EP2108735B1 - Loadable fibres and textile sheets - Google Patents
Loadable fibres and textile sheets Download PDFInfo
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- EP2108735B1 EP2108735B1 EP08007156A EP08007156A EP2108735B1 EP 2108735 B1 EP2108735 B1 EP 2108735B1 EP 08007156 A EP08007156 A EP 08007156A EP 08007156 A EP08007156 A EP 08007156A EP 2108735 B1 EP2108735 B1 EP 2108735B1
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- Prior art keywords
- microspheres
- cognis
- pmma
- washes
- active ingredients
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
Definitions
- the invention is in the field of sustained release of active ingredients, in particular for the finishing of fibers and fabrics.
- the term "wearing comfort” summarizes the increased demands of the consumer, who no longer wants to be satisfied with the fact that the clothes he wears directly on the skin, such as lingerie or tights, neither scratch nor cause reddening of the skin, but are expected in the opposite way. that it has a positive effect on the condition of his skin. This can be either to remedy fatigue, as well as to convey a fresh scent or to avoid skin roughness. There has therefore been no lack of efforts to equip textiles, for example, women's tights, with cosmetic agents that merge when wearing on the skin and there cause the desired effects.
- Database WPI Week198848 (AN 1988-343069) and JP 63-256769 disclose a textile provided with a mixture of loaded porous microcapsules and film-forming polymers.
- Database WPI Week199019 (AN 1990-142321) and JP 02-084595 discloses a material that releases insecticides; it contains porous three-dimensional microcapsules that make an insecticide.
- US 2006/0264547 A1 describes refractory superabsorbent polymexes that can absorb many times their own weight in water. It also discloses a blend of superabsorbent microspheres loaded with flame retardant agents and a film forming binder.
- EP 1,600,210 Al describes loaded microspheres. It involves loading microspheres with active ingredients and then applying the loaded microspheres to textile surfaces where they are physically adsorbed without the use of binders. Although in this technical solution, a certain wash resistance is given, but this does not meet the highest requirements.
- WO 2006/015718 A1 describes fibers and fabrics which are characterized by being blended with mixtures of (a) hydrophobic actives and (b) binders.
- binders are agents without the mediation of microcapsules or the like applied to Textilobef lake, but not directly, but by means of film-forming polymers (binders). This technical solution lacks a controlled release of the active ingredients.
- wash permanence is to be understood that the above-mentioned desirable properties of the textiles are lessened by washing only to a limited extent.
- microspheres (a) are unloaded. They fulfill the function that they can be loaded by the user as desired and, after release of the active ingredients, can also be reloaded as desired.
- Absorbent microspheres are structures that have a largely homogeneous structure.
- the absorbent microspheres used in the context of the present invention have the property of being able to absorb and also release active substances, both of which can be done several times, ie. Active substances can be absorbed by loading or reloading and released again over time. Because of this property, these microspheres are referred to as absorbent microspheres.
- the term "absorbent" (* capable of taking active ingredients) will be omitted below and simply referred to as microspheres.
- the active ingredients can be adsorbed on the surface of the microspheres and / or dissolved in the microspheres and / or in the microspheres e.g. be embedded in fine channels.
- Microspheres are dimensionally stable, i. they are not destroyed in the release of the active ingredients. It should be expressly stated that microcapsules, which are indeed destroyed in the release of the active substances, do not fall under the definition of microspheres.
- microspheres are fixed by - one or more - film-forming polymers on the textile surface, resulting in a relative to the prior art, relative improvement of the washing permanence.
- microspheres are preferably spherical in shape, but are not limited in geometry to spheroidal shape, but may have other spatial shapes, for example, they may represent rotatiosellipsoids or have a rod shape.
- the microspheres preferably have an average particle size in the range of 1 to 15 microns, and more preferably 5 to 10 microns.
- microsphere based on polymethylmethacrylate is used.
- PMMA polymethylmethacrylate
- examples are, for example, Covabead LH 85 or LH 170 from the company LCW or Cosmedia PMMA V8, Cosmedia PMMA V 12 or Cosmedia SILC from Cognis.
- silicone-based or SiO 2 -based microspheres are used.
- examples are "Dow Corning 9509 Silicone Elastomer Suspension” from Dow Corning.
- microspheres based on polymethylmethacrylate are used.
- Suitable polyurethanes (PU) and polyethylvinyl acetates (EVA) are, for example, the commercially available products from the Cognis 3011-A or Cognis 3009-A range from Cognis.
- 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.
- melamine refers to oligomeric or polymeric condensation products of melamine with formaldehyde, urea, phenol or mixtures thereof.
- glyoxals are understood as meaning the self-condensation products of glyoxal ("polyglyoxals").
- Silicone compounds are, for example, dimethylpolysiloxanes, methylphenylpolysiloxanes, cyclic silicones and amino, fatty acid, alcohol, polyether, epoxy, fluorine, glycoside and / or alkyl-modified silicone compounds which are preferably solid or resin-form at room temperature.
- simethicones which are mixtures of dimethicones having an average chain length of from 200 to 300 dimethylsiloxane units and hydrogenated silicates.
- Particularly preferred is the use of aminosiloxanes, eg Cognis 3001 from Cognis. Their further crosslinking with H-siloxanes, eg Cognis 3002 from Cognis, can further increase the performance as a binder.
- Poly (meth) acrylates are homo- and copolymerization products of acrylic acid, methacrylic acid and optionally their esters, especially their esters with lower alcohols, such as methanol, ethanol, isopropyl alcohol, the isomeric butanols, cyclohexanol and the like to understand which are obtained in a conventional manner, for example by free-radical polymerization under UV irradiation.
- 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.
- the binders (b) - based on the component (a) - in amounts of 0.5 to 15, preferably 1 to 10 and especially 1 to 5 wt .-% applied to the fibers.
- Component (a) is to be understood as meaning the microspheres in unloaded form.
- active ingredients that are intended to load the microspheres are not critical per se and depends exclusively on which effect is to be effected on the skin.
- active ingredients are preferred which have moisturizing properties or counteract cellulite.
- Typical examples are tocopherol, tocopherol acetate, tocopherol palmitate, carotenes, caffeine, ascorbic acid, (deoxy) ribonucleic acid and their fragmentation products, ⁇ -glucans, retinol, bisabolol, allantoin, phytantriol, panthenol, AHA acids, amino acids, ceramides, pseudoceramides, chitosan, dihydroxyacetone , Menthol, squalane, essential oils (eg lavender oil, lemon oil, eucalyptus oil or peppermint oil), vegetable oils (eg Monoi de Tahiti, shea butter, almond oil, passion fruit oil, rosehip seed oil or apricot oil), vegetable proteins and their hydrolysis products, plant extracts, such as Extracts of Ginkgo biloba, Camellia sinensis, Trifolium pratensis, Oleacea europensis, Litchi sinensis, Valeriana oficinalis, Medicago s
- the active compounds from the group formed by essential oils, vegetable oils, squalane, chitosan, menthol, retinol (or vitamin A), caffeine, vegetable or animal proteins and their hydrolysis products, carotenes and jojoba oil.
- the weight ratio between the component (a) - such as the finely divided PMMA - and the active ingredients is 10: 90 to 99: 1, preferably 3: 1 to 1: 1 and more preferably about 2: 1.
- the "Covabed LH 85" microspheres were converted into a 10% by weight aqueous dispersion using the "Cognis 6003-A” surfactant in demineralized water.
- the dispersing unit used was an Ultra-Turrax type agitator).
- the dispersion thus prepared contained 10% by weight of PMMA microspheres.
- the dispersion is hereinafter referred to as DISP-1.
- PA / EL 76/24%) knit (knit fabric in which the yarn is made of 76% polyamide and 24% spandex (e.g., Lycra)) was impregnated with the following solution (liquor) by means of a laboratory padder:
- the "Cosmedia PMMA V8" microspheres were converted into a 10% by weight aqueous dispersion using the "Cognis 6003-A” surfactant in demineralized water.
- the dispersing unit used was an Ultra-Turrax type agitator).
- the dispersion thus prepared contained 10% by weight of PMMA microspheres.
- the dispersion is hereinafter referred to as DISP-2.
- a PA / EL (76/24%) - knit fabric was impregnated by means of a laboratory padder with the following - microsphere-free - solution (liquor):
- the padded swatches prepared according to Examples 1 to 3 above were each dried at 120 ° C for 3 minutes.
- the dried swatches were then treated with 10% by weight Cognis 4001-S 1 by weight.
- the application took place again on the padder.
- the fabric samples thus obtained were each divided into 4 parts and each washed 0-, 1-, 3- and 10 times and dried on a leash.
- the laundry was carried out in accordance with ISO 6330 (Miele household washing machine, 13 g / l ECE detergent, 40 ° C easy-care program).
- Sample 1 Microspheres "Covabed LH 85" loaded with 10% "Cognis 4001-S1": 0, 1, 3 and 10 household washes. washes % Monoi % Vitamin E acetate 0 0.266 0.085 1 0.163 0, 066 3 0,139 0.058 10 0.121 0.053
- The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
- Sample 2 "Cosmedia PMMA V8" microspheres loaded with 10% "Cognis 4001-S1": 0, 1, 3 and 10 household washes. washes % Monoi % Vitamin E acetate 0 0,269 0.084 1 0.097 0,045 3 0.114 0.043 10 0.104 0,042
- The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
- The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
- samples 1 and 2 according to the invention showed in particular FIGS. 1 and 3 Wash significantly higher levels of the cosmetic ingredients Monoi and vitamin E acetate on, which is a higher wash permanence proven.
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Abstract
Description
Die Erfindung befindet sich auf dem Gebiet der verzögerten Freisetzung von Wirkstoffen, insbesondere für die Ausrüstung von Fasern und textilen Flächengebilden.The invention is in the field of sustained release of active ingredients, in particular for the finishing of fibers and fabrics.
Unter dem Begriff "Tragekomfort" werden gestiegene Anforderungen des Verbrauchers zusammengefasst, der sich nicht mehr allein damit zufrieden geben will, dass die von ihm unmittelbar auf der Haut getragene Wäsche, wie beispielsweise Dessous oder Strumpfhosen weder kratzen noch Hautrötungen verursachen, sondern ganz umgekehrt erwartet, dass sie sich positiv auf den Zustand seiner Haut auswirkt. Dabei kann es sich sowohl darum handeln, Ermüdungserscheinungen abzuhelfen, als auch einen frischen Duft zu vermitteln oder Hautrauhigkeiten zu vermeiden. Es hat daher nicht an Bemühungen gefehlt, Textilien, beispielsweise Damenstrumpfhosen, mit kosmetischen Wirkstoffen auszurüsten, die beim Tragen auf die Haut übergehen und dort die gewünschten Effekte hervorrufen.The term "wearing comfort" summarizes the increased demands of the consumer, who no longer wants to be satisfied with the fact that the clothes he wears directly on the skin, such as lingerie or tights, neither scratch nor cause reddening of the skin, but are expected in the opposite way. that it has a positive effect on the condition of his skin. This can be either to remedy fatigue, as well as to convey a fresh scent or to avoid skin roughness. There has therefore been no lack of efforts to equip textiles, for example, women's tights, with cosmetic agents that merge when wearing on the skin and there cause the desired effects.
Eine wichtige technische Aufgabenstellung besteht vor diesem Hintergrund darin, Textilien mit Wirkstoffen auszurüsten; von Bedeutung sind hierbei insbesondere:
- Wirkstoffe werden in Mikrokapseln eingebracht und die beladenen Mikrokapseln auf Textilien aufgebracht. Durch mechanische Zerstörung der Mikrokapseln, z.B. durch Reibung auf der Haut, werden die Wirkstoffe freigesetzt. Nachteilig an dieser Lösung ist, dass die Mikrokapseln, also gewissermaßen die "Behälter" der Wirkstoffe, zerstört werden.
- Active substances are introduced into microcapsules and the loaded microcapsules are applied to textiles. By mechanical destruction of the microcapsules, eg by friction on the skin, the active ingredients are released. A disadvantage of this solution is that the microcapsules, so to speak, the "container" of the active ingredients are destroyed.
Database WPI Week198848 (AN 1988-343069) und
Database WPI Week199019 (AN 1990-142321) und
Es war die Aufgabe der vorliegenden Erfindung war es, eine technische Lösung dafür bereitzustellen, die gewährleistet, dass Textilien vom Anwender mit an sich beliebigen Wirkstoffen geladen und auch nachgeladen (reload) werden können. Dabei sollte eine kontrollierte Freisetzung der Wirkstoffe gegeben sein. Ferner sollte eine gegenüber dem bekannten Stand der Technik verbesserte Waschpermanenz gegeben sein. Unter Waschpermanenz ist zu verstehen, dass die oben genannten erwünschten Eigenschaften der Textilien, durch Waschen in nur mäßigem Umfang gemindert werden.It was the object of the present invention to provide a technical solution for ensuring that textiles can be loaded and reloaded by the user with any desired active ingredients. In this case, a controlled release of the active ingredients should be given. Furthermore, an improved compared to the prior art washing permanence should be given. By wash permanence is to be understood that the above-mentioned desirable properties of the textiles are lessened by washing only to a limited extent.
Gegenstand der Erfindung sind zunächst Fasern und textile Flächengebilde, dadurch gekennzeichnet, dass sie mit Mischungen aus
- (a) absorbierenden Mikrosphären und
- (b) filmbildenden Polymeren
- (a) absorbent microspheres and
- (b) film-forming polymers
Die Mikrosphären (a) sind unbeladen. Sie erfüllen die Funktion, dass sie vom Anwender je nach Wunsch beladen und nach Freisetzung der Wirkstoffe auch je nach Wunsch wieder neu beladen werden können.The microspheres (a) are unloaded. They fulfill the function that they can be loaded by the user as desired and, after release of the active ingredients, can also be reloaded as desired.
Bei absorbierenden Mikrosphären handelt es sich um Gebilde, die eine weitgehend homogene Struktur aufweisen. Die im Rahmen der vorliegenden Erfindung zum Einsatz kommenden absorbierenden Mikrosphären haben die Eigenschaft, Wirkstoffe aufnehmen und auch wieder freisetzen zu können, wobei beides mehrfach geschehen kann, d.h. Wirkstoffe können durch Beladen oder Wiederbeladen aufgenommen und im Laufe der Zeit wieder freigesetzt werden. Wegen dieser Eigenschaft werden diese Mikrosphären als absorbierende Mikrosphären bezeichnet. Der Einfachheit halber wird jedoch im folgenden der Zusatz "absorbierend" (* zur Aufnahme von Wirkstoffen fähig) weggelassen und einfach von Mikrosphären gesprochen. Die Wirkstoffe können an der Oberfläche der Mikrosphären adsorbiert und/oder in den Mikrosphären gelöst und/oder in den Mikrosphären z.B. in feinen Kanälen eingelagert sein. Mikrosphären sind formstabil, d.h. sie werden bei der Freisetzung der Wirkstoffe nicht zerstört. Ausdrücklich sei festgestellt, dass Mikrokapseln, die ja bei der Freisetzung der Wirstoffe zerstört werden, nicht unter die Definition von Mikrosphären fallen.Absorbent microspheres are structures that have a largely homogeneous structure. The absorbent microspheres used in the context of the present invention have the property of being able to absorb and also release active substances, both of which can be done several times, ie. Active substances can be absorbed by loading or reloading and released again over time. Because of this property, these microspheres are referred to as absorbent microspheres. For the sake of simplicity, however, the term "absorbent" (* capable of taking active ingredients) will be omitted below and simply referred to as microspheres. The active ingredients can be adsorbed on the surface of the microspheres and / or dissolved in the microspheres and / or in the microspheres e.g. be embedded in fine channels. Microspheres are dimensionally stable, i. they are not destroyed in the release of the active ingredients. It should be expressly stated that microcapsules, which are indeed destroyed in the release of the active substances, do not fall under the definition of microspheres.
Der zentrale Punkt der durch die vorliegende Erfindung vorgeschlagenen technischen Lösung besteht in einer Kombination mehrerer Faktoren:
- Die Mikrosphären wirken als Container für Wirkstoffe.
- Die Mikrosphären sind formstabil und werden durch Freisetzung der Wirkstoffe nicht zerstört.
- Die Mikrosphären können mehrfach - auch mit unterschiedlichen Wirkstoffen - nachbeladen werden (reload).
- The microspheres act as containers for active ingredients.
- The microspheres are dimensionally stable and are not destroyed by release of the active ingredients.
- The microspheres can be reloaded several times - even with different active ingredients - (reload).
Die Mikrosphären werden durch - ein oder mehrere - filmbildende Polymere auf der Textiloberfläche fixiert, wodurch sich eine im Vergleich zum Stand der Technik relative Verbesserung der Waschpermanenz ergibt.The microspheres are fixed by - one or more - film-forming polymers on the textile surface, resulting in a relative to the prior art, relative improvement of the washing permanence.
Die Mikrosphären weisen vorzugsweise Kugelform auf, sind jedoch hinsichtlich ihrer Geometrie nicht auf Kugelform beschränkt, sondern können auch andere Raumformen aufweisen, beispielsweise können sie Rotatiosellipsoide darstellen oder Stäbchenform aufweisen.The microspheres are preferably spherical in shape, but are not limited in geometry to spheroidal shape, but may have other spatial shapes, for example, they may represent rotatiosellipsoids or have a rod shape.
Die Mikrosphären weisen bevorzugt eine mittlere Teilchengröße im Bereich von 1 bis 15 Mikrometern und insbesondere von 5 bis 10 Mikrometern auf.The microspheres preferably have an average particle size in the range of 1 to 15 microns, and more preferably 5 to 10 microns.
In einer Ausführungsform setzt man Mikrosphären auf Basis von Polymethylmethacrylat (PMMA) ein. Beispiele sind etwa Covabead LH 85 oder LH 170 der Fa. LCW oder Cosmedia PMMA V8, Cosmedia PMMA V 12 oder Cosmedia SILC der Fa. Cognis.In one embodiment, microsphere based on polymethylmethacrylate (PMMA) is used. Examples are, for example, Covabead LH 85 or LH 170 from the company LCW or Cosmedia PMMA V8, Cosmedia PMMA V 12 or Cosmedia SILC from Cognis.
In einer Ausführungsform setzt man Mikrosphären auf Silikon- oder SiO2-Basis ein. Beispiel sind "Dow Coming 9509 Silicone Elastomer Suspension" der Fa. Dow Corning.In one embodiment, silicone-based or SiO 2 -based microspheres are used. Examples are "Dow Corning 9509 Silicone Elastomer Suspension" from Dow Corning.
In einer bevorzugten Ausführungsform setzt man Mikrosphären auf Basis von Polymethylmethacrylat (PMMA) ein.In a preferred embodiment, microspheres based on polymethylmethacrylate (PMMA) are used.
Die im Sinne der Erfindung in Betracht kommenden filmbildenden Polymeren (b), die auch als Bindemittel bezeichnet werden können, können an sich beliebiger Natur sein. Vorzugsweise werden sie ausgewählt aus der Gruppe, die gebildet wird von
- Polyurethanen (PU),
- Polyethylvinylacetaten (EVA),
- polymeren Melaminverbindungen,
- polymeren Glyoxalverbindungen,
- polymeren Siliconverbindungen,
- epichlorhydrinvernetzten Polyamidoaminen und
- Poly(meth)acrylaten
- Polyurethanes (PU),
- Polyethylvinyl acetates (EVA),
- polymeric melamine compounds,
- polymeric glyoxal compounds,
- polymeric silicone compounds,
- epichlorohydrin crosslinked polyamidoamines and
- Poly (meth) acrylates
Geeignete Polyurethane (PU) und Polyethylvinylacetate (EVA) stellen etwa die im Handel erhältlichen Produkte aus der Reihe Cognis 3011-A oder Cognis 3009-A der Firma Cognis.Suitable polyurethanes (PU) and polyethylvinyl acetates (EVA) are, for example, the commercially available products from the Cognis 3011-A or Cognis 3009-A range from Cognis.
Polymere Melaminverbindungen: Melamin (synonym : 2,4,6-triamino-1,3,5-triazin) entsteht üblicherweise durch Trimerisierung von Dicyandiamid oder durch Cyclisierung von Harnstoff unter Abspaltung von Kohlendioxid und Ammoniak. Im Sinne der Erfindung werden unter Melaminen oligomere oder polymere Kondensationsprodukte des Melamins mit Formaldehyd, Harnstoff, Phenol oder deren Gemischen verstanden. Polymere Glyoxalverbindungen: Glyoxal (synonym : Oxaldehyd, Ethandial) entsteht bei der Dampfphasenoxidation von Ethylenglycol mit Luft in Gegenwart von Silberkatalysatoren. Im Sinne der Erfindung werden unter Glyoxalen die Eigenkondensationsprodukte des Glyoxals ("Polyglyoxale") verstanden. 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. For the purposes of the invention, melamine refers to oligomeric or polymeric condensation products of melamine with formaldehyde, urea, phenol or mixtures thereof. Polymeric Glyoxal Compounds: Glyoxal (synonym: oxaldehyde, ethanedial) results from the vapor phase oxidation of ethylene glycol with air in the presence of silver catalysts. For the purposes of the invention, glyoxals are understood as meaning the self-condensation products of glyoxal ("polyglyoxals").
Polymere Siliconverbindungen: Geeignete Siliconverbindungen sind beispielsweise Dimethylpolysiloxane, Methylphenylpolysiloxane, cyclische Silicone sowie amino-, fettsäure-, alkohol-, polyether-, epoxy-, fluor-, glykosid- und/oder alkylmodifizierte Siliconverbindungen, die bei Raumtemperatur vorzugsweise fest oder harzförmig vorliegen. Weiterhin geeignet sind Simethicone, bei denen es sich um Mischungen aus Dimethiconen mit einer durchschnittlichen Kettenlänge von 200 bis 300 Dimethylsiloxan-Einheiten und hydrierten Silicaten handelt. Besonders bevorzugt ist der Einsatz von Aminosiloxanen, z.B Cognis 3001 der Fa. Cognis. Deren weiteren Vernetzung mit H-Siloxanen, z.B. Cognis 3002 der Fa. Cognis kann die Leistung als Bindemittel noch weiter steigern. Silicone compounds: Suitable silicone compounds are, for example, dimethylpolysiloxanes, methylphenylpolysiloxanes, cyclic silicones and amino, fatty acid, alcohol, polyether, epoxy, fluorine, glycoside and / or alkyl-modified silicone compounds which are preferably solid or resin-form at room temperature. Also suitable are simethicones, which are mixtures of dimethicones having an average chain length of from 200 to 300 dimethylsiloxane units and hydrogenated silicates. Particularly preferred is the use of aminosiloxanes, eg Cognis 3001 from Cognis. Their further crosslinking with H-siloxanes, eg Cognis 3002 from Cognis, can further increase the performance as a binder.
Epichlorhydrinvernetzte Polyamidoamin: Epichlorhydrinvernetzte Polyamidoamine, die auch als "Fibrabones" oder "Wet strength resins" bezeichnet werden, sind aus der Textil- und Papiertechnologie hinreichend bekannt. Zu ihrer Herstellung geht man vorzugsweise von zwei Verfahren aus:
- 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 quatemierten 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.
- 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 non-quaternized 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)acrylate: Unter dem Begriff Poly(meth)acrylate sind Homo- und Copolymerisationsprodukte der Acrylsäure, Methacrylsäure sowie gegebenenfalls deren Ester, speziell deren Ester mit niederen Alkoholen, wie z.B. Methanol, Ethanol, Isopropylalkohol, den isomeren Butanolen, Cyclohexanol und dergleichen zu verstehen, welche in an sich bekannter Weise, beispielsweise durch radikalische Polymerisation unter UV-Bestrahlung erhalten werden. Typischerweise liegt das mittlere Molekulargewicht der Polymeren zwischen 100 und 10.000, vorzugsweise bei 200 und 5.000 und insbesondere 400 bis 2.000 Dalton. Poly (meth) acrylates: The term poly (meth) acrylates are homo- and copolymerization products of acrylic acid, methacrylic acid and optionally their esters, especially their esters with lower alcohols, such as methanol, ethanol, isopropyl alcohol, the isomeric butanols, cyclohexanol and the like to understand which are obtained in a conventional manner, for example by free-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.
Üblicherweise werden die Bindemittel (b) - bezogen auf die Komponente (a) - in Mengen von 0,5 bis 15, vorzugsweise 1 bis 10 und insbesondere 1 bis 5 Gew.-% auf die Fasern aufgebracht. Dabei sind unter Komponente (a) die Mikrosphären in unbeladener Form zu verstehen.Usually, the binders (b) - based on the component (a) - in amounts of 0.5 to 15, preferably 1 to 10 and especially 1 to 5 wt .-% applied to the fibers. Component (a) is to be understood as meaning the microspheres in unloaded form.
Die Auswahl der Wirkstoffe, die zur Beladung der Mikrosphären bestimmt sind, ist an sich unkritisch und richtet sich ausschließlich danach, welcher Effekt auf der Haut bewirkt werden soll. Für die textile Ausrüstung, aber auch für die kosmetische Anwendungen, sind solche Wirkstoffe bevorzugt, die feuchtigkeitsspendende Eigenschaften aufweisen oder Cellulite entgegenwirken sind. Typische Beispiele sind Tocopherol, Tocopherolacetat, Tocopherolpalmitat, Carotine, Koffein, Ascorbinsäure, (Desoxy)Ribonukleinsäure und deren Fragmentierungsprodukte, β-Glucane, Retinol, Bisabolol, Allantoin, Phytantriol, Panthenol, AHA-Säuren, Aminosäuren, Ceramide, Pseudoceramide, Chitosan, Dihydroxyaceton, Menthol, Squalan, ätherische Öle (z.B. Lavendelöl, Zitronenöl, Eukalytusöl oder Pfefferminzöl), pflanzliche Öle (z.B. Monoi de Tahiti, Shea Butter, Mandelöl, Passionsfruchtöl, Hagebuttenkernöl oder Aprikosenöl), pflanzliche Proteine und deren Hydrolyseprodukte, Pflanzenextrakte, wie z.B. Extrakte von Ginkgo biloba, Camellia sinensis, Trifolium pratensis, Oleacea europensis, Litchi sinensis, Valeriana oficinalis, Medicago sativa, Vitis vinifera, Passiflora incarnata und dergleichen sowie Vitaminkomplexe zu verstehen.The choice of active ingredients that are intended to load the microspheres is not critical per se and depends exclusively on which effect is to be effected on the skin. For the textile equipment, but also for cosmetic applications, such active ingredients are preferred which have moisturizing properties or counteract cellulite. 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 lavender oil, lemon oil, eucalyptus oil or peppermint oil), vegetable oils (eg Monoi de Tahiti, shea butter, almond oil, passion fruit oil, rosehip seed oil or apricot oil), vegetable proteins and their hydrolysis products, plant extracts, such as Extracts of Ginkgo biloba, Camellia sinensis, Trifolium pratensis, Oleacea europensis, Litchi sinensis, Valeriana oficinalis, Medicago sativa, Vitis vinifera, Passiflora incarnata and the like as well as vitamin complexes.
Besonders bevorzugt wählt man die Wirkstoffe aus der Gruppe, die gebildet wird von ätherischen Ölen, pflanzlichen Ölen, Squalan, Chitosan, Menthol, Retinol (bzw. Vitamin A), Koffein, pflanzlichen oder tierischen Proteinen und deren Hydrolyseprodukten, Carotinen und Jojobaöl. Diese verfügen über ein sehr breites Eigenschaftsprofil und tragen einzeln bzw. in Kombination zum Gleichgewicht der cutanen Hydrolipidschicht bei, beugen dem Wasserverlust und damit der Faltenbildung vor, erfrischen die Haut und wirken Ermüdungserscheinungen entgegen, verleihen der Haut ein weiches und elastisches Gefühl, verbessern die Hautdrainage, die Zufuhr von Nährstoffen und die Blutzirkulation, wirken gegen oxidativen Stress, Umweltgifte, Hautalterung und freie Radikale, gleichen den durch Wasser und Sonne bewirkten Verlust an Fetten aus, verbessern die Wasserbeständigkeit von UV-Filtern, gewährleisten eine homogene Bräunung und besutzen schließlich zudem auch antimikrobielle Eigenschaften.It is particularly preferable to select the active compounds from the group formed by essential oils, vegetable oils, squalane, chitosan, menthol, retinol (or vitamin A), caffeine, vegetable or animal proteins and their hydrolysis products, carotenes and jojoba oil. These have a very broad property profile and contribute individually or in combination to the balance of the cutaneous hydrolipid layer, prevent the loss of water and thus the formation of wrinkles, refresh the skin and counteract fatigue, give the skin a soft and elastic feeling, improve the skin drainage, the supply of nutrients and the 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 have antimicrobial properties.
Üblicherweise beträgt das Gewichtsverhältnis zwischen der Komponente (a) - etwa dem feinverteilten PMMA - und den Wirkstoffen 10 : 90 bis 99 : 1, vorzugsweise 3 : 1 bis 1 : 1 und besonders bevorzugt ca. 2 : 1.Usually, the weight ratio between the component (a) - such as the finely divided PMMA - and the active ingredients is 10: 90 to 99: 1, preferably 3: 1 to 1: 1 and more preferably about 2: 1.
- Cosmedia PMMA V8: PMMA Microsphären der Fa. Cognis Cosmedia PMMA V8 : PMMA microspheres from Cognis
- Covabed LH 85: PMMA Microsphären der Fa. LCW Covabed LH 85 : PMMA microspheres from LCW
- Cognis 3001-A: Aminosiloxanemulsion der Fa. Cognis Cognis 3001-A : Aminosiloxane emulsion from Cognis
- Cognis 3002-A: H-Polydimethylsiloxanemulsion der Fa. Cognis Cognis 3002-A : H-polydimethylsiloxane emulsion from Cognis
- Cognis 6003-A: Alkylpolyglycolether, Tensid (Netzmittel) der Fa. Cognis Cognis 6003-A : alkyl polyglycol ether, surfactant (wetting agent) from Cognis
- Cognis 4001-S1: Kosmetische Emulsion der Fa. Cognis Cognis 4001-S1 : Cosmetic emulsion from Cognis
Die Microsphären "Covabed LH 85" wurden mithilfe des Tensids "Cognis 6003-A" in vollentsalztem Wasser in eine 10 Gew.-%-ge wässrige Dispersion überführt. Als Dispergieraggregat diente ein Rührer vom Typ Ultra-Turrax). Die so hergestellte Dispersion enthielt 10 Gew.% an PMMA-Microsphären. Die Dispersion wird nachflgnd als DISP-1 bezeichnet.The "Covabed LH 85" microspheres were converted into a 10% by weight aqueous dispersion using the "Cognis 6003-A" surfactant in demineralized water. The dispersing unit used was an Ultra-Turrax type agitator). The dispersion thus prepared contained 10% by weight of PMMA microspheres. The dispersion is hereinafter referred to as DISP-1.
Anschließend wurde ein PA/EL (76/24%)-Gestrick (Strickware, bei der das Garn aus 76% Polyamid und 24% Elasthan (z.B. Lycra) besteht) mittels eines Laborfoulards mit folgender Lösung (Flotte) imprägniert:Next, a PA / EL (76/24%) knit (knit fabric in which the yarn is made of 76% polyamide and 24% spandex (e.g., Lycra)) was impregnated with the following solution (liquor) by means of a laboratory padder:
Die Microsphären "Cosmedia PMMA V8" wurden mithilfe des Tensids "Cognis 6003-A" in vollentsalztem Wasser in eine 10 Gew.-%-ge wässrige Dispersion überführt. Als Dispergieraggregat diente ein Rührer vom Typ Ultra-Turrax). Die so hergestellte Dispersion enthielt 10 Gew.% an PMMA-Microsphären. Die Dispersion wird nachflgnd als DISP-2 bezeichnet.The "Cosmedia PMMA V8" microspheres were converted into a 10% by weight aqueous dispersion using the "Cognis 6003-A" surfactant in demineralized water. The dispersing unit used was an Ultra-Turrax type agitator). The dispersion thus prepared contained 10% by weight of PMMA microspheres. The dispersion is hereinafter referred to as DISP-2.
Anschließend wurde ein PA/EL (76/24%)-Gestrick mittels eines Laborfoulards mit folgender Lösung (Flotte) imprägniert:Subsequently, a PA / EL (76/24%) - knitted fabric was impregnated by means of a laboratory foulard with the following solution (liquor):
Ein PA/EL (76/24%)-Gestrick wurde mittels eines Laborfoulards mit folgender - Mikrosphären-freien - Lösung (Flotte) imprägniert:A PA / EL (76/24%) - knit fabric was impregnated by means of a laboratory padder with the following - microsphere-free - solution (liquor):
Die gemäß den obigen Beispielen 1 bis 3 hergestellten foulardierten Stoffproben wurden jeweils bei 120 °C für 3 Minuten getrocknet.
Die getrockneten Stoffproben wurden dann mit 10 Gew.-% Cognis 4001-S 1 - bezogen auf das Stoffgewicht - behandelt. Die Applikation erfolgte wiederum am Foulard.
Die so erhaltenen Stoffproben wurde jeweils in 4 Teile geteilt und jeweils 0-, 1-, 3- und 10-mal gewaschen und an der Leine getrocknet. Die Wäsche erfolgte in Anlehnung an ISO 6330 (Miele Haushaltswaschmaschine, 13 g/l ECE-Waschmittel, 40°C-Pflegeleicht-Programm).The padded swatches prepared according to Examples 1 to 3 above were each dried at 120 ° C for 3 minutes.
The dried swatches were then treated with 10% by weight Cognis 4001-S 1 by weight. The application took place again on the padder.
The fabric samples thus obtained were each divided into 4 parts and each washed 0-, 1-, 3- and 10 times and dried on a leash. The laundry was carried out in accordance with ISO 6330 (Miele household washing machine, 13 g / l ECE detergent, 40 ° C easy-care program).
- Probe 1, Mikrosphären "Covabed LH 85", beladen mit 10% "Cognis 4001-S1": 0, 1, 3 und 10 Haushaltswäschen.Sample 1, microspheres "Covabed LH 85" loaded with 10% "Cognis 4001-S1": 0, 1, 3 and 10 household washes.
- Probe 2, Mikrosphären "Cosmedia PMMA V8", beladen mit 10% "Cognis 4001-S1": 0, 1, 3 und 10 Haushaltswäschen.Sample 2, "Cosmedia PMMA V8" microspheres loaded with 10% "Cognis 4001-S1": 0, 1, 3 and 10 household washes.
- Probe 3, keine Mikrosphären, beladen mit 10% Cognis 4001-S1: 0, 1, 3 und 10 Haushaltswäschen.Sample 3, no microspheres, loaded with 10% Cognis 4001-S1: 0, 1, 3 and 10 household washes.
Alle diese Proben wurden mit Tetrahydrofuran (Lösungsmittel) extrahiert und anschließend der Extrakt per GC-MS analysiert. Als Referenzsubstanzen dienten die in der kosmetischen Emulsion "Cognis 4001-S 1" enthaltenen kosmetischen Inhaltsstoffe "Monoi" (Monoi de Tahiti = Kokosöl mit Spuren von Tiare-Blume) und Vitamin E-Acetat.All of these samples were extracted with tetrahydrofuran (solvent) and then the extract analyzed by GC-MS. The reference substances used in the cosmetic emulsion "Cognis 4001-S 1" cosmetic ingredients "Monoi" (Monoi de Tahiti = coconut oil with traces of Tiare flower) and vitamin E acetate.
Probe 1: Mikrosphären "Covabed LH 85", beladen mit 10% "Cognis 4001-S1": 0, 1, 3 und 10 Haushaltswäschen.
Die % Angaben dieser Tabelle sind zu verstehen als: Gew.-% des jeweiligen Wirkstoffs (Monoi bzw. Vitamin E-acetat) bezogen auf das Stoffgewicht.The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
Normiert man die Mengen der Inhaltsstoffe vor dem Waschvorgang (also bei 0 Wäschen) auf 100, so ist die relative Abnahme der Wirkstoffmengen bei den Wäschen wie folgt:
Probe 2: Mikrosphären "Cosmedia PMMA V8", beladen mit 10% "Cognis 4001-S1": 0, 1, 3 und 10 Haushaltswäschen.
Die % Angaben dieser Tabelle sind zu verstehen als: Gew.-% des jeweiligen Wirkstoffs (Monoi bzw. Vitamin E-acetat) bezogen auf das Stoffgewicht.The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
Normiert man die Mengen der Inhaltsstoffe vor dem Waschvorgang (also bei 0 Wäschen) auf 100, so ist die relative Abnahme der Wirkstoffmengen bei den Wäschen wie folgt:
Probe 3: keine Mikrosphären, beladen mit 10% Cognis 4001-S1: 0, 1, 3 und 10 Haushaltswäschen
Die % Angaben dieser Tabelle sind zu verstehen als: Gew.-% des jeweiligen Wirkstoffs (Monoi bzw. Vitamin E-acetat) bezogen auf das Stoffgewicht.The% data in this table are to be understood as:% by weight of the respective active substance (mono egg or vitamin E acetate) based on the weight of the substance.
Normiert man die Mengen der Inhaltsstoffe vor dem Waschvorgang (also bei 0 Wäschen) auf 100, so ist die relative Abnahme der Wirkstoffmengen bei den Wäschen wie folgt:
Im Vergleich zur Probe 3 (Referenz zum Vergleich), bei der die Textilien nur mit Binder ausgerüstet waren, jedoch keine Mikrosphären enthielten, wiesen die erfindungsgemäßen Proben 1 und 2, bei denen die Textilien mit Mikrosphären und Bindern ausgerüstet waren, insbesondere nach 1 und 3 Wäschen deutlich höhere Gehalte an den kosmetischen Inhaltsstoffen Monoi und Vitamin E-Acetat auf, womit eine höhere Waschpermanenz belegt ist.In comparison to sample 3 (reference for comparison), in which the textiles were only provided with binders but did not contain any microspheres, samples 1 and 2 according to the invention, in which the textiles were equipped with microspheres and binders, showed in particular FIGS. 1 and 3 Wash significantly higher levels of the cosmetic ingredients Monoi and vitamin E acetate on, which is a higher wash permanence proven.
Claims (2)
- Fibres and textile fabrics, characterized in that they are endowed with mixtures of(a) absorbent microspheres, and(b) film-forming polymers,with the proviso that component (a) is fixed to the textile surface using component (b), wherein the microspheres (a) are unloaded.
- Fibres and textile fabrics according to Claim 1, wherein polymethyl methacrylate (PMMA) is used as component (a).
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AT08007156T ATE547555T1 (en) | 2008-04-11 | 2008-04-11 | LOADABLE FIBERS AND TEXTILE STRUCTURES |
EP08007156A EP2108735B1 (en) | 2008-04-11 | 2008-04-11 | Loadable fibres and textile sheets |
PCT/EP2009/002399 WO2009124686A1 (en) | 2008-04-11 | 2009-04-02 | Chargeable fibres and textile fabrics |
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