DETERGENT COMPOSITIONS HAVING IMPROVED OLFACTORY PROPERTIES

Abstract

A composition having at least one composition for washing and/or care of fabrics, and at least one solid microcapsule having a mean diameter between 1 μm and 30 μm, with a core consisting of a composition C1 comprising at least one perfuming agent, and a solid crosslinked-polymer envelope totally encapsulating the core at its circumference, wherein the solid envelope comprises a crosslinked polymer obtained by polymerizing at least one monomer or polymer having at least one reactive moiety selected from the group consisting of acrylate, methacrylate, vinyl ether, N-vinyl ether, vinyl ester, thiolene, maleate, epoxy, siloxane, amine, lactone, phosphate, and carboxylate moieties, and wherein the thickness of the solid envelope is between 0.1 μm and 20 μm.

Claims

1. A composition comprising: at least one composition for washing and/or care of fabrics, and at least one solid microcapsule having a mean diameter between 1 μm and 30 μm, comprising: a core consisting of a composition C1 comprising at least one perfuming agent, wherein the composition C1 is in the form of an emulsion, and a solid crosslinked-polymer envelope totally encapsulating the core at its circumference, wherein the solid envelope comprises a crosslinked polymer obtained by polymerizing at least one monomer or polymer having at least one reactive moiety selected from the group consisting of acrylate, methacrylate, vinyl ether, N-vinyl ether, vinyl ester, thiolene, maleate, epoxy, siloxane, amine, lactone, phosphate, and carboxylate moieties, and wherein the thickness of the solid envelope is between 0.1 μm and 20 μm.

2. The composition according to claim 1, comprising solid microcapsules, wherein each of the solid microcapsules is as defined in claim 1, and wherein the standard deviation of the microcapsule diameter distribution is less than 50%, or less than 1 μm.

3. The composition according to claim 1, wherein the composition C1 of the core of the solid microcapsules comprises at least 20 wt % perfuming agent relative to the total weight of the composition C1.

4. The composition according to claim 1, wherein the composition C1 further comprises at least one aqueous gellant, preferably selected from the group consisting of cellulose derivatives, polyacrylates, polyvinylpyrrolidone polyacrylamide and derivatives thereof, polyvinyl alcohol and derivatives thereof, poly(ethylene glycol), poly(propylene glycol) and derivatives thereof, polysaccharides, protein-derivatives, polyurethanes and derivatives thereof, and clays and silicates.

5. The composition according to claim 4, wherein the composition C1 is in the form of an emulsion comprising a continuous phase in the form of an aqueous gel.

6. The composition according to claim 1, wherein the crosslinked polymer is obtained by polymerization from a monomer or polymer selected from aliphatic or aromatic esters or polyesters, urethanes or polyurethanes, anhydrides or polyanhydrides, saccharides or polysaccharides, ethers or polyethers, amides or polyamides, and carbonates or polycarbonates, wherein the monomers or polymers further include at least one reactive moiety selected from the group consisting of acrylate, methacrylate, vinyl ether, N-vinyl ether, vinyl ester, thiolene, maleate, epoxy, siloxane, amine, lactone, phosphate, and carboxylate moieties.

7. The composition according to claim 1, wherein the crosslinked polymer is selected from the group consisting of crosslinked polymers, crosslinked polyepoxys, and crosslinked polyurethanes.

8. The composition according to claim 1, wherein the crosslinked polymer of the envelope of the solid microcapsules is obtained by polymerizing a composition C2 comprising at least one monomer or polymer having at least one reactive moiety as defined in claim 1, at least one crosslinking agent, and optionally at least one crosslinking photoinitiator or catalyst.

9. The composition according to claim 1, wherein the solid microcapsules are obtained by a method comprising the following steps: a) adding, whilst stirring, a composition C1 as defined in claim 1, to a polymer composition C2, wherein the compositions C1 and C2 are not miscible, wherein the viscosity of the composition C2 is between 500 mPa.Math.s and 100 000 mPa.Math.s at 25° C., and is preferably greater than the viscosity of composition C1, wherein the composition C2 comprises: at least one monomer or polymer having at least one reactive moiety as defined in claim 1, at least one crosslinking agent, and optionally at least one crosslinking photoinitiator or catalyst, resulting in an emulsion (E1) comprising drops of composition C1 dispersed in the composition C2; b) adding, whilst stirring, the emulsion (E1) to a composition C3, wherein the compositions C2 and C3 are not miscible, wherein the viscosity of the composition C3 is between 500 mPa.Math.s and 100 000 mPa.Math.s at 25° C., and is preferably greater than the viscosity of the emulsion (E1), resulting in a double emulsion (E2) comprising drops dispersed in the composition C3; c) applying a shear stress to the emulsion (E2), resulting in a double emulsion (E3) comprising drops of controlled size dispersed in the composition C3; and d) polymerizing the composition C2, resulting in solid microcapsules dispersed in the composition C3.

10. The use of a composition according to claim 1 for washing and/or care of fabrics.

Description

EXAMPLES

Example 1

Preparation of the Microcapsules

[0322] A mechanical stirrer (Ika Eurostar 20) equipped with a saw tooth propeller is used to carry out all stirring steps.

Preparation of Composition C1

[0323]

TABLE-US-00001 TABLE 1 Mass Proportion Raw materials (g) (%) Phase A Romance 0330 (IFF) 7.84 40 Neobee M5 (Stepan) 1.96 10 Pluronic L81 (Sigma Aldrich) 0.2 1 Phase B Tween 80 (Sigma Aldrich) 0.4 2 Deionized water 9.2 47 Total 19.6 100

[0324] The ingredients of phase A are stirred together at 300 rpm until homogenization. To prepare phase B, Tween 80 is gradually added to distilled water with stirring at 2000 rpm until homogenization. Phase A is then gradually added to phase B with stirring at 2000 rpm. The components are stirred for a 2 min, then sonicated (SFX 550, Branson) in an ice bath for 1.5 min (pulse 10 s/5 s) at 40% amplitude.

[0325] Following coiling, 1.4 g of Aculyn 44N gellant (Dow) is added to the mixture with stirring at 200 rpm until gelation in order to obtain composition C1.

Preparation of the First Emulsion (E1)

[0326]

TABLE-US-00002 TABLE 2 % in % in Raw materials composition E1 Composition C1 — 50 Composition C2 Aliphatic epoxy acrylate 78.6 50 oligomer (Genomer 2312, Rahn) Propoxylated glyceryl 20.4 triacrylate oligomer (SR9020, Sartomer) Photoinitiator (Darocure 1 1173, Sigma Aldrich) Total 100 100

[0327] The composition C1 is gradually added to the composition C2 with stirring at 300 rpm.

Preparation of the Second Emulsion (E2)

[0328]

TABLE-US-00003 TABLE 3 % in % in Raw materials composition E2 Emulsion E1 — 5 Composition C3 Sodium alginate (Sigma 11 95 Aldrich) Deionized water 89 Total 100 100

[0329] The composition C3 is stirred at 1 000 rpm until complete homogenization, then allowed to rest for 1 h at room temperature (RT).

[0330] The first emulsion (E1) is then gradually added to the composition C3 with stirring at 2000 rpm. Thus, the second emulsion (E2) is obtained.

Adjustment of the Size of the Second Emulsion

[0331] The second polydispersed emulsion (E2) resulting from the foregoing step is stirred at 2000 rpm for 3 min. This results in a monodispersed emulsion (E2).

Crosslinking of the Envelope of the Capsules

[0332] The second monodispersed emulsion (E3), obtained in the previous step, is irradiated for 10 min using a UV light source (Dymax LightBox ECE 2000) with a maximum light intensity of 0.1 W/cm.sup.2 at a wavelength of 365 nm.

[0333] The resultant microcapsules have an average size of 9.5 μm, and their size distribution has a standard deviation of 3.1 μm, i.e. 33%.

[0334] The resultant microcapsules are subjected to 3 successive dilution cycles with distilled water and centrifuged in order to produce a suspension of microcapsules in distilled water containing 50 mass % microcapsules.

Example 2

Biodegradability Test

[0335] The biodegradability of the microcapsules prepared according to Example 1 is measured according to OECD guideline 301 A, available at the OECD website at the following URL: https://www.oecd-ilibrary.org/fr/environment/essai-n-301-biodegradabilite-facile_9789264070356-fr.

[0336] In brief, the microcapsule suspensions are diluted with distilled water at a concentration such that their concentration in dissolved organic carbon (DOC) is between 10 and 40 mg DOC/L, and incubated with a seeding from an urban organic water treatment plant in a lightproof chamber with stirring at 22° C. The DOC analysis is carried out regularly, and a biodegradation rate of 70% in 28 days is found.

[0337] The microcapsules prepared according to Example 1 are thus biodegradable.

Example 3

Preparation of a Formula for a Main Wash Product

[0338] The following formula for a main wash product is provided:

TABLE-US-00004 TABLE 4 % in Raw materials composition Biodegradable anionic Sodium dodecylbenzene 9.6 surfactant sulphonate (Sigma Aldrich) Biodegradable anionic Sodium dodecyl sulphate 5 surfactant (Sigma Aldrich) Biodegradable nonionic C12-C15 ethoxylated 5 surfactant alcohols (Tomadol 25-7, Evonik) pH adjuster Sodium hydroxide 2.5 Detergent additive Sodium citrate (Sigma 2 Aldrich) Antiredeposition agent Polyacrylate (Acusol 445N, 1 Dow) Biodegradable optical 4,4′-distyryl biphenyl 0.05 brightener derivative (Tinopal CBS-X, BASF) Solvent Deionized water 72.35 Total 100

[0339] Two samples are prepared from this formula containing the same concentration of Romance 0330 perfume: Sample LP1 containing 5 mass % of microcapsules prepared according to Example 1 and sample LP2 containing 0.97 mass % Romance 0330 perfume.

Example 4

Formula for Fabric Softening Rinse

[0340] The following formula for a fabric softener is provided:

TABLE-US-00005 TABLE 5 % in Raw materials composition Biodegradable cationic TEA quat diester 16.67 softener compound (Stepantex VT-90, Stepan) Detergent additive Sodium chloride 0.15 (Sigma Aldrich) Solvent Deionized water 73.18 Total 100

[0341] Two samples are prepared from this formula containing the same concentration of Romance 0330 perfume: Sample AD1 containing 5 mass % of microcapsules prepared according to Example 1 and sample AD2 containing 0.97 mass % Romance 0330 perfume.

Example 5

Preparation of Washed Cotton Fabric Sample

[0342] 10 g of one of the products produced according to Example 3 or 4 is mixed with 1 L deionized water. 5 6×10 cm cotton fabric samples are stirred for 5 min in the resultant solution, drained, then stirred for 2 min in 1 L deionized water, drained, and then dried in open air for 12 h.

Example 6

Sensory Test After 12 Hours

[0343] Cotton fabric samples prepared according to Example 5 are evaluated by a panel of 5 persons according to a scent intensity scale from 0-5, where 0 represents no scent and 5 an extremely strong scent. Each person has two fabric samples per fabric care product sample: One is evaluated intact, the other is evaluated after rubbing the fabric against itself. The intensities perceived for each sample (mean±SD) are shown in the table below:

TABLE-US-00006 TABLE 6 No rubbing After rubbing LP1 1.7 ± 0.6 3.9 ± 0.2 LP2 2.5 ± 0.3 2.6 ± 0.4 AD1 1.9 ± 0.5 4.0 ± 0.3 AD2 2.7 ± 0.3 2.5 ± 0.5

[0344] These results show the targeting qualities of the microcapsules on fabric fibers with the two types of fabric care product tested. The intensity perceived before rubbing is lower in the samples containing microcapsules because the perfume is confined inside the microcapsules. Under the effect of rubbing, the microcapsules break to release the perfume inside. The intensity perceived following rubbing is thus greater in the samples containing the microcapsules, showing that the quantity of perfume deposited on the fibers of the fabric is greater than that deposited when the perfume is free.

Example 7

Sensory Test After 7 Days

[0345] Samples of cotton fabric prepared according to Example 5 are stored in a non-airtight box for 7 days, then evaluated by a panel of 5 persons according to the protocol described in Example 6. The intensities perceived for each sample (mean±SD) are shown in the table below:

TABLE-US-00007 TABLE 7 No rubbing After rubbing LP1 - 7j 0.6 ± 0.3 2.5 ± 0.6 LP2 - 7j 0.3 ± 0.4 0.6 ± 04  AD1 - 7j 0.5 ± 0.5 1.8 ± 0.6 AD2 - 7j 0.5 ± 0.3 0.4 ± 0.5

[0346] These results show the protection against evaporation provided to the perfume by the microcapsules. Indeed, after rubbing, the intensity perceived is considerably greater when the perfume is encapsulated than when it is free, thus showing that the quantity of perfume remaining on the fabric after 7 days is greater.