DE102017222998A1 - Production process for spherical scented pearls - Google Patents

Abstract

The present invention relates to a process for the preparation of spherical fragrance particles, the fragrance particles thus obtained, as well as their use for fragrancing objects, in particular textile fabrics.

Description

The present invention relates to a process for the preparation of spherical fragrance particles, the fragrance particles thus obtained, as well as their use for fragrancing objects, in particular textile fabrics.

In the use of detergents and cleaners, the consumer not only aims to wash, cleanse or care for the objects to be treated, but also desires that the treated objects, such as textiles, after treatment, for example after washing, smell pleasant. For this reason in particular, most commercially available detergents and cleaners contain fragrances. Most fragrances, however, are volatile. For this reason, when using conventional washing or cleaning agents after use, especially after washing, only a small proportion of the fragrance used remains on the treated object. As a result, often only a faint scent of the treated object, especially the laundry, goes out, which then already weaker after a short time. Thus, the pleasant feeling of freshness of the treated object disappears after a short time.

Often fragrances are used in the form of perfume particles either as an integral part of a washing or cleaning agent, or dosed directly into the washing drum at the beginning of a wash cycle in a separate form. In this way, the consumer can control the fragrance of the laundry to be washed by individual dosage.

Such fragrance particles are usually provided in the form of fragrance-containing enamel bodies. In such processes, only one or more constituents of the shaped body, ie usually the at least one carrier polymer, are first melted and, as required, further constituents are metered into the melt. This is followed by the cooling / transformation of the melt. In particular, the sedimentation of individual components of the melt, however, can lead to disturbances in the pastillation process.

The fragrance particles which can be prepared by such known processes, which usually have a lens shape, are described, for example, in the European patent EP 2 496 679 B1 described.

However, fragrance particles in a spherical or at least approximately spherical shape, ie in spherical form, are particularly aesthetically pleasing. These are not only visually appealing, but can also be dosed well and simply.

The object of the present invention is therefore to provide a method for producing spherical fragrance particles. Surprisingly, it has been shown that spherical fragrance particles can be obtained by dropping a melt into a cooling bath.

1. a) Herstellen einer Schmelze, umfassend wenigstens einen Träger sowie wenigstens einen Duftstoff und anschließendes
2. b) Vertropfen der Schmelze in ein Kühlbad, und
3. c) Abkühlen der Schmelze, wodurch diese zu festen, harten Partikeln erstarrt.

In a first embodiment, the object underlying the present invention is therefore achieved by a process for producing water-soluble spherical fragrance particles comprising:

1. a) producing a melt, comprising at least one carrier and at least one perfume and then
2. b) dripping the melt into a cooling bath, and
3. c) cooling the melt, whereby it solidifies to solid, hard particles.

Drip methods are known from other fields of technology, such as pharmacy. However, a melt which comprises a carrier and at least one perfume has not yet been described with regard to dripping methods for the production of fragrance particles in the field of textile care. It was also not to be expected that can be obtained by the inoculation of spherical fragrance particles, since due to the presence of the fragrance a pain with low viscosity at the same time the lowest possible melting temperature of the carrier or low temperature of the melt is needed.

Furthermore, the present invention is directed to fragrance particles obtained by the process according to the invention. In a further aspect, the present invention is directed to the use of corresponding spherical fragrance particles for fragrancing objects, in particular textile fabrics.

These and other aspects, features, and advantages of the invention will become apparent to those skilled in the art from a study of the following detailed description and claims. Any feature of one aspect of the invention may be employed in any other aspect of the invention. Further, it is to be understood that the examples contained herein are intended to describe and illustrate the invention, but not to limit it, and in particular that the invention is not limited to these examples.

All percentages are by weight, unless otherwise stated, and are in each case based on the stated composition. Numeric ranges indicated in the format "from x to y" include the stated values x and y. If more preferred numeric ranges are specified in this format, it is It goes without saying that all areas that result from the combination of the various endpoints are also recorded.

"At least one" or "at least one" as used herein refers to 1 or more, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or more. In particular, this indication refers to the type of agent / compound and not the absolute number of molecules. "At least one perfume" therefore means, for example, that at least one type of perfume is detected, as well 2 . 3 or more different types of fragrances may be included.

"Water-soluble" as used herein means a solubility in water at 20 ° C of at least 1 g / L, preferably at least 10 g / L, more preferably at least 50 g / L.

"Water-dispersible" as used herein means that the corresponding molecule can be dispersed in water at 20 ° C by known methods.

"About" or "approximately" as used herein in connection with a numerical value means the numerical value ± 10%, preferably ± 5%.

"Melt body" as used herein preferably refers to a solid that is water soluble or water dispersible and substantially nonporous at standard conditions (20 ° C, 1013 mbar) and obtainable by cooling from the melt dispersions or melts described herein is. For the purposes of the present invention, "melt" does not necessarily mean a melt in the thermodynamic sense. So it is generally a flowable at elevated temperature mass, which goes into a solid state at ambient temperature.

The melt comprises according to the invention at least one perfume. This may be an encapsulated perfume or an unencapsulated perfume, for example a free perfume oil. It is also possible according to the invention for both an encapsulated fragrance and an unencapsulated fragrance to be present in the melt and thus also in the resulting spherical fragrance particle. For the purposes of the present invention, "perfume" includes both the perfume itself and perfume precursors or perfume precursors, both in encapsulated and non-encapsulated form.

According to the invention, the melt may contain as perfume in a microcapsule an encapsulated perfume oil, an encapsulated perfume or an encapsulated perfume precursor or mixtures thereof. According to the invention, in addition to the microcapsules, it may also have a perfume or a perfume precursor or a perfume oil which is incorporated in the carrier in an unencapsulated form. As a result, the fragrance experience of the agent according to the invention can be further enhanced and the intensity of the scenting of the object can be improved.

In general, a fragrance is a chemical stimulating the sense of smell. In order to stimulate the sense of smell, the chemical substance should be at least partially redistributable in the air, i. the perfume should be at least slightly volatile at 25 ° C. If the fragrance is now very volatile, the odor intensity sounds quickly again. However, with lower volatility the odor impression is more sustainable, i. he does not disappear so fast. In one embodiment, therefore, the perfume has a melting point in the range of -100 ° C to 100 ° C, preferably from -80 ° C to 80 ° C, more preferably from -20 ° C to 50 ° C, especially of 30 ° C to 20 ° C. In a further embodiment, the perfume has a boiling point ranging from 25 ° C to 400 ° C, preferably from 50 ° C to 380 ° C, more preferably from 75 ° C to 350 ° C, especially from 100 ° C to 330 ° C is located.

Overall, a chemical substance should not exceed a certain molecular weight to act as a fragrance, since too high molecular weight, the required volatility can no longer be ensured. In a preferred embodiment, the fragrance has a molecular weight of 40 to 700 g / mol, more preferably 60 to 400 g / mol.

The smell of a fragrance is perceived by most people as pleasant and often corresponds to the smell of, for example, flowers, fruits, spices, bark, resin, leaves, grasses, mosses and roots. Thus, fragrances can also be used to superimpose unpleasant odors or even to provide a non-smelling substance with a desired odor. As fragrances, individual fragrance compounds, for example, the synthetic products of the ester type, ethers, aldehydes, ketones, alcohols and hydrocarbons can be used.

Fragrance compounds of the aldehyde type are, for example, adoxal (2,6,10-trimethyl-9-undecenal), anisaldehyde (4-methoxybenzaldehyde), cymal (3- (4-isopropyl-phenyl) -2-methylpropanal), ethylvanillin, florhydral ( 3- (3-isopropylphenyl) butanal), helional (3- (3,4-methylenedioxyphenyl) -2-methylpropanal), heliotropin, hydroxycitronellal, lauraldehyde, lyral (3- and 4- (4-hydroxy-4-methylpentyl) - 3-cyclohexene-1-carboxaldehyde), methylnonylacetaldehyde, lilial (3- (4-tert-butyl) Butylphenyl) -2-methylpropanal), phenylacetaldehyde, undecylenealdehyde, vanillin, 2,6,10-trimethyl-9-undecenal, 3-dodecene-1-al, alpha-n-amylcinnamaldehyde, melonal (2,6-dimethyl-5- heptenal), 2,4-dimethyl-3-cyclohexene-1-carboxaldehyde (Triplal), 4-methoxybenzaldehyde, benzaldehyde, 3- (4-tert-butylphenyl) -propanal, 2-methyl-3- (para-methoxyphenyl ) propanal, 2-methyl-4- (2,6,6-timethyl-2 (1) -cyclohexen-1-yl) butanal, 3-phenyl-2-propenal, cis- / trans-3,7-dimethyl- 2,6-octadiene-1-al, 3,7-dimethyl-6-octene-1-al, [(3,7-dimethyl-6-octenyl) oxy] acetaldehyde, 4-isopropylbenzylaldehyde, 1,2,3, 4,5,6,7,8-Octahydro-8,8-dimethyl-2-naphthaldehyde, 2,4-dimethyl-3-cyclohexene-1-carboxaldehyde, 2-methyl-3- (isopropyl-1-phenyl) propanal, 1 Decanal, 2,6-dimethyl-5-heptenal, 4- (tricyclo [5.2.1.0 (2,6)] decylidene-8) -butanal, octahydro-4,7-methane-1H-indenecarboxaldehyde, 3-ethoxy 4-hydroxybenzaldehyde, para-ethylalpha, alpha-dimethylhydrocinnamaldehyde, alpha-methyl-3,4- (methylenedioxy) -hydrocinnamaldehyde, 3,4-methylenedioxybenzaldehyde, alpha-nH exylcinnamaldehyde, m-cymene-7-carboxaldehyde, alpha-methylphenylacetaldehyde, 7-hydroxy-3,7-dimethyloctanal, undecenal, 2,4,6-trimethyl-3-cyclohexene-1-carboxaldehyde, 4- (3) (4- Methyl 3-pentenyl) -3-cyclohexene carboxaldehyde, 1-dodecanal, 2,4-dimethylcyclohexene-3-carboxaldehyde, 4- (4-hydroxy-4-methylpentyl) -3-cyclohexene-1-carboxaldehyde, 7-methoxy-3 , 7-dimethyloctan-1-al, 2-methyl undecanal, 2-methyldecanal, 1-nonanal, 1-octanal, 2,6,10-trimethyl-5,9-undecadienal, 2-methyl-3- (4- tert-butyl) propanal, dihydrocinnamaldehyde, 1-methyl-4- (4-methyl-3-pentenyl) -3-cyclohexene-1-carboxaldehyde, 5- or 6-methoxy-hexahydro-4,7-methanindan-1 or-2 -carboxaldehyde, 3,7-dimethyloctan-1-al, 1-undecanal, 10-undecene-1-al, 4-hydroxy-3-methoxybenzaldehyde, 1-methyl-3- (4-methylpentyl) -3-cyclohexenecarboxaldehyde, 7 Hydroxy-3J-dimethyl-octanal, trans-4-decenal, 2,6-nonadienal, para-tolylacetaldehyde, 4-methylphenylacetaldehyde, 2-methyl-4- (2,6,6-trimethyl-1-cyclohexene-1 yl) -2-butenal, ortho-methoxycinnamaldehyde, 3,5,6-trimethyl-3-cy clohexene carboxaldehyde, 3J-dimethyl-2-methylene-6-octenal, phenoxyacetaldehyde, 5,9-dimethyl-4,8-decadienal, peonyaldehyde (6,10-dimethyl-3-oxa-5,9-undecadiene-1 al), hexahydro-4,7-methanindane-1-carboxaldehyde, 2-methyloctanal, alpha-methyl-4- (1-methylethyl) benzeneacetaldehyde, 6,6-dimethyl-2-norpinen-2-propionaldehyde, para-methylphenoxyacetaldehyde, 2-methyl-3-phenyl-2-propen-1-al, 3,5,5-trimethylhexanal, hexahydro-8,8-dimethyl-2-naphthaldehyde, 3-propyl-bicyclo- [2.2.1] -hept- 5-en-2-carbaldehyde, 9-decenal, 3-methyl-5-phenyl-1-pentanal, methylnonylacetaldehyde, hexanal and trans-2-hexenal.

For example, ketone-type perfume compounds are methyl-beta-naphthyl ketone, muskedanone-1-one (1,2,3,5,6,7-hexahydro-1,1,2,3,3-pentamethyl-4H-inden-4-one), Tonalid (6-acetyl-1,1,2,4,4,7-hexamethyltetralin), alpha-damascone, beta-damascone, delta-damascone, iso-damascone, damascenone, methyldihydrojasmonate, menthone, carvone, camphor, koavon (3 , 4,5,6,6-pentamethylhept-3-en-2-one), fenchone, alpha-ionone, beta- lonone, gamma-methyl-ionone, fleuramon (2-heptylcyclopentanone), dihydrojasmon, cis-jasmone , Iso-E-Super (1- (1,2,3,4,5,6J, 8-octahydro-2,3,8,8-tetramethyl-2-naphthalenyl) -ethan-1-one (and isomers) ), Methyl cienyl ketone, acetophenone, methyl acetophenone, para-methoxy acetophenone, methyl beta-naphthyl ketone, benzyl acetone, benzophenone, para-hydroxyphenyl butanone, celery ketone (3-methyl-5-propyl-2-cyclohexenone), 6-isopropyldecahydro-2-naphthone , Dimethyloctenone, Frescomenthe (2-butan-2-yl-cyclohexan-1-one), 4- (1-ethoxyvinyl) -3,3,5,5-tetramethylcyclohexanone, methylheptenone, 2- (2- (4-methyl) 3-cyclohe xen-1-yl) propyl) cyclopentanone, 1- (p-menthene-6 (2) yl) -1-propanone, 4- (4-hydroxy-3-methoxyphenyl) -2-butanone, 2-acetyl-3, 3-dimethylnorbornane, 6,7-dihydro-1,1,2,3,3-pentamethyl-4 (5H) -indanone, 4-damascol, dulcinyl (4- (1,3-benzodioxol-5-yl) butane 2-one), hexalon (1- (2,6,6-trimethyl-2-cyclohexene-1-yl) -1,6-heptadien-3-one), isocyclone E (2-acetonaphthone-1,2,3, 4,5,6,7,8-octahydro-2,3,8,8-tetramethyl), methylnonyl ketone, methylcyclocitron, methyllavedelketone, orivone (4-tert-amylcyclohexanone), 4-tert-butylcyclohexanone, dolphon (2- pentyl cyclopentanone), Muscon (CAS 541-91-3), neobutenone (1- (5,5-dimethyl-1-cyclohexenyl) pent-4-en-1-one), Plicaton (CAS 41724-19-0) , Velouton (2,2,5-trimethyl-5-pentylcyclopentan-1-one), 2,4,4,7-tetramethyl-oct-6-en-3-one and tetrameran (6,10-dimethylundecene-2-one) on).

Fragrance compounds of the alcohol type are, for example, 10-undecen-1-ol, 2,6-dimethylheptan-2-ol, 2-methylbutanol, 2-methylpentanol, 2-phenoxyethanol, 2-phenylpropanol, 2-tert. Butycyclohexanol, 3,5,5-trimethylcyclohexanol, 3-hexanol, 3-methyl-5-phenyl-pentanol, 3-octanol, 3-phenyl-propanol, 4-heptenol, 4-isopropylcyclohexanol, 4-tert-butycyclohexanol , 6,8-dimethyl-2-nonanol, 6-nonene-1-ol, 9-decene-1-ol, α-methylbenzyl alcohol, α-terpineol, amyl salicylate, benzyl alcohol, benzyl salicylate, β-terpineol, butyl salicylate, citronellol , Cyclohexyl salicylate, decanol, di-hydromyrcenol, dimethylbenzylcarbinol, dimethylheptanol, dimethyloctanol, ethyl salicylate, ethylvaniline, eugenol, farnesol, geraniol, heptanol, hexyl salicylate, isoborneol, isoeugenol, isopulegol, linalool, menthol, myrtenol, n-hexanol, nerol, nonanol, octanol , p-menthan-7-ol, phenylethyl alcohol, phenol, phenyl salicylate, tetrahydrogeraniol, tetrahydrolinalool, thymol, trans-2-cis-6-nonadicnol, trans-2-nonen-1-ol, tra ns-2-octenol, undecanol, vanillin, champiniol, hexenol and cinnamyl alcohol.

Fragrance type compounds of the ester type include, for example, benzyl acetate, phenoxyethyl isobutyrate, p-tert-butylcyclohexyl acetate, linalyl acetate, dimethylbenzylcarbinylacetate (DMBCA), Phenylethyl acetate, benzyl acetate, ethylmethylphenyl glycinate, allyl cyclohexyl propionate, styrallyl propionate, benzyl salicylate, cyclohexyl salicylate, floramate, melusate and jasmacyclate.

Ethers include, for example, benzyl ethyl ether and ambroxan. The hydrocarbons mainly include terpenes such as limonene and pinene.

Preference is given to using mixtures of different fragrances which together produce an attractive fragrance. Such a mixture of perfumes may also be referred to as perfume or perfume oil. Such perfume oils may also contain natural perfume mixtures as are available from plant sources.

Fragrances of plant origin include essential oils such as angelica root oil, aniseed oil, arnica blossom oil, basil oil, bay oil, champacilla oil, citrus oil, fir pine oil, pinecone oil, elemi oil, eucalyptus oil, fennel oil, pine needle oil, galbanum oil, geranium oil, ginger grass oil, guaiac wood oil, gurdy balm oil, helichrysum oil, Ho oil , Ginger oil, iris oil, jasmine oil, cajeput oil, calamus oil, chamomile oil, camphor oil, kanaga oil, cardamom oil, cassia oil, pine oil, copaiba balsam, coriander oil, spearmint oil, caraway oil, cumin oil, labdanum oil, lavender oil, lemongrass oil, lime blossom oil, lime oil, tangerine oil, lemon balm oil, mint oil, musk kernel oil , Muscatel oil, Myrrh oil, Clove oil, Neroli oil, Niaouli oil, Olibanum oil, Orange blossom oil, Orange peel oil, Origanum oil, Palmarosa oil, Patchouli oil, Peru balsam oil, Petitgrain oil, Pepper oil, Peppermint oil, Pimento oil, Pine oil, Rose oil, Rosemary oil, Sage oil, Sandalwood oil, Celery oil, Spik oil, Star anise oil, turpentine oil, thuja oil, thyme oil, verbena oil, vetiver oil, juniper berry oil, wormwood oil, wintergreen oil, ylang-ylang oil, hyssop oil, cinnamon oil, cinnamon oil, lemon oil, lemon oil and cypress oil and ambrettolide, ambroxan, alpha-amylcinnamaldehyde, anethole, anisaldehyde, Anisalcohol, anisole, methyl anthranilate, acetophenone, benzylacetone, benzaldehyde, ethyl benzoate, benzophenone, benzyl alcohol, benzyl acetate, benzyl benzoate, benzyl formate, benzyl valerate, borneol, bornyl acetate, Boisambrene forte, alpha-bromostyrene, n-decyl aldehyde, n-dodecyl aldehyde, eugenol, eugenol methyl ether, eucalyptol , Famesol, fenchone, fenchyl acetate, geranyl acetate, geranyl formate, heliotropin, heptincarboxylic acid methyl ester, heptaldehyde, hydroquinone dimethyl ether, hydroxycinnamaldehyde, hydroxycinnamyl alcohol, indole, iron, isoeugenol, isoeugenol methyl ether, isosafrole, jasmone, camphor, Karvakrol, Karvon, p-cresol methyl ether, coumarin, p Methoxyacetophenone, methyl n-amyl ketone, methyl anthranilic acid meth ylester, p-methylacetophenone, methylchavikol, p-methylquinoline, methyl-beta-naphthyl ketone, methyl-n-nonylacetaldehyde, methyl-n-nonyl ketone, muscone, beta-naphthol ethyl ether, beta-naphthol methyl ether, nerol, n-nonyl aldehyde, nonyl alcohol, n-octylaldehyde, p-oxy-acetophenone, pentadecanolide, beta-phenylethyl alcohol, phenylacetic acid, pulegone, safrole, isoamyl salicylate, methyl salicylate, hexyl salicylate, cyclohexyl salicylate, santalol, sandelice, skatole, terpineol, thymes, thymol, troenan, gamma undelactone, vanillin, Veratraldehyde, cinnamaldehyde, cinnamyl alcohol, cinnamic acid, cinnamic acid ethyl ester, cinnamic acid benzyl ester, diphenyloxide, limonene, linalool, linalyl acetate and propionate, melusate, menthol, menthone, methyl-n-heptenone, pinene, phenylacetaldehyde, terpinyl acetate, citral, citronellal, and mixtures thereof.

The fragrances mentioned can be in the form of perfume microcapsules (or also perfume microcapsules) in the melt according to the invention. Likewise, said fragrances may also be present as perfume oil (free fragrance) in a preferred form in addition to the microcapsules.

The proportion of the at least one perfume in the melt is preferably in the range of 0.1 wt .-% to 20 wt .-%, preferably 1 wt .-% to 20 wt .-%, more preferably 1 wt .-% to 15 Wt .-%, in particular 3 wt .-% to 10 wt .-%, based on the total weight of the melt or the fragrance particles.

The microcapsules are microcapsules containing the perfume inside, ie the perfume. The microcapsules may be water-soluble and / or water-insoluble microcapsules. For example, melamine-urea-formaldehyde microcapsules, melamine-formaldehyde microcapsules, urea-formaldehyde microcapsules or starch microcapsules can be used.

The microcapsule in encapsulated form not only the perfume, so the perfume itself have. According to the invention, it can also have a scent precursor. Corresponding precursors or fragrance precursors are those compounds which release the actual fragrance only after chemical conversion / cleavage, typically by the action of light or other ambient conditions, such as pH, temperature, pressure or friction, etc. Such perfume precursors or perfume precursors can be present both in the form of the microcapsule as perfume in the agent according to the invention. Also included in the invention is that the perfume precursor is processed directly in unencapsulated form with the carriers.

The melt further comprises at least one carrier. In a first preferred embodiment, the carrier is a polymer.

The support is preferably selected from polyethylene glycols (PEG), EO / PO block copolymers or highly alkoxylated nonionic surfactants. In a preferred embodiment, the support is a polyethylene glycol, in particular one having a molecular weight of> 4000 g / mol. The molecular weight is the average molar mass. Particularly preferred are polyethylene glycols having an average molar mass in the range of 4000 g / mol to 15000 g / mol. The polyethylene glycol preferably has an average molar mass in the range from 4000 to 9000, preferably in the range from 4500 to 8500, particularly preferably from 5000 to 8000, very particularly preferably from 5500 g / mol to 7000 g / mol.

In a further preferred embodiment, the support is an EO / PO block copolymer. In various embodiments, the at least one block copolymer is characterized by having a melting point of 44 ° C to 120 ° C, preferably 44 ° C to 80 ° C.

EO / PO block copolymers suitable according to the invention are composed of blocks of ethylene oxide (EO) and propylene oxide (PO) units. Preference is given to block copolymers of the formulas HO- (EO) _x (PO) _y (EO) _z -H, HO- (PO) _x (EO) _y (PO) _z -H, HO- (EO) _x (PO) _y (PO) _z -H and HO- (EO) _x (EO) _y (PO) _z -H, in which the indices x, y and z are independently an integer from 5 to 500, preferably 10 to 250, still more preferably 15 to 100. In various embodiments, it is preferred that the EO content in the block copolymer is greater than 50% by weight, preferably greater than 60% by weight, more preferably greater than 70% by weight, most preferably about 80% by weight .-% is. The molecular weight of the PO block is preferably at least 1500 g / mol, particularly preferably 1750 to 3250 g / mol. Melting temperatures typically increase with the molecular weight of the PO block and the proportion of EO.

The block copolymers preferably have number average molecular weights (Mn) <20,000 g / mol, preferably <10,000 g / mol. Particular preference is given to molecular weights (Mn) in the range from 4000 g / mol to 9000 g / mol, in particular 6000 g / mol to 8000 g / mol.

When the term "average molecular weight" is used in this application, these data refer in each case to the number-average molecular weights (Mn), which are calculated mathematically from the OH number according to DIN 53240-1 , in particular DIN 53240-1: 2012-07 , revealed.

Particularly preferred according to the invention are EO-PO block copolymers having a molecular weight Mn of about 8000 g / mol, an EO content of about 80 wt.% And a molar mass of the PO block of at least 1750 g / mol. Such polymers are sold, for example, by the company BASF under the trade name Pluronic ^®. Pluronic ^® PE 6800 and Pluronic ^® F 68 are according to the invention very particularly preferred block copolymers.

In addition to the block copolymer having a melting point> 40 ° C, the melts may optionally contain at least one further EO / PO block copolymer with a melting point ≤40 ° C. The melting point is preferably in the range from 0 ° C to 40 ° C, more preferably from 20 ° C to <40 ° C, in particular in the range from 30 ° C to <40 ° C.

According to the invention suitable EO / PO block copolymers are having a melting point ≤40 ° C are also composed of blocks of ethylene oxide (EO) - and propylene oxide (PO) units. Preference is given to block copolymers of the formulas HO- (EO) _x (PO) _y (EO) _z -H, HO- (PO) _x (EO) _y (PO) _z -H, HO- (EO) _x (PO) _y (PO) _z -H and HO- (EO) _x (EO) _y (PO) _z -H, in which the indices x, y and z are independently an integer from 5 to 500, preferably 10 to 250, still more preferably 15 to 100. In various embodiments, it is preferred that the proportion of EO in the block copolymer is less than 50% by weight, preferably about 40% by weight or less. The molecular weight of the PO block is preferably ≦ 3250 g / mol, for example, 2750 g / mol or less.

Corresponding block copolymers having a melting point ≦ 40 ° C. preferably have number-average molecular weights (Mn) <20,000 g / mol, preferably <10,000 g / mol. Particularly preferred are molecular weights (Mn) in the range of 2000 to 8000, in particular 2000 to 6000 g / mol.

Such polymers are also marketed by BASF under the trade name Pluronic®. Pluronic ^® PE 9400 and Pluronic ^® PE 10400 are particularly preferred according to the invention block copolymers.

Thus, according to the invention, the support may comprise an EO / PO block copolymer or consist of two or more block copolymers.

In a further preferred embodiment, the carrier is a highly alkoxylated nonionic surfactant. The nonionic surfactants used are preferably alkoxylated, advantageously ethoxylated, in particular primary, alcohols having preferably 8 to 18 carbon atoms and on average 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol radical can be linear or preferably methyl-branched in the 2-position or linear and methyl-branched radicals in the mixture can contain, as they are usually present in Oxoalkoholresten. In particular, however, alcohol ethoxylates with linear radicals of alcohols of natural origin having 12 to 18 carbon atoms, for example of coconut, palm, tallow or oleyl alcohol, and on average 2 to 8 EO per mole of alcohol are preferred. Preferred ethoxylated alcohols include, for example, C _12-14 alcohols with 3 EO or 4 EO, C _9-11 n-alcohol with 7 EO, C _13-15 alcohols containing 3 EO, 5 EO, 7 EO or 8 EO , C _12-18 alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C _12-14 - alcohol with 3 EO and C _12-18 -alcohol with 5 EO. The degrees of ethoxylation given represent statistical means which, for a particular product, may be an integer or a fractional number. Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE). In addition to these nonionic surfactants, fatty alcohols with more than 12 EO can also be used. Examples include tallow fatty alcohol with 14 EO, 25 EO, 30 EO or 40 EO.

Another class of preferred nonionic surfactants used either as the sole nonionic surfactant or in combination with other nonionic surfactants are alkoxylated, preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably

The melt usually comprises the carrier in an amount of 95% by weight or less. The proportion of carrier is preferably in the range of 30 to 95 wt .-%, preferably from 40 to 90 wt .-%, for example 45 to 90 wt .-%, each based on the total weight of the melt or the fragrance particles.

As an alternative to the polymeric support materials described above, specific carrier salts may also be used. These specific salts are in particular water-containing salts whose water vapor partial pressure at a certain temperature in the range from 30 to 100 ° C. corresponds to the H ₂ O partial pressure of the saturated solution of this salt.

The fragrance particles as described herein are prepared from a solution of the carrier material in the water / water of crystallization contained in the composition, and for such a solution, the term "melt" is also used to refer to the state to designate, in which the carrier material dissolves by the elimination of water in its own water of crystallization and thus forms a liquid. The term "melt" as used herein thus refers to the liquid state of the composition which results when the temperature is exceeded at which the support material splits off water of crystallization and then dissolves in the water contained in the composition. The corresponding dispersion containing the herein described (solid) substances dispersed in the melt of the carrier material is thus also the subject of the invention. Thus, when reference is made below to the solid, particulate composition, the corresponding melt / melt dispersion from which it is obtainable is always included. Since these do not differ in composition except for the state of matter, the terms are used interchangeably herein.

A preferred support material is characterized in that it is selected from hydrous salts whose water vapor partial pressure at a temperature in the range of 30 to 100 ° C corresponds to the H ₂ O partial pressure of the saturated solution of this salt at the same temperature. As a result, the corresponding hydrous salt, also referred to herein as a "hydrate", dissolves on reaching or exceeding this temperature in its own water of crystallization, thereby changing from a solid to a liquid state of matter. Preferably, the support materials of the invention exhibit this behavior at a temperature in the range of 40 to 90 ° C, more preferably between 50 and 85 ° C, even more preferably between 55 and 80 ° C.

The water-soluble carrier materials from the group of hydrous salts described above include in particular the sodium acetate trihydrate (Na (CH ₃ COO) .3H ₂ O), the Glauber salt (Na ₂ SO ₄ .10H ₂ O) and the trisodium phosphate dodecahydrate (Na ₃ PO ₄ x 12 H ₂ O).

A particularly suitable hydrate is sodium acetate trihydrate (Na (CH ₃ COO) .3H ₂ O), since it dissolves in its own water of crystallization in the particularly preferred temperature range of 55 to 80 ° C, concretely at about 58 ° C. The sodium acetate trihydrate can be used directly as such, but it is alternatively possible to use anhydrous sodium acetate in combination with free water, the trihydrate then forming in situ. In such embodiments, the amount of water used is in less than or more than stoichiometric amount, based on the amount necessary to convert all the sodium acetate to sodium acetate trihydrate, preferably in an amount of at least 60% by weight, preferably at least 70% by weight %, more preferably at least 80%, most preferably 90%, 100% or more by weight of the amount theoretically required to convert all of the sodium acetate to sodium acetate trihydrate (Na (CH 3) 2) ₃ COO) · 3H ₂ O). Particularly preferred is the superstoichiometric use of water. With respect to the compositions according to the invention, this means that when ( anhydrous) sodium acetate is used alone or in combination with a hydrate thereof, preferably the trihydrate, also water is used, the amount of water being at least equal to the amount stoichiometrically necessary to ensure that at least 60% by weight. the total amount of sodium acetate and its hydrates, preferably at least 70% by weight, more preferably at least 80% by weight, even more preferably at least 90% by weight, most preferably at least 100% by weight, in the form of sodium acetate. Trihydrate is present. As already described above, it is particularly preferred that the amount of water exceeds the amount that would theoretically be necessary to convert all of the sodium acetate to the corresponding trihydrate. This means, for example, that a composition containing 50% by weight of anhydrous sodium acetate and no hydrate thereof, at least 19.8% by weight of water (60% of 33% by weight, which would theoretically be necessary to remove all of the sodium acetate into the trihydrate).

All of the embodiments described below can be explicitly combined with both of the aforementioned alternatives.

In various embodiments, the at least one support material from the group of hydrous salts whose water vapor partial pressure at a temperature in the range of 30 to 100 ° C corresponds to the H ₂ O partial pressure of the saturated solution of this salt at the same temperature, used in an amount in that the resulting enamel body contains from 30 to 95% by weight, preferably from 40 to 90% by weight, for example 45 to 90% by weight, based on the total weight of the fragrance particles, of the support material.

The two particularly preferred support materials are polyethylene glycol and sodium acetate trihydrate.

In various embodiments, the melter according to the invention may additionally contain further ingredients which can be used to adjust desired properties of the melt or of the fragrance particles produced therefrom. These substances described below can each be contained individually or in any desired combinations. Thus, for example, the melt may further comprise an adsorber material for receiving a fragrance, in particular the non-encapsulated fragrance, inert fillers or auxiliaries, dyes, rheology modifiers, moisture regulators, plasticizers, surfactants or other ingredients such as textile or skin care compounds. These and other optional components are explained below.

If the melt has surfactants, these are, in particular, anionic surfactants, preferably alkylsulfate, in particular C _8-12- alkyl sulfates.

In preferred embodiments, the melt may, for example, comprise one or more adsorbent materials for receiving the fragrance. A corresponding adsorber material can be present in amounts of up to 25% by weight, based on the total weight of the melt. The proportion is preferably in the range from 0.0% by weight to 25% by weight, in particular from 0.5% by weight to 20% by weight, preferably from 1% by weight to 15% by weight. or from 3 wt% to 10 wt%, more preferably from 5 wt% to 8 wt%. Suitable adsorber materials are, for example, porous inorganic substances, such as, for example, silica. Organic substances, such as crosslinked polymers, for example crosslinked polyvinylpyrrolidone, can also be used as the adsorbent material.

In addition, the melt may further comprise fillers or auxiliaries, such as emulsifiers, which for example improve the processability in the preparation or the homogeneity of the distribution of the microcapsules or the perfume in the carrier. Suitable fillers and auxiliaries are known to the person skilled in the art.

In various embodiments, as described herein, the melt may further comprise at least one fabric conditioning compound. In this context, a textile care compound is understood to mean any compound which gives textile fabrics treated therewith a beneficial effect, such as, for example, a textile softening effect, crease resistance or the harmful or negative effects which result during cleaning and / or conditioning and / or or wearing, such as fading, graying, etc., reduced.

The fabric care composition may preferably be made from fabric softening compounds, bleaches, bleach activators, enzymes, silicone oils, anti redeposition agents, optical brighteners, grayness inhibitors, anti-shrinkage agents, wrinkle inhibitors, color transfer inhibitors, antimicrobial agents, germicides, fungicides, antioxidants, antistatic agents, ironing aids, phobizers and the like Impregnating agents, swelling and slipping agents, UV absorbers and mixtures thereof are selected.

It is particularly preferred that the fabric care compound is a fabric softening compound. It is very particularly preferred that the textile-softening compound of polysiloxanes, textile-softening clays, cationic polymers and mixtures thereof.

The use of polysiloxanes and / or cationic polymers as textile-care compounds is advantageous because they not only have a softening effect, but also enhance the perfume impression on the laundry. The use of softening clays as textile-care compound is also advantageous because they additionally have a water-softening effect and thus, for example, limescale deposits on the laundry can be prevented.

1. a)
   
   mit R¹= unabhängig voneinander C₁-C₃₀-Alkyl, vorzugsweise C₁-C₄-Alkyl, insbesondere Methyl oder Ethyl, n = 1 bis 5000, vorzugsweise 10 bis 2500, insbesondere 100 bis 1500.

A polysiloxane preferably usable as textile softening compound has at least the following structural unit

1. a)
   
   with R ¹ = independently of one another C ₁ -C ₃₀ -alkyl, preferably C ₁ -C ₄ -alkyl, in particular methyl or ethyl, n = 1 to 5,000, preferably 10 to 2,500, in particular 100 to 1,500.

• b)
  
  mit R¹= C₁-C₃₀-Alkyl, vorzugsweise C₁-C₄-Alkyl, insbesondere Methyl oder Ethyl, Y = ggf. substituiertes, lineares oder verzweigtes C₁-C₂₀-Alkylen, vorzugsweise -(CH₂)m- mit m= 1 bis 16, vorzugsweise 1 bis 8, insbesondere 2 bis 4, im speziellen 3, R², R³ = unabhängig voneinander H oder gegebenenfalls substituiertes, lineares oder verzweigtes C₁-C₃₀-Alkyl, vorzugsweise mit Aminogruppen substituiertes C₁-C₃₀-Alkyl, besonders bevorzugt -(CH₂)_b-NH₂ mit b = 1 bis 10, äußerst bevorzugt b = 2, x = 1 bis 5000, vorzugsweise 10 bis 2500, insbesondere 100 bis 1500.

It may be preferred that the polysiloxane additionally has the following structural unit:

• b)
  
  with R ¹ = C ₁ -C ₃₀ -alkyl, preferably C ₁ -C ₄ -alkyl, in particular methyl or ethyl, Y = optionally substituted, linear or branched C ₁ -C ₂₀ -alkylene, preferably - (CH ₂ ) m with m = 1 to 16, preferably 1 to 8, in particular 2 to 4, in particular 3, R ² , R ³ = independently of one another H or optionally substituted, linear or branched C ₁ -C ₃₀ -alkyl, preferably substituted by amino groups C ₁ -C ₃₀ -alkyl, particularly preferably - (CH ₂ ) _b -NH ₂ where b = 1 to 10, most preferably b = 2, x = 1 to 5000, preferably 10 to 2500, in particular 100 to 1500.

If the polysiloxane has only the structural unit a) with R ¹ = methyl, it is a polydimethylsiloxane. Polydimethylpolysiloxanes are known as efficient fabric care compounds.

Suitable polydimethysiloxanes include DC-200 (ex Dow Corning), Baysilone® M 50, Baysilone® M 100, Baysilone® M 350, Baysilone® M 500, Baysilone® M 1000, Baysilone® M 1500, Baysilone® M 2000 or Baysilone® M 5000 (all ex GE Bayer Silicones).

However, it may also be preferred that the polysiloxane contains the structural units a) and b). A particularly preferred polysiloxane has the following structure: (CH ₃ ) ₃ Si [O-Si (CH ₃ ) ₂ ] _n - [O-Si (CH ₃ ) {(CH ₂ ) ₃ -NH- (CH ₂ ) ₂ -NH ₂ }] _x -OSi ( CH ₃ ) ₃ where the sum n + x is a number between 2 and 10,000.

Suitable polysiloxanes having the structural units a) and b) are for example commercially available under the trade names DC2-8663, DC2-8035, DC2-8203, DC05-7022 or DC2-8566 (all ex Dow Corning). According to the invention are also suitable for example the products commercially available Dow Corning ^® 7224, Dow Corning ^® 929 Cationic Emulsion or Formasil 410 (GE Silicones).

A suitable fabric softening clay is, for example, a smectite clay. Preferred smectite clays are beidellite clays, hectorite clays, laponite clays, montmorillonite clays, nontronite clays, saponite clays, sauconite clays, and mixtures thereof. Montmorillonite clays are the preferred softening clays. Bentonites contain mainly montmorillonites and can serve as a preferred source of fabric softening clay. The bentonites can be used as powder or crystals.

Suitable bentonites are sold for example under the names Laundrosil® ^® from Sud-Chemie or under the name Detercal by the company Laviosa. It is preferable that the textile-care composition contains a powdery bentonite as a fabric-care compound.

Suitable cationic polymers include in particular those described in "CTFA International Cosmetic Ingredient Dictionary", Fourth Edition, J. Chem. Nikitakis, et al, Editors, published by the Cosmetic, Toiletry, and Fragrance Association, 1991, and collectively collectively referred to as "Polyquaternium." In the following, some suitable polyquaternium compounds are listed in more detail.

POLYQUATERNIUM-1 (CAS number: 68518-54-7)
Definition: {(HOCH ₂ CH ₂ ) ₃ N ⁺ -CH ₂ CH = CHCH ₂ - [N ⁺ (CH ₃ ) ₂ -CH ₂ CH = CHCH ₂ ] _x -N ⁺ (CH ₂ CH ₂ OH) ₃ } [ Cl ^- ] _{x + 2}

POLYQUATERNIUM-2 (CAS number: 63451-27-4)
Definition: [-N (CH ₃ ) ₂ -CH ₂ CH ₂ CH ₂ -NH-C (O) -NH-CH ₂ CH ₂ CH ₂ -N (CH ₃ ) ₂ -CH ₂ CH ₂ OCH ₂ CH ₂ - ] ²⁺ (Cl ^- ) ₂

Polyquaternium-3
Definition: copolymer of acrylamide and trimethylammoniumethyl methacrylate methosulfate

POLYQUATERNIUM-4 (CAS number: 92183-41-0)
Definition: Copolymer of Hydroxyethyl Cellulose and Diallyldimethyl Ammonium Chloride Available for example as Celquat® H 100 or Celquat® L200 (ex National Starch)

POLYQUATERNIUM-5 (CAS number: 26006-22-4)
Definition: Copolymer of acrylamide and β-methacrylyloxyethyltrimethylammonium methosulfate.

POLYQUATERNIUM-6 (CAS number: 26062-79-3)
Definition: Polymer of dimethyldiallylammonium chloride

POLYQUATERNIUM-7 (CAS number: 26590-05-6)
Definition: Polymeric quaternary ammonium salt consisting of acrylamide and dimethyldiallylammonium chloride monomers.

Polyquaternium-8
Definition: Polymeric quaternary ammonium salt of methyl and stearyldimethylaminoethyl methacrylate quaternized with dimethyl sulfate

Polyquaternium-9
Definition: Polymeric quaternary ammonium salt of polydimethylaminoethyl methacrylate quaternized with methyl bromide

POLYQUATERNIUM-11 (CAS number: 53633-54-8)
Definition: Quaternary ammonium polymer formed by reaction of diethyl sulfate with the copolymer of vinylpyrrolidone and dimethylaminoethyl methacrylate.

POLYQUATERNIUM-12 (CAS number: 68877-50-9)
Definition: Quaternary ammonium polymer salt obtainable by reaction of the ethyl methacrylate / -abietyl methacrylate / diethylaminoethyl methacrylate copolymer with dimethyl sulfate

POLYQUATERNIUM-13 (CAS number: 68877-47-4)
Definition: Polymeric quaternary ammonium salt obtainable by reaction of the ethyl methacrylate / oleyl methacrylate / diethylaminoethyl methacrylate copolymer with dimethyl sulfate

POLYQUATERNIUM-14 (CAS number: 27103-90-8)
Definition: Polymeric quaternary ammonium salt of the formula - {- CH ₂ -C- (CH ₃ ) - [C (O) O-CH ₂ CH ₂ -N (CH ₃ ) ₃ ^- ]} _x ⁺ [CH ₃ SO ₄ ] ^- _x

POLYQUATERNIUM-15 (CAS number: 35429-19-7)
Definition: copolymer of acrylamide and β-methacrylyloxyethyltrimethylammonium chloride

POLYQUATERNIUM-16 (CAS number: 95144-24-4)
Definition: Polymeric quaternary ammonium salt formed from methylvinylimidazolium chloride and vinylpyrrolidone

POLYQUATERNIUM-17 (CAS number: 90624-75-2)
Definition: Polymeric quaternary ammonium salt obtainable by reaction of adipic acid and dimethylaminopropylamine with dichloroethyl ether.

Polyquaternium-18
Definition: Polymeric quaternary ammonium salt, which is obtainable by reaction of azelaic acid and dimethylaminopropylamine with dichloroethyl ether.

Polyquaternium-19
Definition: Polymeric quaternary ammonium salt, which is obtainable by reaction of polyvinyl alcohol with 2,3-epoxypropylamine.

Polyquaternium-20
Definition: Polymeric quaternary ammonium salt, obtainable by reaction of polyvinyloctadecyl ether with 2,3-epoxypropylamine.

POLYQUATERNIUM-21 (CAS number: 102523-94-4)
Definition: polysiloxane / polydimethyldialkylammonium acetate copolymer

POLYQUATERNIUM-22 (CAS number: 53694-17-0)
Definition: dimethyldiallylammonium chloride / acrylic acid copolymer

POLYQUATERNIUM-24 (CAS number: 107987-23-5)
Definition: Polymeric quaternary ammonium salt from the reaction of hydroxyethylcellulose with a lauryldimethylammonium substituted epoxide

Polyquaternium-27
Definition: Block copolymer from the reaction of Polyquaternium-2 with Polyquaternium-17.

POLYQUATERNIUM-28 (CAS number: 131954-48-8)
Definition: Vinylpyrrolidone / methacrylamidopropyltrimethylammonium chloride copolymer

Polyquaternium-29
Definition: Chitosan, which was reacted with propylene oxide and quaternized with epichlorohydrin

Polyquaternium-30
Definition: Polymeric quaternary ammonium salt of the formula: - [CH ₂ C (CH ₃ ) (C (O) OCH ₃ )] _x - [CH ₂ C (CH ₃ ) (C (O) OCH ₂ CH ₂ N ⁺ (CH ₃ ) ₂ CH ₂ COO ^- )] _y -

Polyquaternium-31 (CAS number: 136505-02-7)

Polyquaternium-32 (CAS number: 35429-19-7)
Definition: Polymer of N, N, N-trimethyl-2 - [(2-methyl-1-oxo-2-propenyl) oxy] -ethanaminium chloride with 2-propenamide

Polyquaternium-37 (CAS number: 26161-33-1)
Definition: homopolymer of methacryloyltrimethyl chloride
For example, available as Synthalen® CR (ex 3V Sigma)

Polyquaternium-44 (CAS number: 150595-70-5)
Definition: Quaternary ammonium salt of the copolymer of vinylpyrrolidone and quaternized imidazoline

POLYQUATERNIUM-68 (CAS-Number: 827346-45-2)
Definition: Quaternized copolymer of vinylpyrrolidone, methacrylamide, vinylimidazole and quaternized vinylimidazole

The amount of fabric care compound in the melt may, in various embodiments, be from 0.1% to 15%, and preferably from 1% to 12%, by weight. Bentonite is preferably used in an amount of up to 5% by weight, typically in amounts of from about 1% to 2% by weight.

The melt is made from the ingredients described. It preferably has a viscosity (Texas Instruments AR-G2 rheometer, plate / plate, 4 cm diameter, 1100 μm gap, shear rate 10 / 1sec) of 1500 mPa · s or less, in particular 1000 mPa · s or less. Particularly preferred is a viscosity between 50 and 1000 mPa · s, in particular between 100 and 800 mPa · s. This is preferred, since a dripping out of spherical particles is made possible in this way. This is then dripped, creating liquid spherical drops. These are then cooled, as a result of which the drops solidify, namely to form almost spherical particles, the spherical fragrance particles according to the invention.

100% spährischer particles would have an aspect ratio of 1. According to the invention, spherical particles in the sense of the present invention also include those which have only an approximately spherical shape, that is to say an aspect ratio of from 0.7 to 1.3, preferably from 0.8 to 1.2, in particular from 0.9 to 1.1 have.

The particles preferably have a diameter in the range from 1 mm to 10 mm, in particular from 1 mm to 5 mm, preferably from 2 mm to 4 mm. Thus, the particles are particularly soluble in water and at the same time for the consumer in a visually appealing size.

The carrier is inventively chosen so that it has a good water solubility as suitability for later use. The melting point must be in an area where fragrances can be well incorporated, but not destroyed, so that they retain their fragrant properties. In addition, the carrier should be non-toxic and ecologically safe.

After cooling, a rapid hardening must take place. Here, solid, hard balls must arise, which may not be sticky. The cooling or cooling can preferably be done by means of air and / or cooling liquid.

Cooling with air can take place, for example, with conditioned air in countercurrent. This is particularly promising if the diameter of the fragrance particles is as small as possible. Here, the heat capacity of the air is sufficient to allow a rapid solidification of the melt into hard, solid spheres.

Furthermore, cooling with coolant is possible. The melt is dripped directly into the cooling liquid. It is also possible to cool the melt both by means of air and by means of cooling liquid. This is done by first cooling the drops with air and then dripping into cooling liquid. By cooling in a cold gas atmosphere, especially in conditioned air, a solidified shell is formed, which guarantees dimensional stability during subsequent dripping into the cooling liquid.

The density of the solidified droplets may be smaller or larger than that of the cooling liquid. Usually, it is smaller than that of the cooling liquid. Accordingly, the solidified droplets float on the surface of the cooling liquid and can be skimmed off or collected via an overflow.

The main task of the cooling bath is to remove the melt drops after dropping heat, so that they solidify as quickly as possible. For this purpose, basically any liquid is suitable as a cooling liquid in the cooling bath. If the particles are removed very quickly after dripping, even water can be used. However, water is not preferred because the particles therein dissolve at least superficially and become sticky. Also, it is technically not easy to remove the particles so fast that they do not dissolve.

In order to avoid these technical disadvantages, as liquids in a first preferred embodiment, those liquids are used which have a reduced dissolving power for the constituents contained in the perfume particles, in particular the carrier material and the perfume.

Thus, the dissolving power of water for PEG or other carriers can be reduced, for example, by the addition of salt or water-miscible solvents.

A more preferred cooling fluid is therefore a saline solution, where salt solution is understood as meaning a solution of an inorganic or organic salt in a concentration such that the dissolution of the carrier polymer is retarded to such an extent that the particles can be harvested. Suitable salts are, for example, sodium chloride or sodium sulfate. Also, water-miscible solvents (such as glycols, glycerol) or other polar substances, such as sugars, sugar alcohols, or the like, which reduce solvent quality for PEG or other carriers, may be added to the water.

The easiest way is to remove residual refrigerant if it is volatile. Here, a simple drying process may be followed by recovery of the cooling liquid, if necessary. Volatile hydrocarbons, for example pentane, hexane, heptane, alcohols (ethanol, (iso) -propanol, etc.) or else volatile silicone oils may preferably be used for this purpose. Another preferred cooling fluid is therefore a volatile hydrocarbon, alcohol or volatile silicone. Volatile in this context means that the corresponding compounds have a boiling temperature of 120 ° C or less.

However, these coolants again have the disadvantage that on the one hand they can leach the perfume out of the particles, in particular if they can not be harvested immediately from the cooling bath for procedural reasons. On the other hand, they are usually flammable.

The latter disadvantages can be avoided by using a halogenated, preferably fluorinated, particularly preferably perfluorinated organic compound as the cooling liquid. Perflourated hydrocarbons, for example perfluorohexane, are often characterized by high stability, inertness and non-toxicity. However, due to a high GWP they can be harmful to the environment. This is avoided by using the liquid perfluoro- (2-methyl-3-pentanone) as a cooling bath. It does not dissolve the carrier or the perfume, is non-flammable, non-toxic and harmless to the environment. As a result of the poor wetting of the particles, moreover, hardly any residues of the cooling liquid remain after the particles have been harvested. Another advantage is the high density. This causes the particles to float on the coolant and thus be easily harvested by skimming or overflow.

A particularly preferred cooling liquid in the context of the present invention is therefore perfluoro (2-methyl-3-pentanone).

A more preferred cooling fluid is a non-aqueous fluid. For example, oils (triglycerides but also silicone oils) can be used. These do not dissolve the carrier but may have the disadvantage that, as they wet the particles, they are entrained in a substantial amount into the finished product and contaminate it or make it sticky. Here it is necessary to remove the remains of the cooling liquid after the particles have been harvested. * Surprisingly, it has been shown that mineral oils or vegetable oils are particularly suitable as a cooling liquid. In a particularly preferred embodiment, the cooling liquid is therefore a mineral oil or a vegetable oil, in particular a vegetable oil. Suitable vegetable oils are For example, those oils which may also be used as a salad oil, such as thistle oil, sunflower oil, olive oil, walnut oil, linseed oil, soybean oil, sunflower oil, tall oil, castor oil, tung oil or others. In principle, vegetable oils derived from oil plants are rich oils. The advantage of vegetable oils is that they are inexpensive to obtain, the fragrance particles do not adversely affect and the fragrance particles can easily be separated from the oils, so it can be easily removed from the cooling bath, without the need for special devices are needed. Also, special safety regulations in the handling of these oils are not necessary, so therefore these oils are preferred.

In addition to the specific selection of suitable cooling liquids described above, there is another possibility for reducing the tendency to dissolve the fragrance particles in the cooling liquid in the at least partial saturation of this liquid with at least one preferably several constituents of the fragrance particles. In particular, the use of cooling liquids which are at least partly saturated with the carrier material and / or the perfume is preferred. The at least partial saturation may be achieved by dissolving the one or more constituents of the perfume particles in the cooling fluid prior to the start of dripping. Of course, it is also possible to achieve the at least partial saturation within the scope of the preparation of the fragrance particles by waiting in the context of production, the setting of a steady state (equilibrium) state and the fragrance particles prepared until this condition is discarded or recycled.

A preferred embodiment of the method is characterized in that at least 90 wt .-%, preferably at least 95 wt .-% and in particular at least 98 wt .-% of the constituents contained in the fragrance particles in the cooling liquid of the cooling bath at the temperature used in the process Cooling bath have a solubility below 10 g / L, preferably below 5 g / L and in particular below 1 g / L.

Another aspect relevant to the process control is the extent to which the cooling liquid wets the surface of the fragrance particles. Preferably, the cooling liquid wets the surface of the fragrance particle only partially, most preferably not at all. The lower the wetting of the particle surface, the lower the residues of the cooling liquid on the particle and the easier the complete removal of the coolant after discharging the fragrance particles from the cooling bath.

In order to allow effective curing of the spherical particles, the cooling bath has a temperature which is below the melting temperature of the carrier. The melting temperature of the support is preferably 100 ° C or less, preferably 40 ° C to 100 ° C, especially 50 ° C to 90 ° C, more preferably 55 ° C to 80 ° C. The temperature of the cooling bath is preferably 50 ° C or less, preferably 40 ° C or less, especially 25 ° C or less, preferably 20 ° C or less, more preferably 15 ° C or less.

The temperature at which the cooling bath is located is not critical to the present invention as long as it is below the melting point of the above-mentioned melt. For example, it is preferable to operate the cooling bath at a common ambient temperature. This avoids, for example, that condenses water from the ambient air.

For the process sequence, in particular the process duration and the product quality, it has proved to be advantageous if the temperature of the cooling bath is at least 10 ° C., preferably at least 25 ° C. and in particular at least 35 ° C. below the melting temperature of the carrier.

If the cooling bath does not come into contact with possibly moist ambient air, it can also be cooled significantly below the room temperature. This has the advantage that the dripped melt solidifies faster and less "twins" form, that is, particles which collide on the surface of the liquid before solidification and adhere to each other.

To avoid the formation of "twins", the surface of the liquid can also be made to flow. As a result, the particles are carried away quickly from the dropping point. In the simplest case, the flow can be generated by stirring.

However, it is more advantageous to create a flow by pumping cooling liquid into the droplet vessel, passing it at the point of introduction, and exiting the vessel at another point together with the floating particles via an overflow. At this point, the particles can be removed by simply screening. A schematic structure with a corresponding flow is in 1 shown. The melt ( 1 ) in a suitable container and via a Eintropfdüse ( 2 ) in the cooling bath ( 4 ) dripped. This solidifies particles ( 3 ). In the embodiment shown here, the solidified particles have a lower density than the cooling liquid, so that the particles on the surface of the Coolant to float. While the melt drips at one end of the cooling bath, there is an overflow at the other end of the cooling bath ( 5 ). Over this occurs the cooling liquid together with the solidified particles ( 3 ) from the cooling bath ( 4 ) and can be stored in a suitable receptacle ( 6 ) are caught. The cooling fluid drains off and can be pumped by means of a circulation pump ( 7 ) back to the cooling bath ( 4 ). By the circulation pump ( 7 ), a flow stream is generated, so that the formation of "twins", ie double particles can be substantially avoided.

Alternatively, it is also possible that the particles ( 3 ) have a higher density than the cooling liquid and at the bottom of the cooling bath ( 4 ) collect. Here then the cooling bath ( 4 ) be configured such that the gravity tapers downwards and the particles can be removed according to the bottom of the cooling bath.

The removal of the particles ( 3 ) can also be removed manually from the cooling bath (eg by means of a sieve or similar suitable devices). 4 ) respectively. If particles are mentioned in the present application, these are to be understood as meaning the fragrance particles according to the invention.

• b1) einleiten der Schmelze über einen Einlass (8) ins Innere eines Behältnisses (9), wobei das Behältnis (9) als Auslass eine Düsenanordnung (10) mit kreisförmigen Öffnungen aufweist, und
• b2) anschließend oder gleichzeitig in Schwung versetzen des Behältnisses (9) mittels eines Schwingungskörpers (11), zum Vertropfen der Schmelze.

Particularly preferably according to the invention, the dripping takes place in a device in which the largest possible number of fragrance particles can be obtained simultaneously. In a preferred embodiment, step b) of the method according to the invention comprises

• b1) introducing the melt through an inlet ( 8th ) into the interior of a container ( 9 ), the container ( 9 ) as outlet a nozzle arrangement ( 10 ) having circular openings, and
• b2) subsequently or simultaneously activating the container ( 9 ) by means of a vibrating body ( 11 ), to drip the melt.

In the method preferred according to the invention, a melt is now introduced via an inlet ( 8th ) into the interior of a suitable container ( 9 ). In 2 is shown schematically a suitable structure of a corresponding device. In the figure, the container ( 9 ) in the form of a perforated plate. The container ( 9 ) may be round or oval in its outer shape, for example. However, it is also possible that the container has quadrangular, rectangular or another shape.

The container ( 9 ) is designed such that it has a cavity inside, in which the melt via an inlet ( 8th ) can be initiated. As an outlet, the container ( 9 ) on a nozzle assembly. The nozzle arrangement ( 10 ) has circular openings. Preferably, the container has at least 10 , preferably at least 50 and in particular at least 100 circular openings. The more openings the container has, the greater the throughput, ie the more amount of melt can pass through the container over a certain period of time ( 9 ). Accordingly, the production amount of fragrance particles is large.

Preference is given to the circular openings which at the bottom of the container ( 9 ) are arranged, annularly arranged on the outer edge of the container. This means that in the middle of the container ( 9 ) no openings are present, but only at the edge of the container ( 9 ) Openings are to be found. However, it is also possible that the circular openings are homogeneous on the underside of the container ( 9 ) are distributed.

Is in the present application of the underside or top of the speech, this is the page to understand how it is to be regarded when using a corresponding device in the process. According to gravity, the melt flows from above through the inlet downwards, ie first into the interior of the container and then in the direction of the nozzle assembly and out of the corresponding circular openings out of the container again.

Into the inner container ( 9 ) a melt is passed. Following the introduction of the melt or even during this time, the container ( 9 ) by means of a vibrating body ( 11 ) vibrated. Preferably, the vibration is an axial vibration.

The oscillation can take place, for example, by means of a plunger, by means of which vibrations from the oscillation body ( 11 ) on the container ( 9 ) be transmitted. Depending on the transmission of the vibration is also the arrangement of the nozzles ( 10 ). Preferably, the container ( 9 ) is not completely covered on the bottom with circular openings, but annular in the outer region of the container ( 9 ). In the middle of an area without openings is present, since the vibration body ( 11 ) would produce a different drop image in this area. In the case of a two-dimensional vibration excitation of the container ( 9 ) by a correspondingly suitable vibration body ( 11 ) is also a complete covering of the underside of the container ( 9 ) with circular openings conceivable. The vibration is basically responsible for producing a uniform droplet image, thereby preserving spherical fragrance particles.

The circular openings of the container ( 9 ) preferably have a diameter in the range of 0.1 mm to 3 mm, in particular in the range of 0.2 mm to 2.5 mm, preferably from 0.5 mm to 2.5 mm, preferably from 1 mm to 2 mm , This opening size ensures a sufficiently high throughput, so that an economic manufacturing process is possible. At the same time, this limits the size of the fragrance particles obtained, so that they are left after leaving the container ( 9 ) quickly solidify and dry, while also being able to dissolve quickly again. In addition, corresponding sizes of the particles are visually appealing to the consumer.

The size of the particles contained, ie the diameter of the particles (fragrance particles) corresponds approximately to twice the diameter of the circular opening of the container ( 9 ).

In order for the drops to deform as little as possible upon impact with the cooling liquid, the container should ( 9 ) either immerse in the coolant or be mounted just above the liquid level of the coolant, that the energy of the trap and thus the deformation are low. A slight deformation can be reversed by the surface tension of the drops before the final curing.

In a further embodiment, the present invention relates to particles (fragrance particles) as obtained by the method according to the invention.

The particles according to the invention (fragrance particles) have a spherical shape. The ingredients correspond to those of the melt.

If the spherical fragrance particles have textile-care compounds as described above, they are used in particular as fragrancing agents in the main wash cycle of an automatic washing or cleaning process. The fragrance particles can be given by the consumer in the desired dosage - in addition to the detergent or cleaning agent - in the corresponding dispenser or directly into the drum of the washing machine. This has the advantage that no additional rinse is necessary and no unsightly deposits occur in the dispenser.

Furthermore fragrance particles according to the invention can be used in the wash cycle of a laundry cleaning process and thus already transport the textile-care compound and the fragrance directly to the laundry at the beginning of the washing process so as to be able to develop its full potential. Furthermore, the fragrance particles are easier and better to handle than liquid compositions, since no drops remain on the edge of the bottle, which lead to subsequent storage of the bottle to edges on the ground or to unsightly deposits in the region of the closure. The same applies in the event that some of the particles are accidentally spilled during dosing. The spilled amount can also be removed easier and cleaner.

The fragrance particle may optionally contain other ingredients. In order to improve the performance and / or aesthetic properties, regardless of their intended use, these additional ingredients are preferably selected from the group consisting of dyes, pearlescing agents, skin-care compounds, bittering agents and mixtures thereof.

In order to improve the aesthetic impression of the particles, it can be colored with suitable dyes. Preferred dyes, the selection of which presents no difficulty to the skilled person, should have a high storage stability and insensitivity to the other ingredients of detergents or cleaning agents and to light and no pronounced substantivity to textile fibers so as not to stain them. The amount is usually 0.0001 wt .-% to 1 wt .-% of dye, preferably 0.001 wt .-% to 0.5 wt .-%.

The fragrance particles may also contain a pearlescing agent to increase the gloss. Examples of suitable pearlescing agents are ethylene glycol mono- and distearate and PEG-3-distearate.

Furthermore, the fragrance particles may comprise one or more skin care compounds.

A skin-care compound is understood to mean a compound or a mixture of compounds which, upon contact of a textile with the composition, attract the textile and, when the textile contacts the skin, confer an advantage on the skin compared with a textile which is not treated with the composition according to the invention has been. This benefit may include, for example, the transfer of the skin care compound from the textile to the skin, less water transfer from the skin to the textile, or less friction on the skin surface through the textile.

1. a) Wachse wie Carnauba, Spermaceti, Bienenwachs, Lanolin, Derivate davon sowie Mischungen daraus;
2. b) Pflanzenextrakte, zum Beispiel pflanzliche Öle wie Avokadoöl, Olivenöl, Palmöl, Palmenkemöl, Rapsöl, Leinöl, Sojaöl, Erdnussöl, Korianderöl, Ricinusöl, Mohnöl, Kakaoöl, Kokosnussöl, Kürbiskernöl, Weizenkeimöl, Sesamöl, Sonnenblumenöl, Mandelöl, Macadamianussöl, Aprikosenkernöl, Haselnussöl, Jojobaöl oder Canolaöl, Kamille, Aloe Vera sowie Mischungen daraus;
3. c) höhere Fettsäuren wie Laurinsäure, Myristinsäure, Palmitinsäure, Stearinsäure, Behensäure, Ölsäure, Linolsäure, Linolensäure, Isostearinsäure oder mehrfach ungesättigte Fettsäuren;
4. d) höhere Fettalkohole wie Laurylalkohol, Cetylalkohol, Stearylalkohol, Oleylalkohol, Behenylalkohol oder 2-Hexadecanol,
5. e) Ester wie Cetyloctanoat, Lauryllactat, Myristyllactat, Cetyllactat, Isopropylmyristat, Myristylmyristat, Isopropylpalmitat, Isopropyladipat, Butylstearat, Decyloleat, Cholesterolisostearat, Glycerolmonostearat, Glyceroldistearat, Glyceroltristearat, Alkyllactat, Alkylcitrat oder Alkyltartrat;
6. f) Kohlenwasserstoffe wie Paraffine, Mineralöle, Squalan oder Squalen;
7. g) Lipide;
8. h) Vitamine wie Vitamin A, C oder E oder Vitaminalkylester;
9. i) Phospholipide;
10. j) Sonnenschutzmittel wie Octylmethoxylcinnamat und Butylmethoxybenzoylmethan;
11. k) Silikonöle wie lineare oder cyclische Polydimethylsiloxane, Amino-, Alkyl-, Alkylaryl- oder Aryl-substituierte Silikonöle und
12. l) Mischungen daraus

umfassen.The skin care composition is preferably hydrophobic, may be liquid or solid, and must be compatible with the other ingredients of the solid, fabric care composition. For example, the skin care compound

1. a) waxes such as carnauba, spermaceti, beeswax, lanolin, derivatives thereof and mixtures thereof;
2. b) Plant extracts, for example vegetable oils such as avocado oil, olive oil, palm oil, palm kernel oil, rapeseed oil, linseed oil, soybean oil, peanut oil, coriander oil, castor oil, poppy seed oil, cocoa oil, coconut oil, pumpkin seed oil, wheat germ oil, sesame oil, sunflower oil, almond oil, macadamia nut oil, apricot kernel oil, hazelnut oil , Jojoba oil or canola oil, chamomile, aloe vera and mixtures thereof;
3. c) higher fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, linoleic acid, linolenic acid, isostearic acid or polyunsaturated fatty acids;
4. d) higher fatty alcohols, such as lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol or 2-hexadecanol,
5. e) esters such as cetyloctanoate, lauryl lactate, myristyl lactate, cetyl lactate, isopropyl myristate, myristyl myristate, isopropyl palmitate, isopropyl adipate, butyl stearate, decyl oleate, cholesterol isostearate, glycerol monostearate, glyceryl distearate, glycerol tristearate, alkyl lactate, alkyl citrate or alkyl tartrate;
6. f) hydrocarbons such as paraffins, mineral oils, squalane or squalene;
7. g) lipids;
8. h) vitamins such as vitamins A, C or E or vitamin alkyl esters;
9. i) phospholipids;
10. j) sunscreens such as octyl methoxyl cinnamate and butyl methoxybenzoyl methane;
11. k) silicone oils such as linear or cyclic polydimethylsiloxanes, amino-, alkyl-, alkylaryl- or aryl-substituted silicone oils and
12. l) mixtures thereof

include.

The amount of skin-care compound is preferably between 0.01% by weight and 10% by weight, preferably between 0.1% by weight and 5% by weight and most preferably between 0.3% by weight and 3 wt .-% based on the total weight of the fragrance particles. It may be that the skin-nourishing compound additionally has a textile care effect.

To prevent ingestion of particles by people, especially children, or animals, they may contain a bittering agent such as Bitrex ^®.

Components contained in the fragrance particles are accordingly contained in the melt.

The present invention furthermore relates to the use of the fragrance particles described herein as textile care agents, preferably fragrancing agents, for the scenting of textile fabrics. For this purpose, fragrance particles are brought into contact with the textile fabrics together with a conventional washing or cleaning agent in the (main) wash cycle of a conventional washing or cleaning process.

With the method according to the invention, aesthetically pleasing, approximately spherical fragrance particles can be produced. This was not possible with the known in the art Pastillierverfahren.

1. 1. Verfahren zur Herstellung wasserlöslicher sphärischer Duftpartikel (3) umfassend
   1. a) Herstellen einer Schmelze (1), umfassend wenigstens einen wasserlöslichen Träger sowie wenigstens einen Duftstoff und anschließendes
   2. b) Vertropfen der Schmelze (1) in ein Kühlbad (4), und
   3. c) Abkühlen der Schmelze (1), wodurch diese zu festen, harten Partikeln erstarrt.
2. 2. Verfahren nach Punkt 1, dadurch gekennzeichnet, dass Schritt b) die folgenden Schritte umfasst:
   • b1) Einleiten der Schmelze über einen Einlass (8) ins Innere eines Behältnisses (9), wobei das Behältnis (9) als Auslass eine Düsenanordnung (10) mit kreisförmigen Öffnungen aufweist, und
   • b2) anschließend oder gleichzeitig in Schwung versetzen des Behältnisses (9) mittels eines Schwingungskörpers (11), zum Vertropfen der Schmelze.
3. 3. Verfahren nach Punkt 2, dadurch gekennzeichnet, dass das Behältnis (9) in axiale Schwingungen versetzt wird.
4. 4. Verfahren nach einem oder mehreren der Punkte 2 oder 3, dadurch gekennzeichnet, dass die kreisförmigen Öffnungen ringförmig an der Unterseite des Behältnisses (9) angeordnet sind.
5. 5. Verfahren nach einem oder mehreren der Punkte 2 bis 4, dadurch gekennzeichnet, dass die kreisförmigen Öffnungen einen Durchmesser im Bereich von 0,1 mm bis 3 mm, insbesondere im Bereich von 0,2 mm bis 2,5 mm, vorzugsweise von 0,5 mm bis 2,5 mm, bevorzugt von 1 mm bis 2 mm aufweisen.
6. 6. Verfahren nach einem oder mehreren der Punkte 1 bis 5, dadurch gekennzeichnet, dass der Träger ausgewählt ist aus der Gruppe der Polymere, vorzugsweise aus der Gruppe der Polyethylenglycole, EO/PO-Blockcopolymere oder hochalkoxylierten nichtionischen Tenside, insbesondere aus der Gruppe der Polyethylenglycole.
7. 7. Verfahren nach einem oder mehreren der Punkte 1 bis 5, dadurch gekennzeichnet, dass der Träger ausgewählt ist aus der Gruppe der wasserhaltigen Salze, deren Wasserdampf-Partialdruck bei einer bestimmten Temperatur im Bereich von 30 bis 100°C dem H₂O-Partialdruck der gesättigten Lösung dieses Salzes entspricht, insbesondere Natriumacetat Trihydrat.
8. 8. Zusammensetzung nach einem oder mehreren der Punkte 1 bis 7, dadurch gekennzeichnet, dass der Gewichtsanteil des Trägers am Gesamtgewicht der Duftpartikel 30 bis 95 Gew.-%, vorzugsweise von 40 bis 90 Gew.-% und insbesondere 45 bis 90 Gew.-% beträgt.
9. 9. Zusammensetzung nach einem oder mehreren der Punkte 1 bis 8, dadurch gekennzeichnet, dass der mindestens eine Duftstoff in Form von Duftstoffkapseln und/oder Parfümölen eingesetzt wird.
10. 10. Zusammensetzung nach einem oder mehreren der Punkte 1 bis 9, dadurch gekennzeichnet, dass der Gewichtsanteil des Duftstoffs am Gesamtgewicht der Duftpartikel 0,1 Gew.-% bis 20 Gew.-%, vorzugsweise 1 Gew.-% bis 20 Gew.-%, weiter bevorzugt 1 Gew.-% bis 15 Gew.-%, insbesondere 3 Gew.-% bis 10 Gew.-% beträgt.
11. 11. Verfahren nach einem oder mehreren der Punkte 1 bis 10, dadurch gekennzeichnet, dass das Kühlbad eine Temperatur aufweist, die unterhalb der Schmelztemperatur des Trägers liegt.
12. 12. Verfahren nach einem oder mehreren der Punkte 1 bis 11, dadurch gekennzeichnet, dass die Schmelztemperatur des Trägers 100°C oder weniger, vorzugsweise 40°C bis 100°C, insbesondere 50°C bis 90°C, besonders bevorzugt 55 °C bis 80°C beträgt.
13. 13. Verfahren nach einem oder mehreren der Punkte 1 bis 12, dadurch gekennzeichnet, dass die Temperatur des Kühlbades 50°C oder weniger, bevorzugt 40°C oder weniger, insbesondere 25°C oder weniger, vorzugsweise 20°C oder weniger, besonders 15°C oder weniger beträgt.
14. 14. Verfahren nach einem oder mehreren der Punkte 1 bis 13, dadurch gekennzeichnet, dass die Temperatur des Kühlbades mindestens 10°C, vorzugsweise mindestens 25°C und insbesondere mindestens 35°C unterhalb der Schmelztemperatur des Trägers liegt.
15. 15. Verfahren nach einem oder mehreren der Punkte 1 bis 14, dadurch gekennzeichnet, dass das Kühlbad eine Kühlflüssigkeit ausgewählt aus Wasser, einer wässrigen Salzlösung, mit Wasser mischbaren Lösungsmitteln, Ölen, Kohlenwasserstoffen, halogenierte Kohlenwasserstoffen sowie Mischungen aus diesen, aufweist.
16. 16. Verfahren nach einem oder mehreren der Punkte 1 bis 15, dadurch gekennzeichnet, dass die Kühlflüssigkeit ein Öl, insbesondere ein Mineralöl oder ein Pflanzenöl, vorzugsweise ein Pflanzenöl ist.
17. 17. Verfahren nach einem oder mehreren der Punkte 1 bis 16, dadurch gekennzeichnet, dass die Kühlflüssigkeit Perfluoro-(2-methyl-3-pentanone) aufweist und insbesondere daraus besteht.
18. 18. Verfahren nach einem oder mehreren der Punkte 1 bis 17, dadurch gekennzeichnet, dass mindestens 90 Gew.-%, vorzugsweise mindestens 95 Gew.-% und insbesondere mindestens 98 Gew.-% der in den Duftstoffpartikeln enthaltenen Bestandteile in der Kühlflüssigkeit des Kühlbades bei der im Verfahren eingesetzten Temperatur des Kühlbades eine Löslichkeit unterhalb 10 g/L, bevorzugt unterhalb 5 g/L und insbesondere unterhalb 1 g/L aufweisen.
19. 19. Verfahren nach einem oder mehreren der Punkte 1 bis 18, dadurch gekennzeichnet, dass die Kühlflüssigkeit die Oberfläche der Duftpartikel nur partiell, ganz besonders bevorzugt gar nicht benetzt.
20. 20. Verfahren nach einem oder mehreren der Punkte 1 bis 19, dadurch gekennzeichnet, dass die Oberfläche der Kühlflüssigkeit im Kühlbad während des Eintropfens in Strömung versetzt wird.
21. 21. Sphärische Duftpartikel erhalten durch ein Verfahren nach einem oder mehreren der Punkte 1 bis 20.
22. 22. Verwendung von Duftpartikeln gemäß Punkt 21 zum Beduften von Objekten, insbesondere von textilen Flächengebilden.

In summary, the present invention provides, inter alia:

1. 1. Process for the preparation of water-soluble spherical fragrance particles ( 3 ) full
   1. a) producing a melt ( 1 ), comprising at least one water-soluble carrier and at least one perfume and then
   2. b) dropping the melt ( 1 ) in a cooling bath ( 4 ), and
   3. c) cooling the melt ( 1 ), which solidifies into solid, hard particles.
2. 2. Method according to point 1 , characterized in that step b) comprises the following steps:
   • b1) introducing the melt through an inlet ( 8th ) into the interior of a container ( 9 ), the container ( 9 ) as outlet a nozzle arrangement ( 10 ) having circular openings, and
   • b2) subsequently or simultaneously activating the container ( 9 ) by means of a vibrating body ( 11 ), to drip the melt.
3. 3. Procedure according to point 2 , characterized in that the container ( 9 ) is set in axial oscillations.
4. 4. Method according to one or more of the points 2 or 3 , characterized in that the circular openings annularly at the bottom of the container ( 9 ) are arranged.
5. 5. Method according to one or more of the points 2 to 4 , characterized in that the circular openings have a diameter in the range of 0.1 mm to 3 mm, in particular in the range of 0.2 mm to 2.5 mm, preferably from 0.5 mm to 2.5 mm, preferably from 1 mm to 2 mm.
6. 6. Method according to one or more of the points 1 to 5 , characterized in that the carrier is selected from the group of polymers, preferably from the group of polyethylene glycols, EO / PO block copolymers or highly alkoxylated nonionic surfactants, in particular from the group of polyethylene glycols.
7. 7. Method according to one or more of the points 1 to 5 , characterized in that the support is selected from the group of hydrous salts whose water vapor partial pressure at a certain temperature in the range of 30 to 100 ° C corresponds to the H ₂ O partial pressure of the saturated solution of this salt, in particular sodium acetate trihydrate.
8. 8. Composition according to one or more of the points 1 to 7 , characterized in that the weight proportion of the carrier in the total weight of the fragrance particles 30 to 95 Wt .-%, preferably from 40 to 90 wt .-% and in particular 45 to 90 wt .-% is.
9. 9. Composition according to one or more of the points 1 to 8th , characterized in that the at least one fragrance is used in the form of perfume capsules and / or perfume oils.
10. 10. Composition according to one or more of the points 1 to 9 , characterized in that the proportion by weight of the fragrance in the total weight of the fragrance particles 0.1 wt .-% to 20 wt .-%, preferably 1 wt .-% to 20 wt .-%, more preferably 1 wt .-% to 15 wt .-%, in particular 3 wt .-% to 10 wt .-% is.
11. 11. Method according to one or more of the points 1 to 10 , characterized in that the cooling bath has a temperature which is below the melting temperature of the carrier.
12. 12. Method according to one or more of the points 1 to 11 , characterized in that the melting temperature of the carrier is 100 ° C or less, preferably 40 ° C to 100 ° C, in particular 50 ° C to 90 ° C, particularly preferably 55 ° C to 80 ° C.
13. 13. Method according to one or more of the points 1 to 12 , characterized in that the temperature of the cooling bath is 50 ° C or less, preferably 40 ° C or less, especially 25 ° C or less, preferably 20 ° C or less, especially 15 ° C or less.
14. 14. Method according to one or more of the points 1 to 13 , characterized in that the temperature of the cooling bath is at least 10 ° C, preferably at least 25 ° C and in particular at least 35 ° C below the melting temperature of the carrier.
15. 15. Method according to one or more of the points 1 to 14 , characterized in that the cooling bath comprises a cooling liquid selected from water, an aqueous salt solution, water-miscible solvents, oils, hydrocarbons, halogenated hydrocarbons and mixtures thereof.
16. 16. Method according to one or more of the points 1 to 15 , characterized in that the cooling liquid is an oil, in particular a mineral oil or a vegetable oil, preferably a vegetable oil.
17. 17. Method according to one or more of the points 1 to 16 , characterized in that the cooling liquid has perfluoro- (2-methyl-3-pentanone) and in particular consists thereof.
18. 18. Method according to one or more of the points 1 to 17 , characterized in that at least 90 wt .-%, preferably at least 95 wt .-% and in particular at least 98 wt .-% of the constituents contained in the perfume particles in the cooling liquid of the cooling bath at the temperature of the cooling bath used in the process, a solubility below 10 g / L, preferably below 5 g / L and in particular below 1 g / L.
19. 19. Method according to one or more of the points 1 to 18 , characterized in that the cooling liquid, the surface of the fragrance particles only partially, most preferably not wetted.
20. 20. Method according to one or more of the points 1 to 19 , characterized in that the surface of the cooling liquid is added in the cooling bath during the dripping in flow.
21. 21. Spherical fragrance particles obtained by a method according to one or more of the items 1 to 20 ,
22. 22. Use of fragrance particles according to item 21 for perfuming objects, in particular textile fabrics.

In the following embodiment, the present invention will not be explained further in a nonlimiting manner.

Embodiment:

Melt of the following compositions according to the invention were prepared: S1 S2 PEG 6000 93.0% 90.0% Perfume oil 1 2.6% Perfume capsules 1 4.4% Perfume oil 2 4.30% Perfume capsules 2 5.70% dye 0.01% 0.010%

These were brought to a temperature of 55 ° C and dripped through a nozzle in a bath, which was kept at room temperature (23 ° C). It was a device according to 1 used.

After solidification, the particles according to the invention, which had approximately spherical shape, were screened off.

QUOTES INCLUDE IN THE DESCRIPTION

This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.

Cited patent literature

• EP 2496679 B1 [0005]

Cited non-patent literature

• DIN 53240-1 [0039]
• DIN 53240-1: 2012-07 [0039]

Claims (12)

Process for preparing water-soluble spherical fragrance particles (3) a) producing a melt (1) comprising at least one water-soluble carrier and at least one perfume and subsequent b) dripping the melt (1) in a cooling bath (4), and c) cooling the melt (1), whereby it solidifies to solid, hard particles. Method according to Claim 1 characterized in that step b) comprises the steps of: b1) introducing the melt into an interior of a container (9) via an inlet (8), the container (9) having as outlet a nozzle arrangement (10) with circular openings, and b2) subsequently or simultaneously set in motion of the container (9) by means of a vibration body (11) for dripping the melt. Method according to Claim 2 , characterized in that the container (9) is set in axial oscillations. Method according to one or more of Claims 2 or 3 , characterized in that the circular openings have a diameter in the range of 0.1 mm to 3 mm, in particular in the range of 0.2 mm to 2.5 mm, preferably of 0.5 mm to 2.5 mm, preferably of 1 mm to 2 mm. Method according to Claim 1 to 4 , characterized in that the melting temperature of the carrier is 100 ° C or less, preferably 40 ° C to 100 ° C, in particular 50 ° C to 90 ° C, particularly preferably 55 ° C to 80 ° C. Method according to one or more of Claims 1 to 5 , characterized in that the temperature of the cooling bath is 50 ° C or less, preferably 40 ° C or less, especially 25 ° C or less, preferably 20 ° C or less, especially 15 ° C or less. Method according to one or more of Claims 1 to 6 , characterized in that the cooling bath has a cooling liquid which is selected from oils, in particular mineral oils or vegetable oils, preferably vegetable oils. Method according to one or more of Claims 1 to 6 , characterized in that the cooling bath comprises a cooling liquid selected from the halogenated hydrocarbons, with perfluoro- (2-methyl-3-pentanone) being particularly preferred. Method according to one or more of Claims 1 to 8th , characterized in that the carrier is selected from polyethylene glycols and sodium acetate trihydrate. Method according to one or more of Claims 1 to 9 , characterized in that the surface of the cooling liquid is added in the cooling bath during the dripping in flow. Spherical fragrance particles obtained by a method according to one or more of Claims 1 to 10 , Use of fragrance particles according to Claim 11 for perfuming objects, in particular textile fabrics.

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