ES2457495T3 - Incorporation of microcapsules to structured liquid detergents - Google Patents

Abstract

A process for incorporating microcapsules with an anionic charge into a structured aqueous concentrated liquid detergent comprising at least 30% by weight, preferably at most 65% by weight, of total surfactant, of which at least 5% by weight, based on the total composition, is an anionic surfactant, including soap, and an external structuring, the process comprising combining the two premixes; premix A which is the structured aqueous concentrated liquid detergent composition without microcapsules and premix B, comprising an aqueous dispersion of the microcapsules with an anionic charge, characterized in that premix B is a dense suspension of microcapsules with a maximum viscosity at 25 ° C of 100 mPa.s and at least 90% by weight of the microcapsules have a particle size in the range of 5 to 30 μm, and because premix B is added to premix A and the resulting combined mixture is passed through a static line mixer with an energy input of 20 to 500 J / kg forming, immediately after the mixer, a structured liquid comprising less than 10%, based on the total number of microcapsule groups, agglomerated groups of microcapsules, an agglomerated group of microcapsules being defined as a group having more than 5 microcapsules grouped together

Description

Incorporation of microcapsules to structured liquid detergents

5 Technical field

The present invention relates to an improved process for incorporating microcapsules into a structured aqueous liquid detergent composition comprising at least 30% by weight of total surfactant.

10 Background

It is desirable to use microcapsules in liquid detergents. Microcapsules that have a cover that protects the internal core contents may provide a delayed release of their contents and / or provide a stable formulation when their contents otherwise interact with the crude liquid. Said microcapsules 15 are well known in the field of detergents, and have been proposed for inclusion in aqueous liquid detergent compositions. The microcapsules are small enough to be usable in large numbers and are generally not visible to the naked eye when they are introduced into the liquid. However, they can cause the liquid to become cloudy. Some microcapsules may be suspended in an unmodified liquid. Others, with an apparent density less closely matching, may require modification of the liquid by

20 thickening or structuring system to avoid the formation of cream or sedimentation. Typical of said microcapsules are perfume encapsulates with melamine-formaldehyde covers as described in US-A-5,066,419. The microcapsules may alternatively contain other liquid laundry treatment additives such as tinting dyes, lubricants, etc. The contents of the microcapsules are not important for the present invention.

When said microcapsules are added to concentrated surfactant solutions, especially those comprising an external structurant such as hydrogenated castor oil or microfibrous cellulose, the microcapsules have been found to experience clumping in lumps during the incorporation stage. These agglomerates remain dispersed in the liquid. This increases the visibility of the microcapsules. Cause

30 also an irregular dosage of its contents by washing, as the liquid is removed from the container. Finally, if the agglomerated microcapsules survive to the point of deposition on clothing, then the contents of the microcapsules are overdosed at that point and distributed irregularly across the surface of the clothing. This could cause unwanted effects such as damage to clothing or the need to use more microcapsules than would otherwise be necessary. Therefore, it is highly desirable to avoid a substantial agglomeration of

35 microcapsules in an aqueous liquid detergent.

Concentrate means a total surfactant content (including soap) of 30% by weight or more.

WO 09135765 A discloses a process for the manufacture of a liquid detergent composition

Structured comprising a beneficial agent in dispersed phase which may be a perfume microcapsule, a microfibrous cellulose structurant, at least 5% by weight of anionic surfactant and 25 to 55% by weight of surfactant, the process comprising the steps of (i) preparation of a microfibrous cellulose premix using high shear mixing, (ii) separate preparation of a mixture of aqueous surfactant, combination of microfibrous cellulose premix and surfactant mixture using high shear and

Perfume microcapsules can then be dosed into the resulting structured structured surfactant structured liquid. The high shear mixing stage is achieved using an in-line mixing process, such as by contacting two process streams directly before an in-line mixer. The microcapsule particle sizes are in the range of 5 to 50 μm, preferably 10 to 30 μm.

Example 4 of WO 09135765 A discloses details of the addition of perfume microcapsules. 1.5% by weight of perfume encapsulates were added to an MFC structured liquid with a surfactant level of 40 to 50% by weight. The addition was made for 30 s, using a Heidolph stirrer, and mixing was continued for 5 min (if necessary). A Heidolph laboratory mixer is an air-powered impeller or vane stirrer. It is not a static online mixer. There is no disclosure about the quality of the

55 liquid detergent product prepared in this way. It has now been found that certain perfume microcapsules tend to suffer agglomeration problems when added in this way.

In US 2005026800 A, microcapsules are stirred in a washing liquid detergent prepared by combining an aqueous premix of high power liquid detergent composition (HDL) and a premix

60 structuring. The HDL premix is prepared by combining HDL components with water in a suitable container with adequate agitation and the structuring agent premix is prepared by combining hydrogenated castor oil and other structuring agent premix ingredients. The microcapsules are then added slowly to the structured liquid while maintaining gentle agitation, paragraph 88.

65 Another prior art does not give details of how the microcapsules are added or says that they are added by stirring.

It is known from US 2005026800 A and other publications that hydrogenated castor oil (HCO) can be used as an external structuring and rheology modifier to stabilize said concentrated liquid detergents.

In WO 2010/034736, the incorporation of perfume microcapsules into a concentrated liquid detergent, structured using hydrogenated castor oil, is described. The microcapsules are added as a dense suspension of encapsulated perfume and mixed using a paddle mixer. The formulations were assessed visually with the naked eye and by microscopy, to identify if there was phase separation or if the encapsulates were still monodispersed. The compositions exhibited no loss or change of structure or dispersion of the encapsulation after being tested for 12 weeks at 5 ° C, 12 weeks at 37 ° C and 4 weeks at 50 ° C. It has now been found that although there is no subsequent agglomeration of the microcapsules, the initial dispersion by the paddle mixer gives an unacceptably high amount of substantially agglomerated perfume encapsulates. These agglomerates do not seem to be redispersed. The presence of said agglomerated material is undesirable for the reasons explained above.

It is an object of the present invention to provide an improved process for the production of externally concentrated structured liquid detergents, said liquid detergents being capable of suspending microcapsules, for example encapsulated fragrances, which are not visible to the naked eye.

Summary of the invention

According to the present invention, a process is provided for the incorporation of microcapsules with an anionic charge into a structured aqueous concentrated liquid detergent comprising at least 30% by weight, preferably at most 65% by weight, of total surfactant, of which at least one 5% by weight, based on the composition

In total, it is an anionic surfactant including soap and an external structurant, the process comprising the combination of two premixes: premix A which is the structured aqueous concentrated liquid detergent composition without microcapsules, and premix B comprising an aqueous dispersion of the microcapsules with anionic charge, characterized in that:

premix B is a dense suspension of microcapsules with a maximum viscosity at 25 ° C of 100 mPas having at least 90% by weight of the microcapsules a particle size in the range of 5 to 30 μm, and because

premix B is added to premix A and the resulting combined mixture is passed through a mixer in

35 static line with an energy input of 20 to 500 J / kg forming, immediately after the mixer, a structured liquid comprising less than 10%, based on the total number of microcapsule groups, agglomerated groups of microcapsules, being defined an agglomerated group of microcapsules as a group that has more than 5 microcapsules grouped together.

Preferably, the maximum viscosity of premix B is 50 mPas, more preferably 20 mPas, even more preferably 15 mPas.

Agglomerate means that more than 5 microcapsules are grouped together. This is determined, for example, by taking a photomicrograph of the liquid and counting the number of microcapsule groups present in

It forms groups of 1, 2, 3, 4 or 5 microcapsules and also counting the number of microcapsules present in the form of agglomerates of more than 5 microcapsules, which is defined as agglomerated microcapsules. If more than 10% of the groups are in the form of said agglomerated microcapsules, then the microcapsules are too agglomerated to be within the scope of this invention.

To obtain the low viscosity of premix B, it may be necessary to reduce the viscosity of the microcapsule concentrate in dense suspension of the raw material. This can be done, for example, by dilution with water if necessary.

The dense suspension of microcapsules can be added to the main liquid by in-line injection or pouring into the

55 bowl with mixed. The mixture is then passed through a static in-line mixer that applies enough energy to break up the agglomerates, preventing the breakdown of the individual microcapsules and retaining the liquid structure. Surprisingly, the resulting structured liquid is highly effective in preventing subsequent agglomeration of the microcapsules over time.

The external structurant is preferably hydrogenated castor oil (castor wax or trihydroxystearin). The external structuring agent may alternatively be another fibrous agent, such as microfibrous cellulose or any other type of external structuring agent.

The microcapsules comprise a solid shell. It has been found that the problem of agglomeration seems

65 be limited to microcapsules that carry an anionic charge. Microcapsules with a cationic charge can be added to concentrated liquids without agglomerate formation and therefore without the need for the process of the present invention. Of course, it is still possible to pass a mixture comprising cationic microcapsules through a static in-line mixer to disperse the microcapsules, if desired.

Most preferably, the microcapsule has a melamine-formaldehyde shell. Other suitable cover materials 5 may be selected from polyurea, polyurethane, starch / polysaccharide and aminoplasts.

The microcapsules can be encapsulated in perfume. It has been found that the inclusion of microcapsules of smaller diameter worsens the agglomeration problem.

It is advantageous to have a very narrow particle size distribution, for example 90% by weight of the microcapsules in the range of 8 to 11 μm. This minimizes the amount of potentially high surface area material that can act as an adhesive and jointly bond larger particles.

Microcapsules in the range of 2 to 5 μm cannot be dispersed as efficiently using the process according to

15 invention due to the high surface area of the minor particles. In contrast, microcapsules larger than 40 μm generally do not require additional processing, since the smaller total surface area is sufficient to avoid substantial agglomeration without the need for increased energy input from a static in-line mixer. However, the process can be used for larger particles, if desired.

The process is more effective for microcapsules in the range of 5 to 30 μm. The removal of microcapsules in the range of 0.1 to less than 1 μm improves the dispersion of microcapsules. It is believed that this is due to the reduction of high surface area material.

Once the microcapsules have been incorporated into the structured liquid and dispersed by the in-line mixer, the structure is very effective in preventing any agglomeration, even in the presence of high levels of surfactant.

The process can be used to make externally structured concentrated liquid compositions comprising at least 30% by weight of surfactant, including anionic surfactant (any soap being included in the calculation and being an anionic surfactant) comprising 0.1 to 2.0% by weight of microcapsules in which the ratio of microcapsules in groups of 5 or less to agglomerated microencapsules (in groups of 5 or more) is more than 9: 1.

When hydrogenated castor oil is used as an external structuring agent, it is suitably present at a level of 0.15 to 0.5% by weight of the total composition. Preferably, it has a dendritic structure in which the fibers

35 are matted and the smallest fiber dimension is a maximum of 40 nm.

Detailed description of the invention

All percentages mentioned herein are by weight calculated on the total composition unless otherwise specified.

Premix A

Although, in principle, premix A can be formed using any of the prior art processes, or

Any other suitable process, when hydrogenated castor oil is used as an external structuring agent, it is preferable to employ a process such as that described in WO 2010/034736, as also described below.

If microfibrous cellulose is used, it is preferred to employ an adaptation of the process described in WO 09135765 A.

External structuring

The preferred external structurant is hydrogenated castor oil. Alternatively, cellulose can be used.

In microfibrose, this material and its properties and use as an external structuring agent are described in the published literature, for example in WO 09135765 A (Unilever) and US 2008108541 A (C P Kelco).

Hydrogenated Castor Oil

Castor oil, also known as beaver musk, is a vegetable oil obtained from the pod of the castor plant (Ricinus communis). Castor oil is a colorless to very pale yellow liquid with a mild to zero odor or taste. It is a triglyceride in which approximately 90% of the fatty acid chains are ricinoleic acid (12-hydroxy-9-cis-octadecenoic acid). Oleic and linoleic acids are the other significant components. Controlled hydrogenation of castor oil provides fully hydrogenated castor oil, which is used in the process and products according to the present invention. At room temperature, the

Hydrogenated castor oil is a hard white wax that melts at a temperature of approximately 86-88 ° C. They are suppliers, for example, Hindustan Unilever, which supplies flakes or granules, Cognis (powder), Vertellus (flakes) or Elementis (flakes or granules), or any mixture thereof. It is a suitable hydrogenated castor oil in the present invention, for example, Thixcin® R available from Elementis.

5 Structuring process

When hydrogenated castor oil is used as an external structuring agent, the external structuring premix A can be produced using a process comprising the following steps:

a) preparation of a first premix by adding surfactants and a water base with stirring at a temperature of at least 55 ° C, preferably at a temperature of 55 to 70 ° C, more preferably 60 to 65 ° C, and most preferably at about 65 ° C, which has a pH of 7.5 to 11, preferably 8 to 10;

15 b) preparation of a second premix by adding hydrogenated castor oil to a liquid non-aqueous organic solvent at a temperature of at least 70 ° C, preferably at a temperature of 70 to 75 ° C, with stirring to dissolve castor oil hydrogenated in the liquid non-aqueous organic solvent, wherein the liquid non-aqueous organic solvent preferably comprises free fatty acid or non-ionic surfactant or mixtures thereof;

c) adding the second premix of step b) to the first premix of step a) at a temperature of at least 55 ° C with mixing, preferably at a temperature of 55 to 70 ° C, more preferably 55 to 65 ° C, most preferably from 60 to 65 ° C, at a weight ratio of b) to a) of 1:40 to 1:10, preferably from 1:30 to 1:15, more preferably at a ratio of about 1:20; with which hydrogenated castor oil remains

25 in solution;

d) cooling the mixture of step c) to a temperature less than 50 ° C, preferably less than 40 ° C, more preferably less than 30 ° C, and subsequent storage of this mixture until the hydrogenated castor oil has crystallized from the solution .

Preferably, in step a) the concentration of surfactants is 20 to 65% by weight, more preferably 25 to 60% by weight, and most preferably 25 to 45% by weight of the total mixture in this stage. In step a), the surfactants preferably comprise synthetic anionic and / or non-ionic surfactants. More preferably, the surfactants in step a) comprise the synthetic anionic linear alkylbenzene sulfonate surfactant

35 (LAS). The pH of the premix in step a) is preferably 9 to 10.

The first premix in step a) comprises surfactants and a water base, and preferably also a hydrotrope. A hydrotrope is a compound that solubilizes hydrophobic compounds in aqueous solutions. Typically, hydrotropes consist of a hydrophilic part and a hydrophobic part, however the hydrophobic part is too small to cause spontaneous self-aggregation and thus do not form micelles such as surfactants. Hydrotropes are used in detergent formulations to allow more concentrated formulations of surfactants. Suitable hydrotropes are, for example, glycerol and propylene glycol. Preferably, the first premix in step a) is a transparent liquid at the temperature prevailing in step c). The base in the premix in step a) preferably comprises an alkali metal hydroxide or triethanolamine, plus

Preferably the neutralizing agent comprises sodium hydroxide, triethanolamine or mixtures thereof. Typically, the premix in step a) is a micellar solution of the surfactants in water.

A second premix is prepared containing hydrogenated castor oil dissolved in a liquid non-aqueous organic solvent at a temperature of at least 70 ° C, preferably 70 to 75 ° C. Preferably, the solvent comprises free fatty acid or non-ionic surfactant, or a mixture thereof. More preferably, the solvent comprises a free fatty acid and, most preferably, the free fatty acid comprises saturated linear C12-C18 alkyl fatty acid. No free water is added to the solvent in the container at this stage b). Preferably, the second premix is performed under low shear conditions, more preferably only gentle mixing is applied. This has the advantage that only one low energy input is required when mixing the second premix.

55 Suitably, this second premix in step b) is a transparent liquid at the temperature prevailing in this stage b).

Preferably, the concentration of hydrogenated castor oil in the second premix is such that the concentration in the final liquid detergent composition obtainable by the process of the invention is from 0.15 to 0.5% by weight of the composition, preferably 0 , 15 to 0.35% by weight, even more preferably 0.2 to 0.35% by weight and most preferably 0.22 to 0.28% by weight of the total composition. The concentration of hydrogenated castor oil in the second premix in step b) is preferably 1.5 to 20% by weight of the premix, more preferably 1.5 to 10% by weight, even more preferably 1.7 at 5% by weight and most preferably from 3.4 to 5% by weight of the premix. Preferably, the second premix comprises only solvent and hydrogenated castor oil, wherein the solvent preferably comprises free fatty acid or non-ionic surfactant or mixtures thereof, most preferably the solvent is free fatty acid by

reasons explained below in relation to stage c).

In the process according to the invention, in step c) the second premix is added to the first premix with stirring, in which the weight ratio of the second and first premix is from 1:40 to 1:10, preferably 1: 30

5 to 1:15, and more preferably about 1:20. Most preferably, the second premix constitutes less than 6% by weight of the total formulation, most preferably about 5% by weight of the total formulation. The temperature in step c) is at least 55 ° C, preferably between 55 and 70 ° C, more preferably between 55 and 65 ° C, most preferably between 60 and 65 ° C.

When the solvent in the second premix in step b) comprises free fatty acid, the base in the first premix acts as a neutralizing agent for the fatty acid, and soap is formed by mixing the first and second premixes in step c). This soap formation leads to a complete or partial removal of the solvent by hydrogenated castor oil and it is believed that this process acts as a seed for its subsequent crystallization to dendritic structure. A similar effect can be obtained by careful selection of a non-anionic surfactant solution that has a phase change with the addition to the anionic surfactant solution, but this type of physical phase change is less preferable than the chemical phase change because neutralization of the free fatty acid solvent. In step c), the first and second premixes are combined with gentle agitation. Generally, the mixture in step c) is transparent to the temperature prevailing in step c), which is at least 55 ° C, preferably 55 to 70 ° C, indicating that suitably the second premix is completely dissolved in the first premix. Usually at this temperature, all ingredients are in solution and hydrogenated castor oil does not crystallize. By gentle mixing in step c), the solubilized hydrogenated castor oil is homogeneously mixed before starting the crystallization process. In step d), the mixture of step c) is cooled to a temperature less than 50 ° C, preferably less than 40 ° C, more preferably less than 35 ° C, even more preferably less than 30 ° C. Subsequently, this

Mix until the hydrogenated castor oil has crystallized from the solution. The specialist can determine when the hydrogenated castor oil has crystallized, since the crystallization of the hydrogenated castor oil can be observed visually as the liquid becomes cloudy. Otherwise, by conventional optical microscopy, it can be seen if hydrogenated castor oil crystals have formed. Preferably, this cooling step d) is carried out while the mixture is gently mixed under low shear conditions. In this case, low shear means that the shear is insufficient to break the emerging dendritic structure.

In a preferred method, in stage d) the mixture of stage c) is cooled to a temperature less than 50 ° C at a cooling rate of at most 1 ° C per minute. Preferably, in step d) the mixture is cooled

35 of step c) at a temperature less than 40 ° C, more preferably 30 ° C, at a cooling rate of at most 1 ° C per minute, preferably at most 0.7 ° C per minute, even more preferably at most 0, 5 ° C per minute, most preferably at most 0.4 ° C per minute. When this preferred cooling stage is applied d), the hydrogenated castor oil present in the premix begins to crystallize properly during the cooling stage, at a temperature below 55 ° C.

In another preferred procedure, in step d) the mixture of step c) is cooled to a temperature less than 40 ° C after 5 minutes, followed by storage of this mixture at a temperature less than 40 ° C for at least 5 minutes . Preferably, in step d) the mixture is cooled to step c) at a temperature less than 35 ° C after 5 minutes, more preferably after 3 minutes, followed by storage of this mixture 45 at a temperature less than 35 ºC for at least 5 minutes. More preferably, in step d) the mixture of step c) is cooled to a temperature less than 30 ° C after 5 minutes, most preferably after 3 minutes, followed by storage of this mixture at a temperature less than 30 ° C for at least 5 minutes. Even more preferably, the mixture of step c) is cooled to a temperature less than 40 ° C after 3

or even 2 minutes, followed by storage at a temperature below 40 ° C for at least 5 minutes. Most preferably, the mixture of step c) is cooled to a temperature of less than 30 ° C after 3 or even 2 minutes, followed by storage at a temperature of less than 30 ° C for at least 5 minutes. In another preferred embodiment, the mixture is stored for at least 8 minutes or, more preferably, at least 10 minutes at the prevailing temperature after the cooling step takes place. When this rapid cooling step is applied d), the hydrogenated castor oil present in the premix begins to crystallize

55 properly during storage of the mixture after rapid cooling.

An example of such a rapid cooling process is the instantaneous cooling in a plate heat exchanger, in which the mixture is cooled to less than 30 ° C in a period of approximately 1 minute. When said rapid cooling process is applied, the mixture will be kept at a temperature below 40 ° C for a period of at least 5 minutes. In this waiting period, the temperature of the mixture remains constant at less than 40 ° C and the crystallization of the hydrogenated castor oil will occur at the temperature at which the premix is maintained after rapid cooling takes place.

In this step d), an opacified non-Newtonian liquid is obtained which preferably has a profile of

65 pseudoplastic behavior to provide a coolant easily dispensed to a washing machine. The solubilized hydrogenated castor oil can be self-assembled into a dendritic structure. A dendritic structure

It is a highly branched structure of solid material that has a core with branches that extend from that core. The dendritic structure appears to be formed by a series of nucleations by cooling the mixture in step d), followed by crystal growth from these nucleation sites, leading to the formation of dendrites. The nucleation site can be described as the core of the dendrimer. Suitably, hydrogenated castor oil grows in a three-dimensional branched structure from this core throughout the formulation, leading to a three-dimensional framework. Hydrogenated castor oil, in the form of dendrimers, forms a structuring network in which the dimensions of the dendrimers are preferably micrometric in size (up to about 100 μm). The dendrimers form a highly tangled fibrous network. The branches (or fibers) of a dendrimer are typically 20 to 40 nm thick and typically extend to more than 10 µm. These branches of dendrimers are relatively long and thin and have an aspect ratio of the order of 1000: 1. In comparison, the prior art wire-type structuring system formed by crystallizing from an emulsion, as described in EP 1,502,944 and elsewhere, has an aspect ratio of up to 200: 1. The smaller size of the particles produced by the solvent process is also much smaller than that obtained by the aqueous emulsion process. According to EP 1,502,944, the smallest dimension

15 preferred for the thread type structurant is 5 to 15 μm. Even at the lower end of 1 μm mentioned in EP 1,502,944, the fibers of the prior art wire type structures are more than twice as thick as the dendrimers formed by the solvent process. The crystallization of hydrogenated castor oil causes the formulation to become translucent due to the size of the dendritic structure, which interferes with the light transmittance through the formulation. The microstructure of the dendrimers and the wire-like structures of the prior art are easily distinguished by microscopic examination as well as their rheological and suspension properties.

Water

The invention is particularly suitable for the addition of microcapsules to compositions comprising less than 40% by weight of water. This low water level hinders the dispersion of the microcapsules when coupled with the high active levels of the compositions of the invention. However, the invention is also applicable to a surfactant-rich composition with high water levels.

Surfactants

Liquid detergent compositions made using the process of the invention preferably comprise from 30 to 65% by weight, more preferably from 30 to 60% by weight, and most preferably from 35 to 45% by weight of a surfactant, preferably selected from materials. active anionic, nonionic, cationic detergents,

35 dipoles or mixtures thereof. In the context of the present invention, anionic surfactants include both soap and synthetic anionic surfactants. The minimum level of anionic surfactant is 5% by weight. In general, surfactants of the surfactant system may be chosen from the surfactants described in "Surface Active Agents" Vol. 1, of Schwartz & Perry, "Interscience" 1949, Vol. 2 of Schwartz, Perry & Berch, "Interscience" 1958, in the current edition of "McCutcheon's Emulsifiers and Detergents" published by the Manufacturing Confectioners Company or in "Tenside Taschenbuch", H. Stache, 2nd ed., Carl Hauser Verlag, 1981.

Soap (fatty acid salt) is a preferred component of the liquid detergent compositions according to the invention. Preferably, the organic non-aqueous solvent used in step b) of the process of the invention comprises a fatty acid. Preferably, the fatty acid comprises saturated linear C12-C18 alkyl fatty acids. Examples of fatty acids suitable for use of the present invention include pure fatty acids.

or hardened derived from palmitoleic, safflower, sunflower, soybean, oleic, linoleic, linolenic, ricinoleic, rapeseed oil or mixtures thereof. An example of a preferred fatty acid is hydrogenated coconut fatty acid, for example Prifac 5908 (supplied by Uniqema, Gouda, The Netherlands). Mixtures of saturated and unsaturated fatty acids may also be used herein.

It will be recognized that fatty acid will be present in the liquid (final) detergent composition primarily in the form of a soap. Suitable cations include sodium, potassium, ammonium, monoethanolammonium, diethanolammonium, triethanolammonium, tetraalkylammonium cations, for example tetramethylammonium to tetradecylammonium.

The amount of fatty acid will vary depending on the particular characteristics desired in the final liquid detergent composition. Preferably, from 0 to 30%, more preferably from 1 to 20%, most preferably from 2 to 10% by weight of fatty acid is present in the liquid detergent composition according to the invention. Mixtures of synthetic anionic and non-ionic surfactants are especially useful in the invention.

Nonionic detergent surfactants are well known in the art. They normally consist of a polyalkoxylene group or a water-soluble monoalkanolamide or dialkanolamide group in chemical combination with an organic hydrophobic group derived, for example, from alkylphenols in which the alkyl group contains from about 6 to about 12 carbon atoms, dialkylphenols with aliphatic alcohols primary, secondary or tertiary (or alkyl-terminated derivatives thereof), preferably from 8 to 20 carbon atoms, monocarboxylic acids of 10 to about 24 carbon atoms in the alkyl and polyoxypropylene group. Also common are fatty acid monoalkanolamides and dialkanolamides in which the group

alkyl of the fatty acid radical contains from 10 to about 20 carbon atoms and the alkylol group has from 1 to 3 carbon atoms. In any of the monoalkanolamide and dialkanolamide derivatives, optionally there may be a polyoxyalkylene moiety that binds the last groups and the hydrophobic part of the molecule. In all surfactants containing polyalkoxylene, the polyalkoxylene moiety preferably consists of 2 to 20 oxide groups of

5 ethylene or ethylene oxide and propylene oxide groups. Among the latter class, those described in EP 225,654 A are particularly preferred. Those non-ionic ethoxylates which are the condensation products of fatty alcohols with 9 to 18 carbon atoms condensed with 3 to 11 moles of ethylene oxide are also preferred. . Examples of these are the condensation products of C9-18 alcohols with an average of 3 to 9 moles of ethylene oxide. Primary linear C12-C15 alcohols with an average of 3 to 9 ethylene oxide groups are preferred for use in the liquid detergent composition of the invention.

A preferred non-ionic surfactant is a C12-C18 ethoxylated alcohol comprising from 3 to 9 units of ethylene oxide per molecule. More preferred are linear linear C12-C15 ethoxylated alcohols with an average of 5 to 9 ethylene oxide groups, more preferably an average of 7 ethylene oxide groups.

Synthetic anionic surfactants suitable for detergent compositions that can be used are usually water-soluble alkali metal salts of organic sulfates and sulphonates having alkyl radicals containing from about 8 to about 22 carbon atoms, the term alkyl being used to include the alkyl portion of higher acyl radicals, including alkyl sulfates, alkyl ether sulfates, alkaryl sulfonates, alkanoyl isethionates, alkyl succinates, alkyl sulfosuccinates, N-alkoxy sarcosinates, alkyl ether carboxylates, a-olefin sulfonates and acylmethyl taurates, especially its sodium, magnesium, ammonium and mono-, di- and triethanolamine salts. The alkyl and acyl groups generally contain from 8 to 22 carbon atoms, preferably from 8 to 18 carbon atoms, even more preferably from 12 to 15 carbon atoms and may be unsaturated. Alkyl ether sulfates and alkyl ether carboxylates

25 may contain 1 to 10 units of ethylene oxide or propylene oxide per molecule, and preferably contain 1 to 3 units of ethylene oxide per molecule.

Examples of suitable synthetic anionics include sodium lauryl sulfate, sodium lauryl ether sulfate, ammonium lauryl sulphosuccinate, ammonium lauryl sulfate, ammonium lauryl sulfate, sodium cocoylisethionate, sodium lauroylisethionate and sodium N-lauryl sarcosinate. Most preferably, the synthetic anionic surfactants comprise the synthetic anionic linear alkylbenzene sulfonate (LAS) surfactant. Another suitable synthetic anionic surfactant in the present invention is sodium alcohol ethoxy ether sulfate (SAES), which preferably comprises high levels of sodium C12 alcohol ethoxy ether sulfate.

Preferred surfactant systems are mixtures of anionic detergent active materials with synthetic nonionics and additionally cationic or amphoteric surfactant. A surfactant system which is a mixture of alcohol ethoxyether sulfate (AES) and a primary C12-C15 ethoxylated alcohol with 3-9 OE ethoxylates and a cationic quaternary ammonium surfactant is especially preferred.

Preferred surfactant systems are mixtures of synthetic anionic and non-ionic detergent active materials and soap, additionally with cationic or amphoteric surfactant. Synthetic anionic surfactants may be present, for example, in amounts in the range of about 5 to about 70% by weight of the total surfactant material.

In a preferred embodiment of the invention, the detergent compositions also comprise a cationic surfactant or an amphoteric surfactant, in which the cationic or amphoteric surfactant is present at a concentration of 1 to 20%, preferably 2 to 15%, more preferably from 3 to 12% by weight of the total surfactant.

Suitable cationic surfactants that can be used are substituted or unsubstituted, straight or branched chain quaternary ammonium salts. Preferably, the cationic surfactant is of the formula:

R1R2R3R4N + X

55 in which:

R1 is C8-C22 alkyl, C8-C22 alkenyl, C8-C22 alkylarylamidopropyl or C8-C22 alkoxyalkylethyl, R2 is C1-C22 alkyl, C2-C22 alkenyl or a group of formula -A- (OA) n-OH, R3 and R4 are C1-C22 alkyl, C2-C21 alkenyl or a group of the formula -A- (OA) n-OH, A is -C2H4- and / or -C3H6- and n is a number from 0 to 20 and X is an anion . It is a commercially available and preferred example of this type of cationic surfactant a compound of the above formula in which R1 is a C12 / 14 alkyl group, R2 is a group of formula -A- (OA) n-OH in which A is -C2H4- and n is 0, and R3 and R4 are both -CH3 (specifically, C1-alkyl). This type of cationic surfactant is commercially available, for example from Clariant, under the name Praepagen HY®. Typical examples of suitable amphoteric and dipolar surfactants are alkyl betaines, alkylamido betaines, amine oxides,

65 aminopropionates, aminoglycinates, amphoteric imidazolium compounds, alkyldimethyl betaines or alkyldipolyethoxybetaines.

Optional ingredients

A wide variety of optional ingredients may be included in the compositions herein.

5 useful in detergent compositions, including other active ingredients, hydrotropes, processing aids, dyes or pigments, carriers, detergent enhancers, antioxidants, fragrances, detersive enzymes, soap suppressants, chelating agents, clay / dirt removal agents, brighteners, fabric softeners, dye transfer inhibitors, bleaching agents and the like; some of which are described in more detail below.

10 carriers

The liquid detergent compositions of the invention may contain various solvents as carriers. Suitable primary or secondary low molecular weight alcohols exemplified by methanol, ethanol, propanol and

15 isopropanol. Other suitable carrier materials are glycols such as mono-, di-, tripropylene glycol, glycerol and polyethylene glycols (PEG) having a molecular weight of 200 to 5,000. The compositions may contain from 1 to 50%, typically from 5 to 30%, preferably from 2 to 10% by weight of said carriers.

Detergent booster

One or more detergent enhancers may be present in the liquid detergent composition.

Examples of suitable organic detergent enhancers, when present, include the salts polyacetates, carboxylates, polycarboxylates, polyacetyl carboxylates, carboxymethyloxysuccinates,

25 carboxymethylximalonates and ethylenediamine-N acid, alkali metal, ammonium and substituted ammonium N-disuccinic acid, polyepoxysuccinate salts, oxidiacetates, triethylenetetraminehexaacetic acid, Nalkylimino diacetates or dipropionates, a-sulfogracinic acid salts, diphoscrylic acid oxides , polyhydroxysulfonates and mixtures thereof.

Specific examples include sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, melitic acid, benzenepolycarboxylic acids and citric acid, monosuccinate tartrate and disuccinate tartrate.

Antioxidants

The liquid detergent compositions obtainable by the process according to the present invention preferably comprise from 0.005 to 2% by weight of an antioxidant. Preferably, the antioxidant is present at a concentration in the range of 0.01 to 0.08% by weight.

40 Antioxidants are substances as described in Kirk-Othmer (Vol 3, p. 424) and in "Uhlmans Encyclopedia" (Vol. 3, p. 91). One class of antioxidants that could be used in the present invention is that of alkylated phenols having the general formula:

Wherein R is linear or branched C1-C22 alkyl, preferably methyl, or branched C3-C6 alkyl; C3-C6 alkoxy, preferably methoxy; R1 is a branched C3-C6 alkyl, preferably tert-butyl; x is 1 or 2. The hindered phenolic compounds are a preferred type of alkylated phenols according to this formula. A preferred hindered phenolic compound of this type is 2,6-di-tert-butylhydroxytoluene (BHT).

An additional class of antioxidants that could be suitable for use in the present invention is that of benzofuran or benzopyran derivatives having the formula: wherein R1 and R2 are each independently alkyl or R1 and R2 can be taken together to form a residue C5-C6 cyclic hydrocarbyl; B is absent or is CH2; R4 is C1-C6 alkyl; R5 is hydrogen or -C (O) R3 in the

5 that R3 is hydrogen or C1-C19 alkyl; R6 is C1-C6 alkyl; R7 is hydrogen or C1-C6 alkyl; X is CH2OH or CH2A in which A is a unit comprising hydrogen, phenyl or substituted phenyl. Preferred nitrogen-containing A units include amino, pyrrolidino, piperidino, morpholino, piperazine and mixtures thereof.

Antioxidants such as tocopherol sorbate, butylated hydroxybenzoic acids and their salts may also be used,

10 Gallic acid and its alkyl esters, uric acid and its salts and alkyl esters, sorbic acid and its salts, and dihydroxyfumic acid and its salts.

Fragrances

The liquid detergent compositions obtainable by the process according to the present invention preferably comprise from 0.001 to 3% by weight of the total composition of a perfume composition, preferably from 0.01 to 2% by weight of the total composition. Said perfume composition preferably comprises at least 0.01% by weight, based on the liquid composition, of a perfume component selected from terpenes, ketones, aldehydes and mixtures thereof. The perfume composition may consist

20 completely in the perfume component, but generally the perfume composition is a complex mixture of perfumes of various different perfume classifications. In this regard, the perfume composition preferably comprises at least 0.1%, more preferably at least 1.0%, even more preferably at least 5% by weight of the perfume component.

25 Detersive Enzymes

"Detersive enzyme", as used herein, means any enzyme that has a cleansing, stain remover or otherwise beneficial effect in a washing application. Suitable enzymes that could be used in the composition of the present invention include proteases, amylases, lipases, cellulases, peroxidases and mixtures thereof, of any suitable origin such as plant, animal, bacterial, fungal and yeast origin. Preferred selections are influenced by factors such as activity according to pH, thermostability and stability against active bleaching detergents, enhancers and the like. In this regard, bacterial and fungal enzymes such as bacterial proteases and fungal cellulases are preferred. Enzymes are included in the present detergent compositions for a variety of purposes, including stain removal based on

35 proteins, based on saccharides or based on triglycerides, to prevent the transfer of refined dye and for the restoration of clothes.

Enzymes are normally incorporated into detergent compositions at levels sufficient to provide an "effective cleaning amount." The term "effective cleaning amount" refers to any quantity capable of

40 produce a cleaning effect, stain remover, dirt remover, bleach or freshness improver on the treated substrate. In practical terms for normal commercial operations, typical amounts are up to about 50 mg by weight, more typically 0.01 to 30 mg, of active enzyme per gram of detergent composition. In other words, the composition of the invention may typically comprise from 0.001 to 3%, preferably from 0.01 to 1% by weight of a commercial enzyme preparation.

45 Protease enzymes are usually present in such commercial preparations at levels sufficient to provide 0.005 to 0.1 Anson units (AU) of activity per gram of composition. Higher active levels may be desirable in highly concentrated detergent formulations. Suitable examples of proteases are subtilisins that are obtained from particular strains of B. subtilis and B. licheniformis. Be

50 obtains a suitable protease from a Bacillus strain that has maximum activity over the pH range of 8-12, developed and sold as Esperase® by NovoZymes of Denmark.

Other suitable proteases include Alcalase® and Savinase® Relase® from Novozymes and Maxatase® from International Bio-Synthetics, Inc., The Netherlands.

The composition may additionally comprise enzymes as found in WO 01/00768.

Lipase enzymes suitable for use in the composition of the invention include those produced by microorganisms of the Pseudomonas group such as Pseudomonas stutzeri ATCC 19,154, as disclosed in GB 1,372,034. Lipase enzyme derived from Humicola lanuginosa and available in Novozymes under the trade name Lipex® is a very suitable lipase enzyme.

Preferred enzymes are added to the compositions after the cooling step d) in the preferred process to form premix A.

Soap Suppressors

Compounds to reduce or suppress soap formation may be incorporated into the compositions of the present invention. The suppression of soaps can be of particular importance in the so-called “process of

15 high concentration cleaning ”as described in US-A-4,489,455 and US-A-4,489,574 and in European front-loading type washers.

A wide variety of materials can be used as suds suppressors, and soaps suppressants are well known to those skilled in the art. See, for example, "Kirk Othmer Encyclopedia of Chemical Technology", 3rd edition, volume 7, pages 430-447 (John Wiley & Sons, Inc., 1979). A category of suds suppressor of particular interest includes monocarboxylic fatty acids and soluble salts thereof. See document US-A-2,954,347. The monocarboxylic fatty acids and salts thereof used as a soap suppressant typically have hydrocarbyl chains of 10 to about 24 carbon atoms, preferably 12 to 18 carbon atoms. Suitable salts include alkali metal salts

25 such as sodium, potassium and lithium, and ammonium and alkanolammonium salts. Favorable antifoaming results were obtained with mixtures of fatty acids comprising lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid and behenic acid. It is a preferred saturated fatty acid of this type Prifac 5908 (trademark of Uniqema).

The detergent compositions herein may also contain non-surfactant soap suppressants. These include, for example: high molecular weight hydrocarbons such as paraffin, fatty acid esters (for example, fatty acid triglycerides), fatty acid esters of monovalent alcohols, C18-C40 aliphatic ketones (for example, stearone), etc. .

35 The preferred category of non-surfactant suds suppressors includes silicone soaps suppressants. This category includes the use of polyorganosiloxane oils, such as polydimethylsiloxane, dispersions

or emulsions of polyorganosiloxane oils or resins and combinations of polyorganosiloxane with silica particles, in which the polyorganosiloxane is chemo absorbed or fused onto the silica. Silicone soap suppressants are well known in the art and are disclosed, for example, in US-A-4,265,779.

For any detergent composition for use in automatic washing machines, soaps should not be formed as they overflow the washing machine.

Soap suppressants, when used, are preferably present in a "suppressor amount of

45 soaps. ” "Soaps suppressing amount" means that the formulator of the composition can select an amount of this soapy-controlling agent that sufficiently controls the soaps, resulting in a low-soap detergent for use in automatic washing machines. . The compositions herein will generally comprise from 0.1 to about 5% soap suppressant.

If high soaping is desired, soaps intensifying compositions such as C10-C16 alkanolamides can be incorporated, typically at levels of 1-10%. C10-C14 monoethanol and dietanol amides illustrate a typical class of such soap intensifiers. If desired, soluble magnesium salts such as MgCl2, MgSO4 and the like can be added, at levels typically 0.1-2%, providing

55 additional soaps and enhancing fat removal performance.

Chelating agents

The liquid detergent compositions herein may optionally also contain one or more iron, copper and / or manganese chelating agents. Such chelating agents may be selected from the group consisting of aminocarboxylates, aminophosphonates, polyfunctional substituted aromatic chelating agents and mixtures thereof, all as defined hereinbelow.

If used, these chelating agents will generally comprise from about 0.1 to about

10% by weight of the detergent compositions herein. More preferably, if used, the chelating agents will comprise from about 0.1 to about 3.0% by weight of said compositions.

Clay / Antiredeposition Dirt Removal Agents

The compositions of the present invention may optionally also contain water-soluble ethoxylated amines having clayey dirt removal and anti-redeposition properties. Liquid detergent compositions typically contain from about 0.01 to about 5% of these agents.

The ethoxylated tetraethylene pentamine is a preferred release and antiredeposition agent. Further suitable ethoxylated amines are described in US-A-4,597,898.

Other types of preferred antiredeposition agent include carboxymethyl cellulose (CMC) materials. These materials are well known in the art.

15 Brighteners

Any optical brightener or other brightening or bleaching agents known in the art may be incorporated at levels typically from about 0.05 to about 1.2% by weight to the liquid detergent compositions herein. Commercial optical brighteners that may be useful in the present invention can be classified into subgroups that include, but are not necessarily limited to, stilbene derivatives, pyrazoline, coumarin, carboxylic acid, metincyanines, 5,5-dibenzotifen dioxide, azoles, heterocycles. of ring of 5 and 6 members and other miscellaneous agents. Examples of such brighteners are disclosed in "The Production and Application of Fluorescent Brightening Agents", M. Zahradnik, published by John Wiley & Sons, New York (1982).

25 Fabric softeners

Various laundry softeners may optionally be used in the wash, especially the impalpable smectite clays of US-A-4,062,647, as well as other softener clays known in the art, typically at levels of about 0.5 to about 10% in The present compositions, providing benefits of clothes softener simultaneously to the cleaning of the clothes. Clay softeners can be used in combination with amine and cationic softeners as disclosed, for example, in US-A-4,375,416 and US-A-4,291,071.

35 Dye transfer inhibiting agents

The compositions of the present invention may also include one or more materials effective to inhibit the transfer of dyes from one clothing to another during the cleaning process. Generally, such dye transfer inhibitors include polyvinyl pyrrolidone polymers, polyamine N-oxide polymers, N-vinyl pyrrolidone and N-vinylmidazole copolymers, manganese phthalocyanine, peroxidases and mixtures thereof. If these agents are used, they typically comprise from about 0.01 to about 10% by weight of the composition, preferably from about 0.01 to about 5% and more preferably from about 0.05 to about 2%.

45 Bleaches

Optionally, the composition according to the present invention may contain a bleach or bleach system. This bleaching agent or bleaching system may be, for example: (a) a bleaching species of peroxygen alone and / or in combination with a bleaching activator and / or a transition metal catalyst and (b) a transition metal catalyst in a composition substantially devoid of peroxygen species.

Bleaching catalysts for stain removal have been developed in recent years and can be used in the present invention. Examples of transition metal bleaching catalysts are found that can be used, for example, in WO 01/48298, WO 00/60045, WO 02/48301, WO

55 00/29537 and WO 00/12667. The catalyst can be provided as an alternative as a free ligand that forms an in situ complex.

Discoloration activators are also well known in the art. The exact mode of action of the bleaching activators to peroxidecolorate compounds is not known, but it is believed that they are formed perished by reacting the activators with the inorganic peroxide compound, and said peracids then release active oxygen by decomposition. They are generally compounds that contain N-acyl or O-acyl residues in the molecule and that exert their activating action on the peroxide compounds in contact with these in the washing liquid.

65 Typical examples of activators in these groups are polycylated alkylenediamines such as N, N, N1, N1 tetraacetylethylenediamine (TAED) and N, N, N1, N1-tetraacetylmethylenediamine (TAMD); acylated glycoluryls such as tetraacetylglycoluryl (TAGU); triacetyl cyanurate and sodium sulfophenylethylcarbonic acid ester.

Peroxide bleaching agents are also well known in the art, for example, peracids (eg, PAP), perborates, percarbonates, peroxyhydrates and mixtures thereof. Specific examples

5 preferred include: sodium perborate, commercially available as mono- and tetrahydrates, and sodium carbonate peroxyhydrate. Other examples of peroxyl species and activators, as well as other transition metal catalysts, are found in WO 02/077145.

It is also preferred to include in the compositions a stabilizer for the bleach or bleaching system, for example, ethylenediamine tetramethylene phosphonate and diethylenetriamine pentamethylene phosphonate or other suitable organic phosphonates or salts thereof. These stabilizers can be used in acid or salt form, which is the salt form of calcium, magnesium, zinc or aluminum. The stabilizer may be present at a level of up to about 1% by weight, preferably from about 0.1 to about 0.5% by weight.

15 Since many bleaching agents and bleaching systems are unstable in aqueous liquid detergents and / or interact unfavorably with the other components of the composition, for example enzymes, they can be protected, for example by encapsulation or by formulating a structured liquid composition, with They are suspended in solid form.

Photodecolorants, including singlet oxygen photodecolorants, could also be used.

PREMIX B

In addition to any viscosity modifying ingredient, water could normally be used, but also hydrotropes. Premix B comprises the microcapsules.

Microcapsules

It is an essential element of the composition as it is carried out by the process according to the invention at least 0.01% by weight of microcapsules with an anionic charge. Such microcapsules can supply a variety of beneficial agents by deposition on substrates such as laundry. To obtain maximum benefit, they should be well dispersed throughout the liquid detergent composition and the vast majority of microcapsules should not be significantly agglomerated. It has been found that any microcapsule that agglomerates during processing thus remains in the container and therefore will be irregularly dispensed

35 during the use of the composition. This is highly undesirable. The contents of the microcapsules are normally liquid. For example, possible fragrances, oils, fabric softening additives and clothing care additives are contained. The invention is not specific to any particular type of content. Preferred microcapsules are particles called core microparticles on deck. As used herein, the term "core core microcapsules" refers to encapsulates in which a shell that is substantially or totally non-water soluble at 40 ° C surrounds a core that comprises or consists of a beneficial agent (which is a liquid or is dispersed in a liquid carrier).

Suitable microcapsules are those described in US-A-5,066,419, which have a crumbly coating, preferably an aminoplast polymer. Preferably, the coating is the product of

The reaction of an amine selected from urea and melamine, or mixtures thereof, and an aldehyde selected from formaldehyde, acetaldehyde, glutaraldehyde or mixtures thereof. Preferably, the coating is 1 to 30% by weight of the particles.

Coated core microcapsules of other classes are also available for use in the present invention. The embodiments of said other microcapsules of beneficial agents such as perfume include precipitation and deposition of polymers at the interface such as in coacervates, as disclosed in GB-A-751.600, US-A-3,341,466 and EP-A-385,534, as well as other polymerization pathways such as interphase condensation, as described in US-A-3,577,515, US-A-2003/0125222, US-A

6,020,066 and WO-A-03/101606. Microcapsules having polyurea walls are disclosed in documents US-A-6,797,670 and US-A-6,586,107.

Other patent applications that specifically relate to the use of melamine-formaldehyde coated core microcapsules in aqueous liquids are WO-A-98/28396, WO 02/074430, EP-A-1,244,768, US-A2004 / 0071746 and US-A-200410142868.

White oil is a highly refined colorless hydrocarbon oil of low volatility and a wide range of viscosities; used for lubrication of food and textile machinery and as medicinal and mineral oil. Melamine coated microcapsules containing white oil are slightly anionic (negatively charged). It has been found that the surface charge on the microcapsules affects their dispersion. A low charge seems to result in an electrostatic repulsion / stabilization too small to keep them apart in water-poor (concentrated) formulations. This gets even worse for

highly concentrated anionic compositions. The problem seems to be worse for weakly anionic particles of a certain size.

Perfume encapsulates are a preferred type of microcapsule suitable for use in the present invention.

The preferred perfume microcapsules used in the present invention are core microcapsules in cover. As used herein, "core microcapsules in cover" refers to encapsulates in which a cover that is substantially or totally non-water soluble at 40 ° C surrounds a core that comprises or consists of perfume (including any liquid carrier thereof) .

A preferred class of cover core perfume microcapsules comprises those disclosed in WO 2006/066654 A1. These comprise a core having about 5 to about 50% by weight of perfume dispersed in about 95 to about 50% by weight of carrier material. This carrier material is preferably a fatty alcohol or fatty ester carrier material

15 non-polymeric solid, or mixtures thereof. Preferably, the esters or alcohols have a molecular weight of about 100 to about 500 and a melting point of about 37 to about 80 ° C, and are substantially non-water soluble. The core comprising the perfume and the carrier material is coated with a substantially non-water soluble coating on its external surfaces. Similar microcapsules are disclosed in US 5,154,842 and these are also suitable.

The microcapsules as described in US-A-5,066,419 have a crumbly coating that is preferably an aminoplast polymer. Preferably, the coating is the reaction product of an amine selected from urea and melamine, or mixtures thereof, and an aldehyde selected from formaldehyde, acetaldehyde, glutaraldehyde or mixtures thereof. Preferably, the coating is 1 to 30% by weight of

25 particles.

Coating core perfume microcapsules of other classes are also available for use in the present invention. The ways of preparing said other perfume microcapsules include precipitation and deposition of polymers at the interface such as in coacervates, as disclosed in GB-A-751.600, USA-3,341,466 and EP-A-385,534, as well as other polymerization pathways such as interphase condensation, as described in US-A-3,577,515, US-A-2003/0125222, US-A-6,020,066 and WO-A-03/101606. Microcapsules having polyurea walls are disclosed in US-A-6,797,670 and US-A-6,586,107.

These are other patent applications that relate specifically to the use of core microcapsules in

Documents melamine-formaldehyde in aqueous liquids documents WO-A-98/28396, WO 02/074430, EP-A1.244.768, US-A-2004/0071746 and US-A-2004/0142868.

The microcapsules can be bonded with suitable substrates, for example, to provide a persistent fragrance that is desirably released after completing the cleaning process.

Liquid detergent compositions

The process provides structured liquid detergent compositions in which the microcapsules are present without a significant proportion of them being in an inefficient and size agglomerated form

45 increased. The composition is concentrated and has 30% by weight or more of surfactant and an external structuring system, preferably hydrogenated castor oil, is present at a concentration of 0.15 to 0.5% by weight of the total composition.

Preferably, the concentration of surfactants in the liquid detergent composition according to the invention is 30 to 65% by weight, more preferably 32 to 60% by weight and most preferably 35 to 50% by weight of the total composition.

The liquid cleaning composition may be formulated as a concentrated cleaning liquid for direct application to a substrate, or for application to a substrate after dilution, such as dilution before or during the use of

55 the liquid composition by the consumer or in the washing apparatus.

Although the composition and method according to the present invention can be used to clean any suitable substrate, the suitable substrate is laundry clothes. Cleaning can be carried out by simply leaving the substrate in contact for a sufficient period of time with a liquid medium constituted by or prepared from the liquid cleaning composition. However, the cleaning medium or containing the substrate is preferably stirred.

Product form

The liquid detergent compositions obtainable by the process according to the present invention are preferably concentrated liquid cleaning compositions. The liquid compositions have a physical form in the range of colable liquid, colable gel to non-colable gel. These forms are conveniently characterized by the viscosity of the product. In these definitions, and unless explicitly stated otherwise, throughout this specification all the viscosities manifested are those measured at a shear rate of 21 s-1 and a temperature of 25 ° C. This shear rate is the shear rate that is

5 usually exerts on the liquid when it is poured from a bottle. The liquid detergent compositions prepared according to the invention are liquids of pseudoplastic behavior.

The collapsible liquid detergent compositions preferably have a viscosity of not more than 1,500 mPa.s, more preferably of not more than 1,000 mPa.s, even more preferably of not more than 500 mPa.s. Typically, the viscosity is less than 500 mPa.s at 21 s-1.

Liquid detergent compositions that are collapsible gels preferably have a viscosity of at least

1,500 mPa.s, but not more than 6,000 mPa.s, more preferably not more than 4,000 mPa.s, even more preferably not more than 3,000 mPa.s and especially not more than 2,000 mPa.s.

The non-collapsible gels preferably have a viscosity of at least 6,000 mPa.s, but not more than 12,000 mPa.s, more preferably not more than 10,000 mPa.s, even more preferably not more than 8,000 mPa.s and especially not more than 7,000 mPa.s.

For the purposes of the invention, a composition is considered physically stable when it remains homogeneous with perfume encapsulates dispersed and suspended for a period of approximately 3 months at temperatures of 5 to 50 ° C.

The invention will now be described further with reference to the following non-limiting examples. 25 Example 1

The composition was prepared as listed in Table 1 (Premix A) by a process as described in WO 2010 034736 A, whose relevant content is repeated above. This process is based on a conventional neutralization process for the manufacture of LAS / SLES / NI and soap-based active high-power liquid detergent. Enzymes and perfume are added after neutralization.

Table 1 - Premix A

Ingredient

Level (%)

LAS acid

12.80

Nonionic with 7OE

19.21

Saturated fatty acid (Prifac 5908)

4.56

sLES 3 OE

6.40

Citric acid

0.94

NaOH

 2.58

Triethanolamine

3.09

Propylene glycol

8.60

Glycerol

 4.78

Kidnapper (Dequest 2066)

0.478

Optical brightener

0.100

PAA / S copolymer (opacifying)

0.097

Enzymes

1.80

HCO (Thixcin R)

0.25

Dyes

0.00078

Fragrance

1.39

Water

Up to 98.00

35 The liquid detergent composition was obtained by the following procedure: Premix 1

200 g of deionized water was added with stirring at 150 rpm, using a rod stirrer, to a 3 L beaker and heated to 30 ° C. 1.47 g of optical brightener was then added to this solution together with 50 g of glycerol, 90 g of propylene glycol and the neutralizing bases 57.5 g of sodium hydroxide and 31.5 g of triethanolamine. 201 g of non-ionic with 7OE, 128 g of linear alkylbenzenesulfonic acid and 20 g of citric acid were then added in rapid succession, generating considerable heat of neutralization and bringing the temperature to 65-70 ° C. This basic temperature of 65-70 ° C was maintained until the addition of premix 2.

Premix 2

47 g of Prifac 5908 were dissolved in a separate 500 ml beaker using stirring at 100 rpm and heating at 70-75 ° C. Then 2 g of Elementis Thixcin ® hydrogenated castor oil was dissolved in the hot fatty acid. This premix is stirred for an additional 5-10 minutes to ensure complete dissolution and mixing of the external structurant. The solution is complete when premix solution 2 is completely transparent.

Premix A (premix 1 + premix 2)

The two premixes are now combined by adding premix 2 (70-75 ° C) to premix 1 (65-70 ° C), increasing the stirring to 200 rpm and allowing the two premixes to mix thoroughly for 10 minutes. Then 16 g of the sequestrant was added followed by 96 g of sodium lauryl ether sulfate (sLES) and allowed to mix for an additional 10 minutes before cooling to 30 ° C. Cooling was performed by natural cooling for a period of 2 hours or, alternatively, the main batch was cooled using a plate heat exchanger, cooling the main mixture from 60-65 ° C to 30 ° C in less than one minute and keeping it for 10 minutes at this low temperature.

Subsequently, 0.08 g of dye dyes were added, as well as 10.5 g of enzymes and 10 g of perfume, and allowed to mix for an additional 10 minutes before pumping out of the container, forming premix A. This mixture is a non-Newtonian fluid with a creep effort of approx. 0.3 Pa and a viscosity of 350 mPas at 21

-

one

s.

Premix B

The microcapsules used had a melamine-formaldehyde coating and were anionic with an average particle size of 15.8 μm. They were available in a dense suspension with a solids content of 48.6% by weight and a dense suspension viscosity of 425 mPas. With dilution with an equivalent volume of water, the resulting premix B has a viscosity at 25 ° C of 10 mPas.

2 parts of premix B were added to 98 parts of premix A in a stirred batch mixer with blades for approx. 15 min, using only shaking the container. This resulted in the formation of microcapsule agglomerates, the agglomerates being well dispersed in the mixture.

To attempt to degrade the agglomerates, the mixture was then pumped through a static in-line mixer. The typical mixing energy supplied by said mixer is approximately 100 times that of a paddle mixer.

When mixed in a liquid in the conventional manner using said paddle mixer, these microparticles produce a dispersion ratio of 70:30 (not agglomerated: agglomerated as defined above) compared to 96: 4 using the process according to the present invention.

The level of microcapsules in the final dispersed mixture is 0.46%.

The microscopic visual inspection of the dispersed microcapsules also proved that there was no rupture of the microcapsules caused by the process.

Claims (5)

1. A process for incorporating microcapsules with an anionic charge into a structured aqueous concentrated liquid detergent comprising at least 30% by weight, preferably at most 65% by weight, of Total surfactant, of which at least 5% by weight, based on the total composition, is an anionic surfactant, including soap, and an external structurant, the process comprising combining the two premixes; premix A which is the structured aqueous concentrated liquid detergent composition without microcapsules and premix B, which comprises an aqueous dispersion of microcapsules with an anionic charge, characterized in that 10 premix B is a dense suspension of microcapsules with a maximum viscosity at 25 ° C of 100 mPa.s and at least 90% by weight of the microcapsules have a particle size in the range of 5 to 30 μm, and because premix B is added to premix A and the resulting combined mixture is passed through a static in-line mixer with an energy input of 20 to 500 J / kg forming, immediately after the mixer, a A structured liquid comprising less than 10%, based on the total number of microcapsule groups, agglomerated groups of microcapsules, an agglomerated group of microcapsules being defined as a group having more than 5 microcapsules grouped together.

2.

 A process according to claim 1, wherein the viscosity of premix B is reduced by dilution with water. twenty

3. A process according to any preceding claim, wherein the external structurant is hydrogenated castor oil (castor wax).

Four.

 A process according to any preceding claim, wherein the microcapsules comprise a melamine-formaldehyde shell.

5. A process according to any one of claims 1 to 3, wherein the microcapsules comprise a shell comprising a material selected from polyurea, polyurethane, starch / polysaccharides and aminoplasts. A process according to any preceding claim in which the microcapsules are encapsulated in perfume.