FR2774389A1 - WATER-DISPERSABLE GRANULES COMPRISING A FRAGRANCE IN A WATER-SOLUBLE OR WATER-DISPERSABLE MATRIX AND METHOD FOR PREPARING THEM - Google Patents

Abstract

The invention concerns water dispersible granulates comprising: at least a hydrophobic perfume (P), in the form of droplets, finely divided in and encapsulated by a water soluble or water dispersible solid organic matrix (MO) selected among: polypeptides (PP) of plant or synthetic origin; polyelectrolytes (PE) belonging to the family of weak polyacids; or their mixtures; and at least an emulsifying agent (AE) at the droplet/matrix interface. The invention also concerns a method, in two steps, for preparing said granulates, the first step consisting in preparing an emulsion in water comprising at least a hydrophobic perfume (P), at least an emulsifying agent (AE); and said water soluble or water dispersible organic matrix (MO), the second step consisting in drying said emulsion until a granulate is formed.

Description

DISPERSABLE GRANULES IN WATER COMPRISING A FRAGRANCE
IN A WATER-SOLUBLE OR HYDRODISPERSABLE MATRIX
AND PROCESS FOR PREPARING THEM
The present invention relates to water-dispersible granules, comprising at least one perfume in a water-soluble or water-dispersible organic polymer matrix, process for their preparation, their use as a perfuming agent in detergent or cosmetic compositions and detergent compositions for laundry or cosmetics comprising said particles.

 The perfuming of washing detergent compositions, especially laundry. requires a number of constraints, more or less important according to the techno-economic objectives and marketing of the formulator.

 One of the first problems posed is to find a suitable mode of addition and distribution of the liquid perfume on the detergent powder.

Generally the perfume is sprayed finely, continuously, on the formulated powder, complete. which transits in any carrier, between the place of manufacture and the place of conditioning. Pneumatic transport can be used for this operation, or the "air lift" systems. It is necessary that the formulated detergent is sufficiently cooled, in particular when the manufacturing process is a spraying process, and that the mixing system allows a minimum loss of the scented substance, which is the most expensive component of the formulation. . The respect of the dosage (% of perfume with respect to the powder) is one of the elements difficult to control and that it is necessary to seek to improve as well for cost problems as for problems of constancy of quality.

The solid-particulate shaping of the composition may represent a first improvement at this level of the laundry manufacturing process.

 Another problem of the washing of the detergents is that of the stability of the perfume (and of all the "notes" it releases) during the storage of the laundry in its packaging.

Indeed, the laundry components themselves are very varied and their chemical natures are very different and can be aggressive or incompatible with the scented composition, which contains chemically fragile components.

Modern detergents often contain bleaching systems based on products releasing hydrogen peroxide and then active oxygen. This is the most destabilizing element for perfumes.

The alkalinity of the compositions is also a factor of degradation of the perfume.

Highly absorbent products such as silicas, clays, zeolites can selectively and more or less strongly absorb the perfume or one of its components and this material contribute to modifying or altering it.

Similarly, water of crystallization, free water, surfactants, sequestering agents, which are always present in the detergent compositions can interfere negatively with the scented compositions.

A third problem, or a third requirement, encountered in the field of laundry perfuming, is the fact that the perception of the chosen odor, which is one of the methods of recognition of the laundry by the buyer, must be effective at all. the life cycles of the laundry, and even beyond.

In particular, the smell of perfume. or at least a fraction of this odor, must be perceptible in the store where the laundry is presented at the purchase, during the life of the package (even open), during the washing itself, from the machine to wash, during the drying, ironing and storage of the washed items, in the storage cabinet, and finally during the wearing or use of the laundry.

Such a series of requirements is obviously not easy to satisfy, but among the means that must be deployed to achieve this satisfaction, encapsulation and encapsulation, which improve storage stability and can allow under certain conditions , a release of the perfume during the washing, are one of the most important and most effective means.

 Several solid forms of perfume shaping have been tried in the past or very recently by perfume manufacturers or laundry manufacturers to solve some or all of these problems.

 One of the first means is to use the absorbing properties of certain porous supports, such as silicas, clays, natural or synthetic zeolites, starches, carboxymethylcellulose, urea, soluble inorganic phosphates.

But the disadvantages of these modes of shaping are numerous, in particular the fact of dividing and spreading the perfume over very large contact surfaces, thus increasing the risk of oxidation at the same time as the exchange surface between perfume and air, and also the risk of selectively retaining one or more components, with restitution of a modified odor.

The simple absorption allows the solid shaping, but is often insufficient for the protection of the perfume during storage. In addition, it is necessary to use a coating of the perfume / support assembly.

 Another form of shaping is the use of products with a particular molecular structure for creating a reception cavity for perfumes, for example products such as cyclodextrins. The disadvantage, besides the cost, is the difficulty in introducing complex compositions based on products of very different and dissimilar molecular weight and steric bulk.

 Organic matrices composed of PEG or paraffins of molecular mass sufficient to be solid at ordinary temperature, have also been proposed to solidify the perfume compositions, with advantages but also disadvantages, particularly that of only partially releasing the perfume or the having to use melted phases of the coating products.

 Also sophisticated and difficult to control methods as interfacial polycondensation microencapsulation techniques have been advanced to obtain encapsulated perfumes, but their cost and complexity has not facilitated their development.

 Finally, the use of preformed microcapsules, either mineral or polymeric, possibly mechanically friable has also been considered, without great commercial success, probably for economic reasons.

 The Applicant has found a solid shaping that can be dispersed in water, liquid perfumes, by encapsulation by a protective matrix which is located outside the finely divided perfume droplets; in this way, said matrix coats the perfume. protects it at the same time as it allows the transition to the solid state.

A first subject of the invention consists of dispersible granules in water, comprising - at least one hydrophobic perfume (P), in the form of droplets, finely divided in and encapsulated by a water-soluble or water-dispersible solid organic matrix (MO), chosen from
the polypeptides (PP) of plant or synthetic origin that are water-soluble or water-dispersible
polyelectrolytes (PE) belonging to the family of weak polyacids
water-soluble or water-dispersible oses, osides or polyholosides (O)
* or their mixtures.

and at least one emulsifying agent (AE) at the droplet / matrix interface.

 For a good embodiment of the invention, said dispersible granules in water comprise 5 to 90%, preferably 25 to 70% of their weight, perfume (P), 5 to 90%, preferably from 25 to 70% of their weight, of water-soluble or water-dispersible organic matrix (MO), of 0.02 to 20%, preferably of 0.1 to 10% of their weight, of emulsifying agent (AE), said percentages being expressed by weight of dry matter.

 Said droplets may have an average particle size of the order of 0.1 to 1 ohm. preferably of the order of 0.2 to 5 pm.

 The term "perfume" is a fragrant essence, or more generally a complex composition obtained with the aid of many odorous products in mixture and excipients which ensure the homogeneity.

Said fragrances according to the invention are isotropic and hydrophobic compounds. Their solubility in water at pH 7 does not exceed 10% by weight.

 The fragrance blend may include a large number of components, selected to achieve the desired fragrance ratings for the intended use, audience and market. There are usually natural products (for example, vegetable or animal essences obtained by steam extraction or by alcohol extraction, which are themselves already mixtures) or synthetic products which may be aliphatic or aromatic ketones, aliphatic aldehydes or aromatics, condensation products of aldehydes and amines, aromatic or aliphatic lactones, aromatic or aliphatic ethers or esters, aliphatic alcohols of various molecular weights, saturated or unsaturated linear, cyclic or aromatic, terpeneic, polynuclear or non-polymeric hydrocarbons .

The most sophisticated perfume compositions can contain up to a hundred ingredients.

As an example of an odorant compound, mention may be made of:
Hexyl cinnamic aldehyde, 2-methyl-3 (para-tert-butylphenyl) -propionaldehyde
7-acetyl-1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphthalene
benzyl salicylate; 7-acetyl-1,1,3,4,4,6-hexamethyltetraline
para-tert-butyl cyclohexyl acetate
methyl dihydrojasmonate; beta-naphthol methyl ether
methyl beta-naphthyl ketone; 2-methyl-2- (para-iso-propylphenyl) -propionaldehyde
1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-cyclopenta-gamma-2-benzopyran
dodecahydro-3a, 6,6,9a-tetramethylnaphtho [2,1b] bifuran; anisaldehyde
coumarin; cedrol; vanillin; Cyclopentadecanolide
tricyclodecenyl acetate; tricyclodecenylpropionate; phenylethyl alcohol
terpineol; the linalool; linalyl acetate; geraniol; nerol
2- (1,1-dimethylethyl) cyclohexanol acetate; benzyl acetate; the terpenes (orange)
eugenol; diethylphthalate
essential oils, resins or resinoids (orange oil, lemon, patchouli, Peruvian pear, Olibanum resinoid, styrax, coriander, lavandin, lavender ...)
Other examples of odorant compounds are described in H 1468 (United States
Statutory Invention Registration).

Among the water-soluble or water-dispersible synthetic polypeptides (PP) that can constitute the matrix, mention may be made of homopolymers and copolymers derived from the polycondensation of amino acids. in particular aspartic and glutamic acid or precursors of said aminodiacides, and hydrolysis. These polymers can be homopolymers derived from aspartic acid or glutamic acid as well as copolymers derived from aspartic acid and glutamic acid in any proportions, or copolymers derived from aspartic and / or glutamic acid and amino acids other. Among the copolymerizable amino acids, mention may be made of glycine, alanine, leucine, isoleucine, phenylalanine and methionine.
Histidine, proline, lysine, serine, threonine, cysteine
Among the polypeptides (PP) of vegetable origin, mention may be made of water-soluble or water-dispersible plant origin proteins. They are preferably hydrolysed; their degree of hydrolysis is preferably less than 40%.

Among the proteins of plant origin, mention may be made, for example, of proteins
from protein crops such as peas, faba beans, lupine,
beans, and lentils; proteins derived from cereal grains in particular
those of wheat, barley, rye, maize, rice, oats, and millet; the
proteins from oilseeds, in particular those from soybeans. of
peanuts, sunflower, rapeseed, and coconut; proteins from
leaves including alfalfa, and nettles; and proteins from organs
plant reserves buried including that of potato, and beet.

 The protein of plant origin comes more particularly from soy or wheat.

The polyelectrolyte (PE) may be chosen from those resulting from the polymerization of monomers which have the general formula
R1R2 C = C R3R4 wherein Rj, same or different, represent H, CH3, CO2H, (CH2) n CO2H with n = 0 to 4.

 By way of nonlimiting examples, mention may be made of acrylic, methacrylic and maleic acids. fumaric, itaconic, crotonic.

Copolymers obtained from the monomers corresponding to the above general formula and those obtained using these monomers and other monomers, in particular vinyl derivatives such as vinyl alcohols and copolymerizable amides, such as acrylamide or methacrylamide. Mention may also be made of copolymers obtained from alkyl vinyl ether and maleic acid, as well as those obtained from vinyl styrene and maleic acid, which are described in particular in the KIRK-OTHMER encyclopedia entitled "ENCYCLOPEDIA OF
CHEMICAL TECHNOLOGY "- Volume 18 - 3rd edition - Wiley interscience publication - 1982.

 Preferred polyelectrolytes have a low degree of polymerization. The weight-average molecular weight of the polyelectrolytes is more particularly less than 20000 g / mol. Preferably, it is between 1000 and 5000 g / mol.

 Among the doses there may be mentioned aldoses such as glucose, mannose, galactose, ribose, and ketoses such as fructose.

 Osseids are compounds that result from the condensation, with elimination of water, of molecules of oses between them or even molecules of oses with non-carbohydrate molecules. Of the osides, holosides which are formed by the combination of exclusively carbohydrate units and more particularly oligoholosides (or oligosaccharides) which comprise only a small number of these units, that is to say a generally lower number, are preferred. or as 10. Examples of oligoholosides include sucrose, lactose, cellobiose, maltose and trehalose.

 The water-soluble or water-dispersible polyholosides (or polysaccharides) are highly depolymerized; they are described, for example, in P. ARNAUD's book titled "course in organic chemistry", Gaultier-Villars Publishers, 1987. More particularly, these polyholosides have a molecular weight by weight of less than 20,000 g / mole.

 By way of nonlimiting example of strongly depolymerized polyholosides, mention may be made of dextran, starch, xanthan gum and galactomannans such as guar or carob, these polysaccharides preferably having a melting point of greater than 1000 ° C. and a solubility in water of between 50 and 500 g / l.

 The emulsifying agents (AE) that may be present are ionic or amphoteric nonionic emulsifiers.

Among the nonionic emulsifiers, mention may in particular be made of polyoxyalkylenated derivatives such as ethoxylated or ethoxy-propoxylated fatty alcohols, ethoxylated or ethoxy-propoxylated triglycerides, ethoxylated or ethoxy-propoxylated fatty acids, and ethoxylated or ethoxylated sorbitan esters. propoxylated - ethoxylated or ethoxy-propoxylated fatty amines - ethoxylated or ethoxy-propoxylated di (1-phenylethyl) phenols - ethoxylated or ethoxy-propoxylated tri (1-phenylethyl) phenols - ethoxylated or ethoxy-propoxylated alkyl phenols
The number of oxyethylene (OE) and / or oxypropylene (OP) units of these nonionic surfactants usually varies from 2 to 100 depending on the desired HLB (hydrophilic / lipophilic balance). More particularly, the number of EO and / or OP units is between 2 and 50. Preferably, the number of EO and / or OP units is between 10 and 50.

 The ethoxylated or ethoxy-propoxylated fatty alcohols generally comprise from 6 to 22 carbon atoms, the EO and OP units being excluded from these numbers. Preferably, these units are ethoxylated units.

 The ethoxylated or ethoxy-propoxylated triglycerides may be triglycerides of vegetable or animal origin (such as lard, tallow, peanut oil, butter oil, cottonseed oil, oil). oil, olive oil, fish oil, palm oil, grape seed oil, soya bean oil, castor oil, rapeseed oil, coconut oil, coconut oil and are preferably ethoxylated.

 The ethoxylated or ethoxy-propoxylated fatty acids are fatty acid esters (such as, for example, oleic acid, stearic acid), and are preferably ethoxylated.

 The ethoxylated or ethoxy-propoxylated sorbitan esters are cyclized fatty acid esters of sorbitol comprising from 10 to 20 carbon atoms such as lauric acid, stearic acid or oleic acid, and are preferably ethoxylated.

 The term ethoxylated triglyceride is intended in the present invention, both the products obtained by ethoxylation of a triglyceride by ethylene oxide and those obtained by transesterification of a triglyceride with a polyethylene glycol.

 Similarly, the term ethoxylated fatty acid includes both the products obtained by the ethoxylation of a fatty acid by ethylene oxide and those obtained by transesterification of a fatty acid with a polyethylene glycol.

 The ethoxylated or ethoxy-propoxylated fatty amines generally have from 10 to 22 carbon atoms, the EO and OP units being excluded from these numbers, and are preferably ethoxylated.

 The ethoxylated or ethoxy-propoxylated alkylphenols are generally 1 or 2 alkyl groups, linear or branched, having 4 to 12 carbon atoms. By way of example, mention may be made especially of octyl, nonyl or dodecyl groups.

 As examples of nonionic surfactants of the group of ethoxylated or ethoxy-propoxylated alkylphenols, ethoxylated di (1-phenylethyl) phenols and ethoxylated or ethoxy-propoxylated tri (1-phenylethyl) phenols, mention may be made of especially ethoxylated di (1-phenylethyl) phenol with 5 EO units, ethoxylated di (1-phenylethyl) phenol with 10 EO units, ethoxylated tri (1-phenylethyl) phenol with 16 EO units, tri (phenyl) Ethoxylated ethoxylated phenol with 20 EO units, ethoxylated tri (1-phenylethyl) phenol with 25 EO units, ethoxylated tri (1-phenylethyl) phenol with 40 EO units, tri (1-phenylethyl) phenols ethoxy-propoxylated with 25 EO + OP units, nonylphenol ethoxylated with 2 EO units, nonylphenol ethoxylated with 4 EO units, nonylphenol ethoxylated with 6 EO units, nonylphenol ethoxylated with 9 EO units, nonylphenols ethoxypropoxylated with 25 EO + units OP, ethoxyl-propoxylated nonylphenols with 30 EO + OP motifs, ethoxyl-propoxylated nonylphenols with 40 EO + OP units, ethoxy-propoxylated nonylphenols with 55 EO + OP units, ethoxypropoxylated nonylphenols with 80 EO + OP units.

 Among the anionic emulsifiers, mention may be made of water-soluble salts of alkyl sulphates, alkyl ether sulphates, alkyl isethionates and alkyl taurates or their salts, alkyl carboxylates, alkyl sulphosuccinates or alkyl succinamates, alkyl sarcosinates, alkyl derivatives of protein hydrolysates and acyl aspartates. the alkyl ester and / or alkyl ether and / or alkylaryl ether phosphates.

The cation is generally an alkali metal or alkaline earth metal, such as sodium, potassium, lithium, magnesium, or an ammonium group NR4 + with R, which may be identical or different, representing an alkyl radical which may or may not be substituted by a hydrogen atom. oxygen or nitrogen.

 Among the cationic emulsifiers, mention may be made of alkyldimethylbenzylammonium halides and alkyldimethylethylammonium halides. . .

Among the amphoteric emulsifiers, mention may be made of alkylbetaines, alkyldimethylbetaines, alkylamidopropylbetaines, alkylamidopropyldimethylbetaines, alkyltrimethylsulfobetaines, imidazoline derivatives such as alkylamphoacetates, alkylamphodiacetates, alkylamphopropionates, alkylamphodipropionates, alkylsultaines or alkylamidopropyl hydroxysultaines. the condensation products of fatty acids and protein hydrolysates. amphoteric derivatives of alkylpolyamines such as Amphionic XL%) marketed by Rhône
Poulenc, Ampholac 7TtXe and Ampholac 7C / X (8) marketed by Berol Nobel, proteins or protein hydrolysates.

A second object of the invention consists of a two-step preparation process, of dispersible granules in water, comprising - at least one hydrophobic perfume (P), in the form of droplets, finely divided in and encapsulated by an organic matrix water-soluble or water-dispersible solid (MO), chosen from
the polypeptides (PP) of plant or synthetic origin that are water-soluble or water-dispersible
polyelectrolytes (PE) belonging to the family of weak polyacids
water-soluble or water-dispersible oses, osides or polyholosides (O)
* or their mixtures.

and at least one emulsifying agent (AE) at the droplet / matrix interface, the first step consisting in preparing an emulsion in water comprising at least one hydrophobic perfume (P), at least one emulsifying agent (AE) and said water-soluble or water-dispersible organic matrix (MO), the second step of drying said emulsion until a granule is formed.

 The term "hydrophobic" is synonymous with solubility in water at pH 7 not exceeding 10% by weight.

 The relative amounts of perfume (P), emulsifying agent (AE) and water-soluble or water-dispersible organic matrix (OM) used are such that said emulsion, expressed in dry form, comprises from 5 to 90%, preferably from 25 to 70% of their weight. hydrophobic perfume (P), - from 5 to 90%, preferably from 25 to 70% by weight, of water-soluble or water-dispersible organic matrix (MO), - from 0.02 to 20%, preferably from 0.1 at 10% of their weight, emulsifying agent (AE), said percentages being expressed by weight of dry matter.

 The amount of dry matter of the emulsion is generally between 10 and 70% by weight and preferably between 20 and 60% by weight.

All methods of preparing emulsions known to those skilled in the art and which are described in "ENCYCLOPEDIA of
EMULSIONS TECHNOLOGY ", volumes 1 to 3 by Paul BECHER edited by MARCEL
DEKKER INC., 1983.

 Thus, the so-called direct phase emulsification method is suitable for the preparation of the granules according to the invention. It is briefly recalled that this method consists in preparing a mixture containing the water, the emulsifier (s), the water-soluble or water-dispersible matrix (OM), and then introducing the perfume in liquid form, with stirring.

 The emulsion can also be prepared by using colloid mills such as MENTON GAULIN and MICROFLUIDIZER (MICROFLUIDICS).

 The average particle size of the emulsion is in general between 0.1 and 10 microns and preferably between 0.2 and 5 microns.

 The emulsification can be carried out at a temperature close to room temperature, although lower or higher temperatures are possible.

 The second step of the preparation process according to the invention consists in drying the emulsion thus formulated to obtain granules.

 The method used to remove water from the emulsion and obtain granules can be carried out by any means known to those skilled in the art.

 For example lyophilization, which corresponds to a freezing step, is suitable. followed by a sublimation step, or even spray drying.

 These modes of drying, and more particularly that by atomization, are particularly indicated because they make it possible to preserve the emulsion in the state and to obtain pellets directly. The water-soluble or water-dispersible vegetable proteins are particularly well adapted to spray drying because they are particularly stable.

 Spray drying may be carried out in the usual manner in any known apparatus such as for example an atomization tower associating a spraying carried out by a nozzle or a turbine with a stream of hot gas.

The conditions of implementation are a function of the nature of the matrix, the thermosensibility of the perfume and the atomizer used; these conditions are generally such that the temperature of the whole product during drying does not exceed 15,000, preferably not more than 110 ° C.

 Unexpectedly, the spray drying in a stream of hot gas is done without altering the perfume.

It should be noted that additives. such that the anti-caking agents may be incorporated into the granules at the time of this second drying step. It is recommended to use a filler selected in particular from calcium carbonate, kaolin, silica, bentonite
The composite particles obtained are redispersible in water.

 The release of the perfume. during the re-dispersal can be controlled by the choice of the organic matrix (MO), choosing a matrix with gradual or slow solubility.

 Another object of the invention is the use of said dispersible granules as a perfuming agent in cosmetic compositions and in particular in detergent compositions for washing clothes (industrial or household washing).

According to the invention, said granules may be used in amounts of about 0.01 to 0.5%, preferably 0.05 to 0.2% by weight, based on the detergent composition.

 A final subject of the invention consists of cosmetic compositions and especially detergent compositions for washing laundry (industrial or household washing), comprising said dispersible granules based on perfume.

 According to the invention, the detergent compositions may contain about 0.01 to 0.5%, preferably 0.05 to 0.2%, of their weight of fragrance-based dispersible granules.

 The detergent compositions according to the invention comprise at least one surfactant, in an amount generally of the order of 5 to 60% by weight. preferably from 8 to 50% by weight.

Among these, there may be mentioned anionic or nonionic surfactants usually used in the field of detergency for washing laundry.

 The detergent compositions which are the subject of the invention may also comprise conventional additives, such as inorganic or organic builders, in an amount such that the total amount of detergency builder is 5 to 80% by weight of said composition, preferably 8 to 40% by weight, antifouling agents, antiredeposition agents, bleaching agents, fluorescence agents, suds suppressing agents, agents softeners, enzymes and other additives.

 The following examples are given for illustrative purposes.

Example 1; - Production of a perfume emulsion in an aqueous solution of soy protein
A mixture of the following composition is prepared

<tb> FP940 <SEP>(SEP>SEP> Protein <SEP>SEP> Soy <SEP>SEP><SEP> Hydrolysis <SEP>SEP><SEP><SEP> in <SEP> weight
<tb> lower <SEP> than <SEP> 5%, <SEP> of <SEP> Protein <SEP> Technologies <SEP> International <SEP>) <SEP> (in <SEP> sec)
<tb><SEP> perfume <SEP> 29.6 <SEP> parts <SEP> in <SEP> weight
<tb> Water <SEP> permuted <SEP> 69
This formulated emulsion has 45.9% of dry matter and a median diameter (d50) of 1.3 Clam.

The composition of this emulsion corresponds to a dry weight ratio AtB of 51/49, in which ratio A and B have the following meanings:
A = (perfume + FP940 protein emulsifier) /% total dry matter X 100
B = protein FP940 matrix /% total dry matter X100 - Drying of the emulsion formulated
This emulsion is then dried by lyophilization. The granules resulting from this treatment have the following composition

<tb> FP940 <SEP>(SEP>SEP> Protein <SEP>SEP>SEP>SEP>SEP>SEP>SEP>SEP><SEP><SEP><SEP> Hydrolysate <SEP> in <SEP> weight
<tb> lower <SEP> than <SEP> 5%, <SEP> of <SEP> Protein <SEP> Technologies <SEP> International <SEP>)
<tb> (emulsifier)
<tb> perfume <SEP> 50 <SEP> parts <SEP> in <SEP> weight
<tb> FP940 <SEP>(SEP>SEP> Protein <SEP>SEP>SEP>SEP>SEP>SEP>SEP>SEP>SEP><SEP><SEP> in <SEP> weight
<tb> lower <SEP> than <SEP> 5%, <SEP> of <SEP> Protein <SEP> Technologies <SEP> International <SEP>)
<tb> (matrix)
<Tb>
The redispersion of the granules in the water gives again a perfume emulsion of fairly uniform particle size distribution and median diameter (d50) of 2.5 Clam.

Example 2: Production of a perfume emulsion in an ethoxylated fatty alcohol
A composition mixture of 20.0% Parfum 1.2% Synperonic Al 1 (ethoxylated fatty alcohol C13-C15 containing 10E average) is prepared. 78.8% Permuted water having a solids content of 21.2%.

The mixture is first pre-emulsified with ultra turrax T25 for 1 minute at 9500 rpm.

The emulsion itself is carried out by means of a microfluidizer (Ml 100 of
Microfluidics) under the following conditions: Pressure: 500 bar - 3 passes through the microfluidizer - Cold water bath at the microfluidizer outlet.

The emulsion obtained has a polydisperse granulometry with a median diameter (d50) of 0.7 mm.

Incorporation of the Polyacrylate Acid Matrix

The matrix incorporated in the emulsion is a polyacrylic acid with a molar mass of 2000 g / mol of Bevaloid.

The composition of the emulsion formulated is as follows: 18.6% Perfume 1.1% Synpernonic Ai 1 (emulsifier) 4.9% Polyacrylic acid Mw = 2000 g / mol (matrix) 75.4% Permuted water
Its dry extract is 24.6%.

The composition of the emulsion thus formulated corresponds to a dry weight ratio
A / B 80/20 with: A = Fragrance + Synperonic All /% total dry matter X 100
B = Polyacrylic acid / total dry matter content X 100 - Drying of the emulsion formulated
This formulation is then dried by freeze-drying. The granules resulting from this treatment have the following composition: 75.6% Fragrance 4.5% Synperonic Ai 1 (emulsifier or dispersant) 19.9% Polyacrylic acid (matrix)
The redispersion of the granules in the water gives again a polydisperse granulometric distribution perfume emulsion with a median diameter (d50) of 1.5 mm.

 Depending on the storage conditions, it may be necessary to add a silica in the following proportions: 66.70% Perfume 4.00% Synperonic All (emulsifier or dispersant) 17.55% Polyacrylic acid (matrix) 11.75% Silica Tixosil T38A (Rhone - Poulenc)

Claims (20)

 1) Water-dispersible granules, comprising - at least one hydrophobic perfume (P), in the form of droplets, finely divided in and encapsulated by a water-soluble or water-dispersible solid organic matrix (MO). chosen from  the polypeptides (PP) of plant or synthetic origin that are water-soluble or water-dispersible  polyelectrolytes (PE) belonging to the family of weak polyacids  water-soluble or water-dispersible oses, osides or polyholosides (O)  * or their mixtures. and at least one emulsifying agent (AE) at the droplet / matrix interface.  2) Granules according to claim 1, characterized in that they comprise - from 5 to 90%, preferably from 25 to 70% of their weight, of perfume (P), from 5 to 90%, preferably from 25 to 70% of their weight, of water-soluble or water-dispersible organic matrix (OM), of 0.02 to 20%, preferably of 0.1 to 10% of their weight, of emulsifying agent (AE), said percentages being expressed by weight of dry matter.  3) Granules according to claim 1) or 2), characterized in that the droplets have an average particle size of the order of 0.1 to 10, ut, preferably of the order of 0.2 to 5 ut.  4) Granules according to any one of claims 1) to 3), characterized in that the perfume (P) comprises natural or synthetic odorants based on aliphatic or aromatic ketones, aliphatic or aromatic aldehydes, condensation products of aldehydes and amines. aromatic or aliphatic lactones, aromatic or aliphatic ethers or esters, aliphatic alcohols, saturated or unsaturated linear, cyclic or aromatic, terpenic, polynuclear or non-polymeric hydrocarbons.  5) Granules according to any one of claims 1) to 4), characterized in that the polypeptides (PP) are chosen from - homopolymers or synthetic copolymers derived from the polycondensation of amino acids or precursors of amino acids , preferably aspartic and / or glutamic acid or their precursors, and hydrolysis - proteins of vegetable origin, in particular soya or wheat, preferably hydrolysed with a degree of hydrolysis of less than 40%  6) Granules according to any one of claims 1) to 4), characterized in that the polyelectrolytes (PE) are selected from low polyacids of molecular weight less than 20000 g / mol, preferably between 1000 and 5000 g / mol.  7) Granules according to any one of claims 1) to 6), characterized in that the emulsifying agent (AE) is nonionic, anionic, cationic or amphoteric.  8) Granules according to claim 7, characterized in that the emulsifying agent (AE) is nonionic and selected from polyoxyalkylenated surfactants.  9) Granules according to claim 7, characterized in that the emulsifying agent (AE) is amphoteric and selected from proteins and protein hydrolysates.  10) A process for the preparation in two steps of dispersible granules in water, comprising: at least one hydrophobic perfume (P), in the form of droplets, finely divided in and encapsulated by a solid organic water-soluble or water-dispersible (OM) matrix, chosen from  the polypeptides (PP) of plant or synthetic origin that are water-soluble or water-dispersible  polyelectrolytes (PE) belonging to the family of weak polyacids  * the dares. water-soluble or water-dispersible osides or polyholosides (O)  * or their mixtures. and at least one emulsifying agent (AE) at the droplet / matrix interface. the first step of preparing an emulsion in water comprising at least one hydrophobic perfume (P), at least one emulsifying agent (AE) and said water-soluble or water-dispersible organic matrix (OM), the second step of drying said emulsion until forming a granule.  11) Process according to claim 10, characterized in that the relative amounts of perfume (P), emulsifying agent (AE) and water-soluble or water-dispersible organic matrix (MO) used are such that said emulsion, expressed in dry, comprises 5 to 90%, preferably 25 to 70% of their weight. hydrophobic perfume (P), 5 to 90%, preferably 25 to 70% of their weight. of water-soluble or water-dispersible organic matrix (OM), from 0.02 to 20%, preferably from 0.1 to 10% by weight, of emulsifying agent (AE), said percentages being expressed by weight of dry matter.  12) Process according to claim 10) or 11), characterized in that the amount of dry matter of the emulsion is between 10 and 70% by weight and preferably between 20 and 60% by weight  13) Process according to any one of claims 10) to 12), characterized in that the average particle size of the emulsion is between 0.1 and 10 microns and preferably between 0.2 and 5 microns.  14) Process according to any one of claims 10) to 13), characterized in that the perfume (P), the emulsifying agent (AE) and the water-soluble or water-dispersible organic matrix (MO) are chosen from those mentioned in the claims 4), 5), 6), 7), 8) or 9).  15) Process according to any one of claims 10) to 14), characterized in that the drying of the dispersion is carried out by lyophilization or by atomization.  16) Process according to any one of claims 10) to 15), characterized in that anti-caking agents are introduced during the drying step.  17) Use in the cosmetic compositions or detergent compositions for washing laundry, granules according to claims 1) to 9) or obtained according to the process of claims 10) to 16) as a perfuming agent.  18) Cosmetic compositions comprising said granules forming the subject of claims 1) to 9) or obtained according to the method forming the subject of claims 10) to 16).  19) Detergent compositions for washing laundry comprising said granules according to claims 1) to 9) or obtained according to the method of claims 10) to 16).  20) Use according to claim 17) or detergent compositions according to claim 19, characterized in that the granules are used in a proportion of approximately 0.01 to 0.5%, preferably 0.05 to 0.2. % with respect to said detergent compositions.