dispersion of the microcapsules, which in turns decreases the likelihood that the integrity of the microcapsules will be compromised.

[0277] Furthermore, lack of agglomeration of the microcapsules ensures efficient delivery of the microcapsules to fabrics treated with a detergent formulation comprising same following a wash cycle and hence maximized delivery of the contents of the microcapsules, such as for example fragrances.

[0278] Therefore in accordance with the present invention it has been observed that it is possible to prepare an externally structured aqueous isotropic liquid laundry detergent formulation in which fragrance encapsulated in microcapsules may be efficiently dispersed throughout the detergent formulation without leading to agglomeration of the microcapsules and without compromising the end delivery of the fragrance held within the microcapsules.