EP1359247A1 - Fibres and textile fabrics finished with microcapsules - Google Patents

Abstract

Fibres and textile sheet, treated with preparations of (a) micro-encapsulated active substances which also contain (b) binders. Independent claims are also included for methods for the treatment of fibres and textiles by impregnation of the substrate with an aqueous preparation containing (a) and (b), or by forced application of such a preparation to the substrate.

Description

Field of the invention

The present invention is in the field of textile technology and relates to new ones finished fibers and fabrics with improved comfort, method to their preparation and the use of mixtures of microencapsulated agents and binders for textile equipment.

State of the art

The term "comfort" summarizes increased demands of the consumer, who does not want to be content with just being alone Nursing worn on the skin, such as underwear or tights scratching still cause skin redness but quite conversely expected to be positive affects the condition of his skin. These may be both fatigue symptoms to remedy, as well as to convey a fresh scent or skin roughness to avoid.

There was therefore no lack of effort, textiles and again especially women's tights - this seems to be a particularly attractive consumer field - with cosmetic To equip active ingredients that transfer to the skin when wearing and there the desired Cause effects. Now it is in the nature of things that the desired Effects only come about when the corresponding active ingredient from the carrier to the Skin is transmitted, i. after a more or less long wearing time is on the garment no active ingredient left. This makes certain to the manufacturer of such products Requirements in the selection of active substances, because, while weighing performance, he has to make a compromise, and not least the associated costs find a product whose effect can be experienced and its increased price can be paid by the customer. Because cosmetic agents that have the desired effects aurweisen, are usually expensive and also the equipment of the final products with additional Costs associated with it, it is of particular importance to the manufacturer that it except by the contact between the finished end product and the wearer's skin to further undesirable losses of active ingredients, as this would lead to the customer is paid more expensive wearing comfort over a shorter time. A particularly undesirable form of drug loss occurs in connection with the Washing of the so finished fibers and textiles. Even if these losses are not Avoid it completely, so it is obvious that it is a particular concern of the manufacturer corresponding products is to apply the active ingredients in such a way on the fibers, that these are not readily dissolved or mechanically detached.

Instead of the often carried out impregnation, in which the active ingredients directly on the Fibers or textiles have been applied, therefore, in recent years the use of microencapsulated Active ingredients gained in importance. Behind this is the consideration, water-soluble or to include water-dispersible active ingredients in water-insoluble capsules, which the active principles during wearing either by controlled release through membrane pores or by mechanical destruction of the enveloping membranes. On this way, the losses that occur over many wash cycles can be compared actually significantly reduce the use of unencapsulated agents. The thus achieved Overall, however, results are far from satisfactory because the encapsulated active ingredients are stored only loosely between the fiber fibrils and thus for example by mechanical Exposure can be easily rinsed out during the washing process.

The object of the present invention has therefore been to those with active ingredients equipped fibers and textiles that are free from the above Disadvantages are, i. the beneficial properties also over a variety of washing cycles without significant drug losses during the wash comes.

Description of the invention

(a) mikroverkapselten Wirkstoffen und

(b) Bindemitteln

ausgerüstet sind. The invention relates to special fibers and fabrics, which are characterized in that they are made with mixtures of

(a) microencapsulated substances and

(b) binders

are equipped.

Surprisingly, it was found that the equipment of fibers and textiles with a Mixture of microencapsulated agents and binders causes the microcapsules and thus also the active ingredients get a firmer adhesion to the fibers and thus during the washing process are less rapidly peeled off and rinsed as comparable finished end products where the microcapsules have no direct adhesion to the fiber fibrils exhibit. In this way, finished fibers and fabrics are obtained where the additional care effect over conventional products of the The prior art both in permanent wear as well as after an equal number of Washing cycles can be perceived by the consumer over a longer period of time.

While commercial skincare agents on average only 2 wt .-% of active Having active ingredients, there is a particular advantage of the present invention equipped fibers and textiles further in that the applied microcapsules are a much higher Have active ingredient content of about 20 to 30 wt .-%.

drugs

Squalan,

Chitosan,

Menthol,

Retinol (Vitamin A),

Koffein,

pflanzliche Proteine und deren Hydrolyseprodukte,

Carotine und

Jojobaöl

da diese

zum Gleichgewicht der cutanen Hydrolipidschicht beitragen,

dem Wasserverlust und damit der Faltenbildung vorbeugen,

die Haut erfrischen und Ermüdungserscheinungen entgegenwirken,

der Haut ein weiches und elastisches Gefühl verleihen,

die Hautdrainage, die Zufuhr von Nährstoffen und die Blutzirkulation verbessern,

gegen oxidativen Stress, Umweltgifte, Hautalterung und freie Radikale wirken,

> den durch Wasser und Sonne bewirkten Verlust an Fetten ausgleichen,

die Wasserbeständigkeit von UV-Filtern verbessern,

eine homogene Bräunung gewährleisten und schließlich zudem auch

antimikrobielle Eigenschaften besitzen.

The selection of the active ingredients is not critical in itself and depends on which effect is to be effected on the skin. Preference is given to active ingredients which have moisturizing properties, counteract cellulite and / or are self-tanning. Typical examples are tocopherol, tocopherol acetate, tocopherol palmitate, carotenes, caffeine, ascorbic acid, (deoxy) ribonucleic acid and their fragmentation products, β-glucans, retinol, bisabolol, allantoin, phytantriol, panthenol, AHA acids, amino acids, ceramides, pseudoceramides, chitosan, dihydroxyacetone Menthol, squalane, essential oils (eg jojoba oil), vegetable proteins and their hydrolysis products, plant extracts, such as Prunus extract, Bambaranussextrakt and vitamin complexes to understand. Particularly preferred is the use of

squalane,

chitosan,

Menthol,

Retinol (vitamin A),

Caffeine,

vegetable proteins and their hydrolysis products,

Carotenes and

jojoba oil

this one

contribute to the balance of the cutaneous hydrolipid layer,

prevent water loss and wrinkling,

refresh the skin and counteract signs of fatigue,

give the skin a soft and elastic feeling,

improve skin drainage, nutrient intake and blood circulation,

act against oxidative stress, environmental toxins, skin aging and free radicals,

> compensate for the loss of fats caused by water and sun,

improve the water resistance of UV filters,

ensure a homogeneous browning and finally also

possess antimicrobial properties.

The proportion of active ingredients in the microcapsules can be 1 to 30, preferably 5 to 25 and in particular 15 to 20 wt .-% amount.

microcapsules

The term "microcapsule" is the expert spherical units with a Diameter in the range of about 0.0001 to about 5 mm understood that at least one solid or liquid core enclosed by at least one continuous shell is. More specifically, it is finely dispersed with film-forming polymers liquid or solid phases, during their preparation, the polymers after emulsification and coacervation or interfacial polymerization on the material to be coated. Another method involves collecting molten waxes in a matrix ("microsponge"), which additionally envelops as microparticles with film-forming polymers could be. The microscopic capsules, also called nanocapsules, can be left like drying powder. Besides mononuclear microcapsules are also multinucleated aggregates, too Microspheres, known as the two or more cores in the continuous shell material distributed. Mononuclear or polynuclear microcapsules can also from an additional second, third, etc. sheath be enclosed. The shell can be made of natural, semisynthetic or synthetic materials. Of course, wrapping materials are for example rubber Arabic, agar-agar, agarose, maltodextrins, alginic acid or its salts, e.g. Sodium or Calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithins, gelatin, Albumin, shellac, polysaccharides such as starch or dextran, polypeptides, protein hydrolysates, Sucrose and waxes. Semi-synthetic shell materials are, inter alia, chemical modified celluloses, in particular cellulose esters and ethers, e.g. Cellulose acetate, ethylcellulose, Hydroxypropylcellulose, hydroxypropylmethylcellulose and carboxymethylcellulose, and starch derivatives, in particular starch ethers and esters. Synthetic wrapping materials are, for example, polymers such as polyacrylates, polyamides, polyvinyl alcohol or polyvinylpyrrolidone.

Examples of microcapsules of the prior art are the following commercial products (in parentheses is the shell material): Hallcrest Microcapsules (gelatin, gum arabic), Coletica Thalaspheres (marine collagen), Lipotec Millicapseln (alginic acid, agar-agar), Induchem Unispheres (lactose , microcrystalline cellulose, hydroxypropylmethylcellulose); Unicerin C30 (lactose, microcrystalline cellulose, hydroxypropylmethylcellulose), Kobo Glycospheres (modified starch, fatty acid esters, phospholipids), Softspheres (modified agar-agar) and Kuhs Probiol Nanospheres (phospholipids) as well as Primaspheres and Primasponges (chitosan, alginates) and Primasys (phospholipids) ,

(a1) aus Gelbildnern, Chitosanen und Wirkstoffen eine Matrix zubereitet,

(a2) gegebenenfalls die Matrix in einer Ölphase dispergiert,

(a3) die gegebenenfalls dispergierte Matrix mit wässrigen Lösungen anionischer Polymere behandelt und gegebenenfalls dabei die Ölphase entfernt.

oder

(b1) aus Gelbildnern, anionischen Polymeren und Wirkstoffen eine Matrix zubereitet,

(b2) gegebenenfalls die Matrix in einer Ölphase dispergiert,

(b3) die gegebenenfalls dispergierte Matrix mit wässrigen Chitosanlösungen behandelt und gegebenenfalls dabei die Ölphase entfernt.

oder

(c1) wässrige Wirkstoffzubereitungen mit Ölkörpern in Gegenwart von Emulgatoren zu O/W-Emulsionen verarbeitet,

(c2) die so erhaltenen Emulsionen mit wässrigen Lösungen anionischer Polymere behandelt,

(c3) die so erhaltene Matrix mit wässrigen Chitosanlösungen in Kontakt bringt und

(c4) die so erhaltenen Verkapselungsprodukte von der wässrigen Phase abtrennt.

Chitosan microcapsules and processes for their preparation are the subject of prior patent applications by the Applicant [WO 01/01926, WO 01/01927, WO 01/01928, WO 01/01929]. Microcapsules with average diameters in the range of 0.0001 to 5, preferably 0.001 to 0.5 and in particular 0.005 to 0.1 mm, consisting of an enveloping membrane and a matrix containing the active ingredients can be obtained, for example, by

(a1) preparing a matrix from gelling agents, chitosans and active substances,

(a2) optionally dispersing the matrix in an oil phase,

(a3) treating the optionally dispersed matrix with aqueous solutions of anionic polymers and optionally removing the oil phase.

or

(b1) preparing a matrix from gelling agents, anionic polymers and active substances,

(b2) optionally dispersing the matrix in an oil phase,

(b3) treating the optionally dispersed matrix with aqueous chitosan solutions and optionally removing the oil phase.

or

(c1) processed aqueous preparations of active substances with oil bodies in the presence of emulsifiers to O / W emulsions,

(c2) treating the emulsions thus obtained with aqueous solutions of anionic polymers,

(c3) contacting the resulting matrix with aqueous chitosan solutions, and

(c4) separating the thus obtained encapsulation products from the aqueous phase.

gelling agent

For the purposes of the invention, such substances are preferably considered as gelling agents, which show the property in aqueous solution at temperatures above 40 ° C gels to build. Typical examples are heteropolysaccharides and proteins. As thermogeling Heteropolysaccharides are preferably suitable agaroses, which in the form of Red algae to be obtained agar-agar also together with up to 30 wt .-% non-gel-forming Agaropectins may be present. Main component of the agaroses are linear polysaccharides from D-galactose and 3,6-anhydro-L-galactose, alternately β-1,3- and β-1,4-glycosidic are linked. The heteropolysaccharides preferably have a molecular weight in the range from 110,000 to 160,000 and are both colorless and tasteless. As alternatives Pectins, xanthans (also xanthan gum) and their mixtures come into question. There are furthermore preference is given to those types which still form gels in 1% strength by weight aqueous solution, which do not melt below 80 ° C and solidify again above 40 ° C. From the group of thermogelling proteins are exemplified the various Called gelatin types.

chitosan

Chitosans are biopolymers and are counted among the group of hydrocolloids. Chemically, they are partially deacetylated chitins of different molecular weight containing the following - idealized - monomer unit:

In contrast to most hydrocolloids, which are negative in the range of biological pHs Chitosans under these conditions are cationic biopolymers positively charged chitosans can interact with oppositely charged surfaces occur and are therefore used in cosmetic hair and body care as well as pharmaceutical Preparations used. For the production of chitosans one goes from chitin, preferably the shell remnants of crustaceans made as cheap raw materials in large Quantities are available. The chitin is thereby in a procedure, the first of Hackmann et al. has been described, usually first by addition of bases deproteinized, demineralized by the addition of mineral acids and finally by addition deacetylated by strong bases, with the molecular weights distributed over a broad spectrum could be. Preferably, such types are used as the average Have molecular weight of 10,000 to 500,000 or 800,000 to 1,200,000 daltons and / or a viscosity according to Brookfield (1 wt .-% in glycolic acid) below 5000 mPas, a degree of deacetylation in the range of 80 to 88% and an ash content of less than 0.3% by weight. For reasons of better water solubility, the Chitosans usually in the form of their salts, preferably used as glycolates.

oil phase

The matrix may optionally be dispersed in an oil phase prior to the formation of the membrane. As oils for this purpose, for example, Guerbet alcohols based on fatty alcohols having 6 to 18, preferably 8 to 10 carbon atoms, esters of linear C ₆ -C ₂₂ fatty acids with linear C ₆ -C ₂₂ fatty alcohols, esters of branched C ₆ -C ₁₃ carboxylic acids with linear C ₆ -C ₂₂ -fatty alcohols, such as myristyl myristate, myristyl palmitate, myristyl stearate, Myristylisostearat, myristyl, Myristylbehenat, Myristylerucat, cetyl myristate, cetyl palmitate, cetyl stearate, Cetylisostearat, cetyl oleate, cetyl behenate, Cetylerucat, Stearylmyristat, stearyl palmitate, stearyl stearate, Stearylisostearat , stearyl oleate, stearyl behenate, Stearylerucat, isostearyl, isostearyl palmitate, Isostearylstearat, isostearyl isostearate, Isostearyloleat, isostearyl behenate, Isostearyloleat, oleyl myristate, oleyl palmitate, oleyl stearate, oleyl isostearate, oleyl oleate, Oleylbehenat, oleyl erucate, behenyl myristate, behenyl palmitate, behenyl, Behenylisostearat, behenyl oleate, behenyl behenate, Behenyleru cat, erucyl myristate, erucyl palmitate, erucyl stearate, erucyl isostearate, erucyl oleate, erucyl behenate and erucyl erucate. In addition, esters of linear C ₆ -C ₂₂ fatty acids with branched alcohols, in particular 2-ethylhexanol, esters of hydroxycarboxylic acids with linear or branched C ₆ -C ₂₂ fatty alcohols, in particular dioctyl malates, esters of linear and / or branched fatty acids with polyhydric alcohols (such as propylene glycol, dimerdiol or trimer triol) and / or Guerbet alcohols, triglycerides based on C ₆ -C ₁₀ fatty acids, liquid mono- / di- / triglyceride mixtures based on C ₆ -C ₁₈ fatty acids, esters of C ₆ -C ₂₂ -fatty alcohols and / or Guerbet alcohols with aromatic carboxylic acids, in particular benzoic acid, esters of C ₂ -C ₁₂ -dicarboxylic acids with linear or branched alcohols having 1 to 22 carbon atoms or polyols having 2 to 10 carbon atoms and 2 to 6 hydroxyl groups, vegetable oils, branched primary alcohols, substituted cyclohexanes, linear and branched C ₆ -C ₂₂ fatty alcohol carbonates, guerbet carbonates, esters of benzoic acid with li linear and branched C ₆ -C ₂₂ -alcohols (eg Finsolv® TN), linear or branched, symmetrical or unsymmetrical dialkyl ethers having 6 to 22 carbon atoms per alkyl group, ring-opening products of epoxidized fatty acid esters with polyols, silicone oils and / or aliphatic or naphthenic Hydrocarbons such as squalane, squalene or dialkylcyclohexanes into consideration.

anionic polymers

The anionic polymers have the task of forming membranes with the chitosans. Salts of alginic acid are preferably suitable for this purpose. Alginic acid is a mixture of carboxyl-containing polysaccharides with the following idealized monomer unit:

The average molecular weight of the alginic acids or alginates is in the range from 150,000 to 250,000. Here, as salts of alginic acid, both their complete as Also to understand their partial neutralization products, in particular the alkali metal salts and among these, preferably the sodium alginate ("algin") and the ammonium and alkaline earth salts. especially preferred are mixed alginates, e.g. Sodium / magnesium or sodium / calcium alginates. In an alternative embodiment of the invention come for this Purpose, however, also anionic chitosan derivatives, such. Carboxylation and especially Succinylierungsprodukte in question. Alternatively, poly (meth) acrylates come with average Molecular weights in the range of 5,000 to 50,000 daltons and the various Carboxymethyl celluloses in question. Instead of the anionic polymers can be used for the Formation of the envelope membrane also anionic surfactants or low molecular weight inorganic Salts, such as pyrophosphates are used.

emulsifiers

Anlagerungsprodukte von 2 bis 30 Mol Ethylenoxid und/ oder 0 bis 5 Mol Propylenoxid an lineare Fettalkohole mit 8 bis 22 C-Atomen, an Fettsäuren mit 12 bis 22 C-Atomen, an Alkylphenole mit 8 bis 15 C-Atomen in der Alkylgruppe sowie Alkylamine mit 8 bis 22 Kohlenstoffatomen im Alkylrest;

Alkyl- und/oder Alkenyloligoglykoside mit 8 bis 22 Kohlenstoffatomen im Alk(en)ylrest und deren ethoxylierte Analoga;

Anlagerungsprodukte von 1 bis 15 Mol Ethylenoxid an Ricinusöl und/oder gehärtetes Ricinusöl;

Anlagerungsprodukte von 15 bis 60 Mol Ethylenoxid an Ricinusöl und/oder gehärtetes Ricinusöl;

Partialester von Glycerin und/oder Sorbitan mit ungesättigten, linearen oder gesättigten, verzweigten Fettsäuren mit 12 bis 22 Kohlenstoffatomen und/oder Hydroxycarbonsäuren mit 3 bis 18 Kohlenstoffatomen sowie deren Addukte mit 1 bis 30 Mol Ethylenoxid;

Partialester von Polyglycerin (durchschnittlicher Eigenkondensationsgrad 2 bis 8), Polyethylenglycol (Molekulargewicht 400 bis 5000), Trimethylolpropan, Pentaerythrit, Zuckeralkoholen (z.B. Sorbit), Alkylglucosiden (z.B. Methylglucosid, Butylglucosid, Laurylglucosid) sowie Polyglucosiden (z.B. Cellulose) mit gesättigten und/oder ungesättigten, linearen oder verzweigten Fettsäuren mit 12 bis 22 Kohlenstoffatomen und/oder

Hydroxycarbonsäuren mit 3 bis 18 Kohlenstoffatomen sowie deren Addukte mit 1 bis 30 Mol Ethylenoxid;

Mischester aus Pentaerythrit, Fettsäuren, Citronensäure und Fettalkohol und/oder

Mischester von Fettsäuren mit 6 bis 22 Kohlenstoffatomen, Methylglucose und Polyolen, vorzugsweise Glycerin oder Polyglycerin.

Mono-, Di- und Trialkylphosphate sowie Mono-, Di- und/oder Tri-PEG-alkylphosphate und deren Salze;

Wollwachsalkohole;

Polysiloxan-Polyalkyl-Polyether-Copolymere bzw. entsprechende Derivate;

Block-Copolymere z.B. Polyethylenglycol-30 Dipolyhydroxystearate;

Polymeremulgatoren, z.B. Pemulen-Typen (TR-1,TR-2) von Goodrich;

Polyalkylenglycole sowie

Glycerincarbonat.

Ethylenoxidanlagerungsprodukte

Examples of suitable emulsifiers are nonionic surfactants from at least one of the following groups:

Addition products of 2 to 30 moles of ethylene oxide and / or 0 to 5 moles of propylene oxide to linear fatty alcohols having 8 to 22 carbon atoms, to fatty acids having 12 to 22 carbon atoms, to alkylphenols having 8 to 15 carbon atoms in the alkyl group and alkylamines with 8 to 22 carbon atoms in the alkyl radical;

Alkyl and / or alkenyl oligoglycosides having 8 to 22 carbon atoms in the alk (en) ylrest and their ethoxylated analogs;

Addition products of 1 to 15 moles of ethylene oxide with castor oil and / or hydrogenated castor oil;

Addition products of 15 to 60 moles of ethylene oxide with castor oil and / or hydrogenated castor oil;

Partial esters of glycerol and / or sorbitan with unsaturated, linear or saturated, branched fatty acids having 12 to 22 carbon atoms and / or hydroxycarboxylic acids having 3 to 18 carbon atoms and their adducts with 1 to 30 moles of ethylene oxide;

Partial esters of polyglycerol (average intrinsic degree of condensation 2 to 8), polyethylene glycol (molecular weight 400 to 5000), trimethylolpropane, pentaerythritol, sugar alcohols (eg sorbitol), alkylglucosides (eg methylglucoside, butylglucoside, laurylglucoside) and polyglucosides (eg cellulose) with saturated and / or unsaturated , linear or branched fatty acids having 12 to 22 carbon atoms and / or

Hydroxycarboxylic acids having 3 to 18 carbon atoms and their adducts with 1 to 30 moles of ethylene oxide;

Mixed esters of pentaerythritol, fatty acids, citric acid and fatty alcohol and / or

Mixed esters of fatty acids having 6 to 22 carbon atoms, methyl glucose and polyols, preferably glycerol or polyglycerol.

Mono-, di- and trialkyl phosphates and mono-, di- and / or tri-PEG-alkyl phosphates and their salts;

Lanolin alcohol;

Polysiloxane-polyalkyl-polyether copolymers or corresponding derivatives;

Block copolymers, for example, polyethylene glycol-30 dipolyhydroxystearates;

Polymer emulsifiers, eg Pemulen types (TR-1, TR-2) from Goodrich;

Polyalkylene glycols as well

Glycerol carbonate.

Ethylene Oxide

The addition products of ethylene oxide and / or of propylene oxide onto fatty alcohols, fatty acids, alkylphenols or castor oil are known, commercially available products. These are homolog mixtures whose mean degree of alkoxylation corresponds to the ratio of the amounts of ethylene oxide and / or propylene oxide and substrate, with which the addition reaction is carried out corresponds. C _12/18 fatty acid _mono- and diesters of addition products of ethylene oxide with glycerol are known as refatting agents for cosmetic preparations.

Alkyl and / or alkenyl oligoglycosides

Alkyl and / or alkenyl oligoglycosides, their preparation and their use are made known in the art. Their preparation is carried out in particular by implementation of glucose or oligosaccharides with primary alcohols of 8 to 18 carbon atoms. With regard to the glycoside radical, it is true that both monoglycosides in which a cyclic sugar residue is glycosidically linked to the fatty alcohol, as well as oligomeric Glycosides with a degree of oligomerization to preferably about 8 are suitable. Of the The degree of oligomerization is a statistical mean, the one for such technical Products usual homolog distribution is based.

partial glycerides

Typical examples of suitable partial glycerides are hydroxystearic acid monoglyceride, Hydroxystearic acid diglyceride, isostearic acid monoglyceride, isostearic acid diglyceride, Oleic acid monoglyceride, oleic acid diglyceride, ricinoleic acid glyceride, ricinoleic acid diglyceride, Linoleic acid monoglyceride, linoleic acid diglyceride, linolenic acid monoglyceride, linolenic acid diglyceride, Erucic acid monoglyceride, erucic acid diglyceride, tartaric acid monoglyceride, Tartaric acid diglyceride, citric acid monoglyceride, citric acid diglyceride, malic acid monoglyceride, Malic acid diglyceride and their technical mixtures subordinated from the manufacturing process may still contain small amounts of triglyceride. Also suitable addition products of 1 to 30, preferably 5 to 10 moles of ethylene oxide to the said partial glycerides.

sorbitan

The sorbitan esters are sorbitan monoisostearate, sorbitan sesquiisostearate, sorbitan diisostearate, Sorbitan triisostearate, sorbitan monooleate, sorbitan sesquioleate, sorbitan dioleate, Sorbitan trioleate, sorbitan monoerucate, sorbitan sesquierucate, sorbitan butucate, Sorbitan trierucate, sorbitan monoricinoleate, sorbitan squiricinoleate, sorbitan dianicinoleate, Sorbitan triricinoleate, sorbitan monohydroxystearate, sorbitan sesquihydroxystearate, sorbitan dihydroxystearate, Sorbitan trihydroxystearate, sorbitan monotartrate, sorbitan sesquitartrate, Sorbitan ditartrate, sorbitan tritartrate, sorbitan monocitrate, sorbitan sesqui citrate, Sorbitan citrate, sorbitan tricitrate, sorbitan monomaleate, sorbitan sesquimaleate, sorbitol adimaleate, Sorbitan trimaleate and their technical mixtures. Also suitable Addition products of 1 to 30, preferably 5 to 10 moles of ethylene oxide to the mentioned Sorbitan.

polyglycerol

Typical examples of suitable polyglycerol esters are polyglyceryl-2 dipolyhydroxystearates (Dehymuls® PGPH), polyglycerol-3-diisostearate (Lameform® TGI), polyglyceryl-4 Isostearates (Isolan® GI 34), polyglyceryl-3 oleates, diisostearoyl polyglyceryl-3 Diisostearate (Isolan® PDI), Polyglyceryl-3 Methylglucose Distearate (Tego Care® 450), polyglyceryl-3 beeswax (Cera Bellina®), polyglyceryl-4 caprate (polyglycerol Caprate T2010 / 90), polyglyceryl-3 cetyl ether (Chimexane® NL), polyglyceryl-3 Distearates (Cremophor® GS 32) and polyglyceryl polyricinoleates (Admul® WOL 1403) Polyglyceryl dimerate isostearates and mixtures thereof. Examples of other suitable Polyol esters are the mono-, optionally reacted with 1 to 30 moles of ethylene oxide, Di- and triesters of trimethylolpropane or pentaerythritol with lauric acid, coconut fatty acid, Tallow fatty acid, palmitic acid, stearic acid, oleic acid, behenic acid and the like.

Anionic emulsifiers

Typical anionic emulsifiers are aliphatic fatty acids having 12 to 22 carbon atoms, such as palmitic acid, stearic acid or behenic acid, and dicarboxylic acids with 12 to 22 carbon atoms, such as azelaic acid or sebacic acid.

Amphoteric and cationic emulsifiers

Furthermore, zwitterionic surfactants can be used as emulsifiers. Zwitterionic surfactants are those surface-active compounds which carry at least one quaternary ammonium group and at least one carboxylate and one sulfonate group in the molecule. Particularly suitable zwitterionic surfactants are the so-called betaines such as the N-alkyl-N, N-dimethylammoniumglycinate, for example Kokosalkyldimethylammoniumglycinat, N-acylaminopropyl-N, N-dimethylammoniumglycinate, for example Kokosacylaminopropyldimethylammoniumglycinat, and 2-alkyl-3-carboxylmethyl-3-hydroxyethylimidazoline each having 8 to 18 carbon atoms in the alkyl or acyl group and the Kokosacylaminoethylhydroxyethylcarboxymethylglycinat. Particularly preferred is the fatty acid amide derivative known under the CTFA name Cocamidopropyl Betaine . Also suitable emulsifiers are ampholytic surfactants. Ampholytic surfactants are understood as meaning those surface-active compounds which, apart from a C _8/18 -alkyl or acyl group in the molecule, contain at least one free amino group and at least one -COOH or -SO ₃ H group and are capable of forming internal salts. Examples of suitable ampholytic surfactants are N-alkylglycines, N-alkylpropionic acids, N-alkylaminobutyric acids, N-alkylirninodipropionic acids, N-hydroxyethyl-N-alkylamidopropylglycines, N-alkyltaurines, N-alkylsarcosines, 2-alkylaminopropionic acids and alkylaminoacetic acids each having about 8 to 18 C In the alkyl group. Particularly preferred ampholytic surfactants are N-cocoalkylaminopropionate, cocoacylaminoethylaminopropionate and C _12/18 acylsarcosine. Finally, cationic surfactants are also suitable as emulsifiers, those of the esterquat type, preferably methyl-quaternized difatty acid triethanolamine ester salts, being particularly preferred.

Production process microcapsules

For the preparation of the microcapsules is usually 1 to 10, preferably 2 to 5 Wt .-% aqueous solution of the gelling agent, preferably the agar agar forth and heated these under reflux. In the boiling heat, preferably at 80 to 100 ° C, a second aqueous solution containing the chitosan in amounts of 0.1 to 2, preferably 0.25 to 0.5 wt .-% and the active ingredients in amounts of 0.1 to 25 and in particular 0.25 to 10 Wt .-% contains; this mixture is called a matrix. The loading of the microcapsules with active ingredients can therefore also be 0.1 to 25 wt .-% based on the capsule weight. If desired, at this time for viscosity adjustment also water-insoluble Ingredients, for example, inorganic pigments are added, wherein these are usually added in the form of aqueous or aqueous / alcoholic dispersions. to Emulsification or dispersion of the active ingredients may also be of benefit to the matrix Add emulsifiers and / or solubilizers. After making the matrix out Gelbildner, chitosan and the active ingredients, the matrix can optionally in an oil phase under strong Shear be very finely dispersed to the next encapsulation as possible to produce small particles. It has proved to be particularly advantageous, the matrix to warm to temperatures in the range of 40 to 60 ° C, while the oil phase to 10 cools to 20 ° C. In the last, now again obligatory step then the actual takes place Encapsulation, i. the formation of the envelope membrane by contacting the chitosan in the matrix with the anionic polymers. For this purpose, it is recommended that in the Oil phase dispersed matrix at a temperature in the range of 40 to 100, preferably 50 to 60 ° C with an aqueous, about 1 to 50 and preferably 10 to 15 wt .-% aqueous To treat solution of the anion polymer and thereby - if necessary - simultaneously or subsequently remove the oil phase. The resulting aqueous preparations have usually a microcapsule content in the range of 1 to 10 wt .-% on. In some Cases, it may be advantageous if the solution of the polymers contains other ingredients, For example, emulsifiers or preservatives. After filtration, microcapsules which on average has a diameter in the range of preferably about 1 mm have. It is advisable to sieve the capsules in order to obtain a uniform size distribution sure. The microcapsules obtained in this way can be manufactured Frame have any shape, but they are preferably approximately spherical. Alternatively, one can also use the anionic polymers for the preparation of the matrix and perform encapsulation with chitosans.

In an alternative process, the preparation of the microcapsules according to the invention is used First, an O / W emulsion is prepared, which in addition to the oil body, water and the Active ingredients contains an effective amount of emulsifier. This is used to make the matrix Preparation with vigorous stirring with an appropriate amount of an aqueous anionic polymer solution added. The membrane formation takes place by adding the chitosan solution. The whole Operation preferably takes place in the weakly acidic range at pH = 3 to 4. If Required, the pH adjustment by addition of mineral acid. After membrane formation the pH is raised to 5 to 6, for example by adding triethanolamine or another base. This leads to an increase in the viscosity, the Addition of further thickening agents, e.g. Polysaccharides, especially xanthan gum, Guar-guar, agar-agar, alginates and tyloses, carboxymethylcellulose and hydroxyethylcellulose, high molecular weight polyethylene glycol mono- and diesters of fatty acids, polyacrylates, Polyacrylamides and the like can still be supported. To conclude the microcapsules of the aqueous phase, for example by decantation, filtration or Centrifuged separated.

binder

(b1) polymeren Melaminverbindungen,

(b2) polymeren Glyoxalverbindungen,

(b3) polymeren Siliconverbindungen,

(b4) epichlorhydrinvernetzten Polyamidoaminen,

(b5) Poly(meth)acrylaten,

(b6) Polyalkylenglycolen und

(b7) polymeren Fluorkohlenwasserstoffen.

The suitable binders for the purposes of the invention may be selected from the group formed by

(b1) polymeric melamine compounds,

(b2) polymeric glyoxal compounds,

(b3) polymeric silicone compounds,

(b4) epichlorohydrin-crosslinked polyamidoamines,

(b5) poly (meth) acrylates,

(b6) polyalkylene glycols and

(b7) polymeric fluorohydrocarbons.

While the binders (b1) to (b4) are preferably for the production of microencapsulated Active ingredient preparations are suitable with which the fibers or textile fabrics are impregnated the binders (b5) to (b7) are preferably used for such preparations Use that are applied by forced application.

Polymeric melamine compounds

Melamine (synonym: 2,4,6-triamino-1,3,5-triazine) is usually formed by trimerization of dicyandiamide or by cyclization of urea with elimination of carbon dioxide and ammonia according to the following equation:

For the purposes of the invention, melamine leads to oligomeric or polymeric condensation products melamine with formaldehyde, urea, phenol or mixtures thereof Understood.

Polymeric glyoxal compounds

Glyoxal (synonym: oxaldehyde, ethanedial) is formed during the vapor-phase oxidation of Ethylene glycol with air in the presence of silver catalysts. Within the meaning of the invention Glyoxals are the self-condensation products of glyoxal ("polyglyoxals") Understood.

Polymeric silicone compounds

Suitable silicone compounds are, for example, dimethylpolysiloxanes, methylphenylpolysiloxanes, cyclic silicones and amino, fatty, alcohol, polyether, epoxy, fluoro-, glycoside- and / or alkyl-modified silicone compounds at room temperature preferably solid or resinous. Also suitable are simethicones, which are mixtures of dimethicones with an average chain length from 200 to 300 dimethylsiloxane units and hydrogenated silicates.

Epichlorohydrin crosslinked polyamidoamines

i) Polyaminoamide werden (a) zunächst mit einer Menge von 5 bis 30 Mol-% - bezogen auf den zur Quaternierung zur Verfügung stehenden Stickstoff - eines Quaternierungsmittels umgesetzt, und (b) anschließend die resultierenden quaternierten Polyaminoamide mit einer dem Gehalt an nicht quaterniertem Stickstoff entsprechenden molaren Menge Epichlorhydrin vernetzt, oder

ii) Polyaminoamide werden (a) zunächst bei 10 bis 35°C mit einer Menge von 5 bis 40 Mol-% - bezogen auf den für die Vernetzung zur Verfügung stehenden Stickstoff - Epichlorhydrin umgesetzt, und (b) das Zwischenprodukt auf einen pH-Wert im Bereich von 8 bis 11 einstellt und bei einer Temperatur im Bereich von 20 bis 45°C mit einer weiteren Menge Epichlorhydrin vernetzt, so dass das molare Einsatzverhältnis in Summe 90 bis 125 Mol-% - bezogen auf den für die Vernetzung zur Verfügung stehenden Stickstoff- beträgt.

Epichlorohydrin-crosslinked polyamidoamines, also referred to as "fibrabones" or "wet strength resins", are well known in textile and paper technology. Their preparation is preferably based on two methods:

i) Polyaminoamides are (a) first reacted with an amount of 5 to 30 mol%, based on the nitrogen available for quaternization, of a quaternizing agent, and (b) subsequently the resulting quaternized polyaminoamides having a content of unquaternized nitrogen corresponding molar amount of epichlorohydrin crosslinked, or

ii) Polyaminoamides are (a) reacted first at 10 to 35 ° C in an amount of 5 to 40 mol% based on the nitrogen available for the crosslinking of epichlorohydrin, and (b) the intermediate product to a pH in the range from 8 to 11 and cross-linked at a temperature in the range of 20 to 45 ° C with a further amount of epichlorohydrin, so that the molar use ratio in total from 90 to 125 mol% - based on the nitrogen available for the crosslinking - is.

Poly (meth) acrylates

The term poly (meth) acrylates homo- and copolymerization of the Acrylic acid, methacrylic acid and optionally their esters, especially their esters with lower alcohols, e.g. Methanol, ethanol, isopropyl alcohol, the isomeric butanols, Cyclohexanol and the like, which in a conventional manner, for example, be obtained by radical polymerization under UV irradiation. Typically, the average molecular weight of the polymers is between 100 and 10,000, preferably 200 and 5,000 and especially 400 to 2,000 daltons.

polyalkylene

The term polyalkylene glycols are homo- and copolymerization products of Ethylene, propylene and optionally the butylene oxide to understand. The condensation The alkylene oxides can be prepared in a manner known per se in the presence of alkaline catalysts although acid catalysis is preferred. For example, mixtures become used by ethylene oxide and propylene oxide, the polymers may be a block or Have random distribution. Typically, the average molecular weight of the Polymers between 100 and 10,000, preferably at 200 and 5,000 and in particular 400 to 2,000 daltons.

quantities

The feed ratio between microcapsules and binder may be 90:10 to 10:90, preferably 75: 25 to 25: 75 and especially 60: 40 to 40: 60 parts by weight. ever According to manufacturing method and use ratio of microcapsules and binders may be different Liability types are realized. When using a smaller amount of binder (For example, weight ratio of microcapsules: binder greater than 50: 50) adhere the Microcapsules in a layer of the binder on the fibrils, which causes it when Contribute to direct contact between the envelope membrane and the skin surface comes. It is obvious that this type of adhesion ("carrier type") due to mechanical Friction very quickly leads to a release of the active ingredient. On the other hand, a larger amount of binder used (for example, weight ratio of microcapsules: binder less than 50:50), so this is usually sufficient to not only the microcapsules to staple to the fibers, but to envelop or provide it with a coating ("igloo type"). Microcapsules of fibers thus treated are not immediately in contact in contact with the skin surface, which causes them in less Quantities are delivered, but are also effective over a longer period. (see illustrations 1 and 2). In general, the preparations are in the form of aqueous dispersions in the trade, having a solids content in the range of 5 to 50, preferably 10 to 40 and especially 15 to 30 wt .-% have.

Industrial Applicability

The preparations of microencapsulated active ingredients and binders serve to fibers and all types of textile fabrics, ie both finished and semi-finished products during the manufacturing process or even after its completion to equip to this Way to improve the wearing comfort on the skin. The selection of materials from which The fibers or textiles are, is thereby largely uncritical. This is how everyone comes common natural and synthetic materials and mixtures thereof, in particular but cotton, polyamides, polyester, viscose, polyamide / lycra, cotton / lycra and cotton / polyester. Equally uncritical is the selection of textiles, being natural Nearby is to equip such products that are in direct contact with the skin, ie especially underwear, swimwear, sleepwear, stockings and tights.

application method

Another object of the present invention relates to a first method of equipment of fibers or textile fabrics, in which the substrates with aqueous preparations containing the microencapsulated agents and the binders impregnated. The Impregnation can be done, for example, by placing the fibers or textiles in a commercial washing machine treated with the preparations of the invention or the application with the help of a dip bath makes.

Alternatively, another aspect of the invention relates to a second method of equipment of fibers and textile fabrics, in which the aqueous preparations containing the microencapsulated agents and binders are forcibly applied. Here are the to be equipped by a substances containing the microencapsulated agents and the binder Submerged drawn, the application then carried out via a press under pressure becomes.

Usually, the application concentration is 1 to 90, and preferably 5 to 60 Wt .-% based on the liquor or the dip. In the case of impregnation are generally higher concentrations than in the case of forced application by the same loadings the fibers or textile fabrics with the microencapsulated active ingredients to achieve.

(a) mikroverkapselte Wirkstoffe und

(b) Bindemittel

zur Ausrüstung von Fasern und textilen Flächengebilden. A final object of the invention finally relates to the use of mixtures containing

(a) microencapsulated agents and

(b) binder

for finishing fibers and textile fabrics.

Examples

Production Example H1. In a 500 ml three-necked flask with stirrer and reflux condenser, 3 g of agar-agar were dissolved in 200 ml of water in the boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Cognis, Dusseldorf / FRG), 5 g of squalane 0.5 g of Phenonip® (preservative mixture containing phenoxyethanol and parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in ad 100 g of water. The resulting matrix was filtered, heated to 60 ° C and dropped into a 0.5 wt .-% sodium alginate solution. After sieving, an aqueous formulation containing 8% by weight microcapsules with a mean diameter of 1 mm was obtained. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 40:60.

Production example H2. In a 500 ml three-necked flask with stirrer and reflux condenser, 3 g of agar-agar were dissolved in 200 ml of water in the boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Cognis, Dusseldorf / FRG), 5 g of tocopherol, 0.5 g of Phenonip® (preservative mixture containing phenoxyethanol and parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in ad 100 g of water. The resulting matrix was filtered, heated to 50 ° C and dispersed with vigorous stirring in 2.5 times the volume of paraffin oil, which had previously been cooled to 15 ° C. The dispersion was subsequently washed with an aqueous solution containing 1% by weight of sodium lauryl sulfate and 0.5% by weight of sodium alginate and then several times with a 0.5% strength by weight aqueous phenone solution, the oil phase being removed. After sieving, an aqueous formulation containing 8% by weight microcapsules with a mean diameter of 1 mm was obtained. Finally, the microcapsules - based on the solids content - were mixed with polymethacrylate (M = 8,000) in a weight ratio of 50:50.

Production Example H3. In a 500 ml three-necked flask with stirrer and reflux condenser, 3 g of agar-agar were dissolved in 200 ml of water in the boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Cognis, Dusseldorf / FRG), 5 g of caffeine, 0.5 g of Phenonip® (preservative mixture containing phenoxyethanol and parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in ad 100 g of water. The resulting matrix was filtered, heated to 60 ° C and added dropwise to a 15% by weight solution of sodium laureth sulfate. After sieving, an aqueous formulation containing 9% by weight microcapsules with a mean diameter of 1 mm was obtained. Finally, the microcapsules - based on the solids content - with a melamine-formaldehyde condensate (M = 8,000) in a weight ratio of 50: 50 mixed.

Production Example H4. In a 500 ml three-necked flask equipped with stirrer and reflux condenser dissolved in boiling heat 3 g agar-agar in 200 ml of water. Subsequently, the mixture became within about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in 100 g of water and then with a preparation of 25 g Chitosan (Hydagen® DCMF, 1% by weight in glycolic acid, Cognis, Dusseldorf / FRG), 5 g Menthol, 0.5 g Phenonip® (preservative mixture containing phenoxyethanol and Parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in 100 g of water. The obtained The matrix was filtered, heated to 60 ° C and into a 15% by weight solution of sodium pyrophosphate dripped. After sieving, an aqueous preparation was obtained which was 8 Wt .-% microcapsules with a mean diameter of 1 mm. In conclusion The microcapsules were - with respect to the solids content - with polyethylene glycol (M = 5,000) in a weight ratio of 70:30.

Production Example H5. In a 500 ml three-necked flask with stirrer and reflux condenser, 3 g of agar-agar were dissolved in 200 ml of water in the boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Cognis, Dusseldorf / FRG), 5 g of beta-carotene, 0.5 g of Phenonip® (preservative mixture containing phenoxyethanol and parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in ad 100 g of water. The matrix thus obtained was filtered, heated to 50 ° C and with vigorous stirring in 2.5 times the volume of paraffin oil, which had previously been cooled to 15 ° C, dispersed. The dispersion was then washed with a 15% by weight sodium pyrophosphate solution and then several times with a 0.5% by weight aqueous phenone solution to remove the oil phase. After sieving, an aqueous formulation containing 10% by weight microcapsules with a mean diameter of 1 mm was obtained. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 70:30.

Production Example H6. In a 500 ml three-necked flask equipped with stirrer and reflux condenser, 3 g of gelatin were dissolved in 200 ml of water at boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Henkel KGaA, Dusseldorf / FRG), 5 g of soy protein, 0.5 g of Phenonip® in ad 100 g of water. The resulting matrix was filtered, heated to 60 ° C and added dropwise to a 0.5% by weight solution of Hydagen® SCD (succinylated chitosan, Cognis). After sieving, an aqueous formulation containing 8% by weight microcapsules with a mean diameter of 1 mm was obtained. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 70:30.

Production Example H7. In a 500 ml three-necked flask with stirrer and reflux condenser, 3 g of agar-agar were dissolved in 200 ml of water in the boiling heat. The mixture was then added over about 30 minutes with vigorous stirring, first with a homogeneous dispersion of 10 g of glycerol and 2 g of talc in ad 100 g of water and then with a preparation of 25 g of chitosan (Hydagen® DCMF, 1 wt .-% in glycolic acid, Cognis, Dusseldorf / FRG), 5 g of jojoba oil, 0.5 g of Phenonip® (preservative mixture containing phenoxyethanol and parabens) and 0.5 g of polysorbate-20 (Tween® 20, ICI) in ad 100 g of water. The resulting matrix was filtered, heated to 60 ° C and dropped into a 0.5 wt .-% sodium alginate solution. To obtain microcapsules of the same diameter, the preparations were then sieved. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 70:30.

Production Example H8. In a stirring apparatus, 0.5 g of preservative (Phenonip®) were dissolved in 50 g of a 2% by weight aqueous preparation of carboxymethylcellulose and the mixture was adjusted to pH = 3.5. Subsequently, with vigorous stirring, a mixture consisting of 1 g of tocopherol and 0.5 g of sorbitan monostearate + 20EO (Eumulgin® SMS 20, Cognis Deutschland GmbH) was added. Thereafter, with further stirring, an amount of a 1% strength by weight solution of chitosan in glycolic acid (Hydagen® CMF Cognis Deutschland GmbH) was added so that a chitosan concentration of 0.075% by weight, based on the preparation, was established. Subsequently, the pH was raised to 5.5 by addition of triethanolamine and the resulting microcapsules were decanted. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 40:60.

Production Example H9. In a stirred apparatus, 0.5 g of preservative (Phenonip®) were dissolved in 50 g of a 2% by weight aqueous preparation of polyacrylic acid (Pemulen® TR-2), which resulted in a pH of 3. Subsequently, with vigorous stirring, a mixture consisting of 1 g of menthol and 0.5 g of sorbitan monolaurate + 15EO (Eumulgin® SML 15, Cognis Deutschland GmbH) was added. Thereafter, with further stirring, an amount of a 1% strength by weight solution of chitosan in glycolic acid (Hydagen® CMF Cognis Deutschland GmbH) was added so that a chitosan concentration of 0.01% by weight, based on the preparation, was established. Subsequently, the pH was raised to 5.5 by addition of triethanolamine and the resulting microcapsules were decanted. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 40:60.

Production Example H10. In a stirred apparatus, 0.5 g of preservative (Phenonip®) were dissolved in 50 g of a 2% by weight aqueous preparation of polyacrylic acid (Pemulen® TR-2), which resulted in a pH of 3. Then, with vigorous stirring, a mixture consisting of 1 g of caffeine and 0.5 g of Coco Glucosides (Plantacare APG 1200, Cognis Deutschland GmbH) was added. Thereafter, with further stirring, an amount of a 1% strength by weight solution of chitosan in glycolic acid (Hydagen® CMF Cognis Deutschland GmbH) was added so that a chitosan concentration of 0.01% by weight, based on the preparation, was established. Subsequently, the pH was raised to 5.5 by addition of triethanolamine and the resulting microcapsules were decanted. Finally, the microcapsules - based on the solids content - were mixed with polyethylene glycol (M = 5,000) in a weight ratio of 40:60.

Application Example 1. Commercially available tights were equipped with a microcapsule preparation according to Preparation Example H8 by forced application and tested by a volunteer panel consisting of 30 volunteers over a period of 8 to 48 h. After every 8 h, the residual content of active ingredients was determined. For comparison, the test series was repeated with tights that had been equipped with the same microcapsules but without the addition of the binder. The results are summarized in Table 1 and represent the respective mean values. Residual active ingredient content as a function of wearing time Wearing time [d] 0 8th 16 24 32 40 48 Active substance [% rel.] Inventive Example H8 100 90 82 78 72 62 62 Comparison without binder 100 80 71 59 40 32 18

It can be seen that the equipment with mixtures of microcapsules and binder to do so causes the drug to be delivered less rapidly.

Application example 2. Commercially available tights were equipped with a microcapsule preparation according to Preparation Example H8 by forced application and 30 times (a) in the washing machine (30 min, 20 ° C, 1 g / L mild detergent) or (b) by hand (15 min, 20 ° C, 1 g / L mild detergent). After each wash cycle, the residual content of active ingredients was determined. For comparison, the test series was again repeated with tights that had been equipped with the same microcapsules, but waiving the addition of the binder. The results are summarized in Table 2. Residual drug content as a function of wash cycles wash cycles 0 1 2 3 4 5 6 7 8th 9 10 15 20 25 30 Active substance [% rel.] For machine wash Inventive Example H8 100 70 58 50 42 40 38 37 33 30 28 22 20 18 16 Comparative example without binder 100 60 39 21 5 0 Active substance content [% rel.] For hand washing Inventive Example H8 100 90 88 82 78 76 74 72 71 70 69 52 45 42 41 Comparative example without binder 100 81 66 51 32 12 3 0

It can be seen that the equipment with mixtures of microcapsules and binder to do so causes the active ingredient to be washed out less rapidly in both machine and hand washing becomes.

Application Example 3. Commercially available tights were equipped with a microcapsule preparation according to Preparation Example H10 by forced application and worn by a volunteer panel consisting of 10 volunteers over a period of 6 h. Subsequently, the hydration of the skin was determined using an 805 PC corneometer versus the untreated condition. For comparison, the test series was again repeated with tights that had been equipped with the same microcapsules, but waiving the addition of the binder. The results are summarized in Table 3. Increase in hydration Family 1 2 3 4 5 6 7 8th 9 10 MW Increase in hydration [% rel.] Inventive Example H10 6 14 4 16 14 7 9 7 9 13 10 Comparative example without binder 5 12 7 8th 11 11 4 5 7 10 8th

It can be seen that in the case of the example according to the invention on average a higher hydration was achieved.

Claims (13)

Fibers and textile fabrics, characterized in that they are made with mixtures of (a) microencapsulated substances and (b) binders are equipped. Fibers and textile fabrics according to Claim 1, characterized in that they are provided with microencapsulated active substances selected from the group consisting of tocopherol, tocopherol acetate, tocopherol palmitate, carotenes, caffeine, ascorbic acid, (deoxy) ribonucleic acid and their fragmentation products, β-glucans, retinol, bisabolol, allantoin, phytantriol, panthenol, AHA acids, amino acids, ceramides, pseudoceramides chitosan, dihydroxyacetone, menthol, squalane, essential oils, vegetable proteins and their hydrolysis products and plant extracts and mixtures thereof. Fibers and textile fabrics according to claims 1 and / or 2, characterized in that the microcapsules have an active substance content of 1 to 30 wt .-%. Fibers and textile fabrics according to at least one of claims 1 to 3, characterized in that they are equipped with microcapsules with average diameters in the range of 0.0001 to 5 mm, consisting of an enveloping membrane and a matrix containing the active ingredients, which are obtainable thereby , that he (a1) preparing a matrix from gelling agents, chitosans and active substances, (a2) optionally dispersing the matrix in an oil phase, (a3) treating the optionally dispersed matrix with aqueous solutions of anionic polymers and optionally removing the oil phase. or (b1) preparing a matrix from gelling agents, anionic polymers and active substances, (b2) optionally dispersing the matrix in an oil phase, (b3) treating the optionally dispersed matrix with aqueous chitosan solutions and optionally removing the oil phase. or (c1) processed aqueous preparations of active substances with oil bodies in the presence of emulsifiers to O / W emulsions, (c2) treating the emulsions thus obtained with aqueous solutions of anionic polymers, (c3) contacting the resulting matrix with aqueous chitosan solutions, and (c4) separating the thus obtained encapsulation products from the aqueous phase. Fibers and textile fabrics according to at least one of claims 1 to 4, characterized in that they contain microcapsules having an average diameter in the range of 0.001 to 0.5 mm. Fibers and textile fabrics according to at least one of claims 1 to 5, characterized in that they are provided with binders selected from the group consisting of polymeric melamine compounds, polymeric glyoxal compounds, polymeric silicone compounds, epichlorohydrin-crosslinked polyamidoamines, polyalkylene glycols, poly ( meth) acrylates and polymeric fluorohydrocarbons and mixtures thereof. Fibers and textile fabrics according to at least one of claims 1 to 6, characterized in that they are equipped with mixtures of microcapsules and binders containing the two components in a weight ratio of 90: 10 to 10: 90. Process for finishing fibers or textile fabrics, in which the substrates with aqueous preparations containing microencapsulated active ingredients and binders impregnated. Process for finishing fibers and textile fabrics using the aqueous preparations containing the microencapsulated agents and the binders zwangsappliziert. Process according to claims 8 and / or 9, characterized in that the microencapsulated active substances and the binders are used in the form of aqueous dispersions. A method according to claim 10, characterized in that the aqueous dispersions have solids contents in the range of 5 to 90 wt .-%. Process according to claims 10 and / or 11, characterized in that the aqueous dispersions are diluted in use to a concentration of 1 to 60 wt .-%. Use of mixtures containing (a) microencapsulated agents and (b) binder for finishing fibers and textile fabrics.

Images