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EP0436524A1 - Dispersions for preparing fibrous material. - Google Patents

Dispersions for preparing fibrous material.

Info

Publication number
EP0436524A1
EP0436524A1 EP87904867A EP87904867A EP0436524A1 EP 0436524 A1 EP0436524 A1 EP 0436524A1 EP 87904867 A EP87904867 A EP 87904867A EP 87904867 A EP87904867 A EP 87904867A EP 0436524 A1 EP0436524 A1 EP 0436524A1
Authority
EP
European Patent Office
Prior art keywords
aqueous dispersion
compound
compounds
carbon atoms
optionally
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP87904867A
Other languages
German (de)
French (fr)
Other versions
EP0436524B1 (en
Inventor
Heinrich Singer
Werner Stechele
Michael Bernheim
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
PFERSEE CHEMIE GMBH
Original Assignee
Chemische Fabrik Pfersee GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chemische Fabrik Pfersee GmbH filed Critical Chemische Fabrik Pfersee GmbH
Priority to AT87904867T priority Critical patent/ATE82337T1/en
Publication of EP0436524A1 publication Critical patent/EP0436524A1/en
Application granted granted Critical
Publication of EP0436524B1 publication Critical patent/EP0436524B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46—Compounds containing quaternary nitrogen atoms
    • D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35—Heterocyclic compounds
    • D06M13/352—Heterocyclic compounds having five-membered heterocyclic rings
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
    • D06M15/29—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides containing a N-methylol group or an etherified N-methylol group; containing a N-aminomethylene group; containing a N-sulfidomethylene group
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material

Definitions

  • the present invention describes aqueous dispersions for the simultaneous softening and hydrophilizing finishing of fiber materials which contain at least one quaternary compound with at least one long-chain alkyl radical and a polymer or copolymer based on alkyl acrylates with alkyl radicals with at least 4 carbon atoms, a process for their preparation and their use.
  • copolymers based on alkyl acrylates for finishing textiles has long been known (DE-AS 1 119 609 and DE-PS 1 209 989).
  • the grip of the fiber materials treated with it is favorably influenced.
  • By varying the monomers and their proportions in the copolymer it is also possible that other effects such as reduced wet soiling.
  • the object of this invention was therefore to find means which remedy this deficiency in the prior art.
  • Claims 11 to 17 describe processes for producing the dispersions according to the invention.
  • the use of the aqueous dispersions is claimed.
  • At least one quaternary compound with at least one long-chain alkyl radical is used as compounds (1). These compounds are generally known and have as the long-chain alkyl radical at least one saturated and / or unsaturated alkyl radical having at least 12, in particular 16 to 22, carbon atoms.
  • Examples include octadecyloxymethyl-pyridinium chloride and stearylamido-methyl-pyridinium chloride.
  • quaternary compounds are particularly suitable as compounds (1) Imidazolinium derivatives and quaternary ammonium derivatives. The following are examples of the particularly suitable compounds:
  • the amounts of compounds (1) used range from 20 to 70 g, in particular 30 to 60 g, per 1000 g of aqueous dispersion.
  • the known polymers or copolymers based on alkyl acrylates with alkyl radicals having at least 4 C atoms are used as compounds (2).
  • the alkyl radicals in these compounds (2) preferably have 4 to 10, in particular 4 to 8, carbon atoms.
  • the following may be mentioned as examples of such base monomers, which are contained in the same in amounts of 60 to 100% by weight, based on the total polymer:
  • butyl acrylate 2-ethylhexyl acrylate, decyl acrylate and especially butyl acrylate.
  • Homopolymers of butyl acrylate are particularly suitable as compounds (2), while ethyl acrylate cannot be used as the base monomer.
  • copolymers based on the corresponding monomers can also be used as compounds (2).
  • These compounds (2) come in the form of 30 to 70% strength aqueous dispersions, 20 to 80 g of which are used to prepare the aqueous dispersions according to the invention. in particular 20 to 60 g of compounds (2), calculated as a 100% polymer, are used.
  • emulsifier (3) which are different from (1) are used as emulsifiers.
  • the person skilled in the art knows the ethoxylated fatty alcohols, fatty amides, fatty acids, alkylphenols and fatty amines or their salts or the quaternary ammonium compounds used, for example, and will have no difficulty in selecting these compounds accordingly.
  • the amounts of emulsifier (3) can be up to 100 wt. %, based on compound (2).
  • the aqueous dispersion additionally contains at least one hydrophilizing silicone, in quantities of 5 to 70 g, in particular 15 to 55 g per 1000 g aqueous dispersion.
  • These additionally used compounds (4) are also known to the person skilled in the art. In general, these are dimethylpolysiloxanes which contain epoxy groups (a) and / or polyethoxy or polypropoxy or polyethoxy / propoxy groups (b) incorporated.
  • Silicones which have groups (a) and (b) in the same molecule are particularly suitable.
  • a typical representative of the compounds (4) UCARSIL® ® EPS (Union Carbide Corp.). Those skilled in the art will have no difficulty in finding similar useful compounds.
  • the invention therefore also relates to a process for the preparation of the aqueous dispersions according to the invention.
  • the production of such dispersions is known in principle.
  • a monomer emulsion is rides, which in addition to the alkyl acrylates with alkyl radicals with at least 4 carbon atoms and optionally further comonomers and possibly the emulsifier (3) contains the quaternary compound with at least one long-chain alkyl radical and preferably also the compound (4).
  • the aqueous dispersions obtained serve for the softening and hydrophilizing finishing of fiber materials of all kinds, in particular terry goods, especially cotton terry goods, but also of bed linen.
  • the textiles are treated in a known manner with liquors which contain 15 to 80 g / l, in particular 20 to 60 g / l, of the aqueous dispersion, based on a dispersion with a solids content of about 20% by weight, so that a A coating of about 0.3 to 3% solid substance results on the fiber material.
  • the hydrophilicity can be increased by brief post-condensation.
  • a pre-emulsion is prepared from 37.5 parts of 1-methyl-2-tallow fatty acid amido-ethyl-imidazoline methosulfate and 20 parts of the acetate of an ethoxylated C-16 fatty amine (total of 10 EO groups each Mol) as an additional emulsifier and subsequent addition of 550 parts of 90 ° C hot water, cooling to 40 ° C and further addition of 2.5 parts of phosphoric acid (pH 5 to 6), 60 parts of butyl acrylate and 45 parts of UCARSIL ® EPS with stirring.
  • the pH is then adjusted to 6 to 7 with 6 parts of triethanolamine at 50 ° C. and the product is then filtered in a known manner. A good cold-resistant, stable aqueous dispersion is obtained.
  • aqueous dispersion B is prepared in the same manner as above, but polymerisation is carried out in the absence of UCARSIL ® EPS.
  • Dispersions A) to D) are treated with a heavy cotton terry fabric (450 g / m 2 ) by immersing them in the liquor, squeezing to 110% liquor absorption and drying at 120 ° C. for 15 minutes (solids deposits approx. 1%).
  • the finished material has the following effects: Aqueous dispersion handle hydrophilicity
  • Example 1 is repeated in the same way, but using compound (1 d) as the quaternary compound having at least one long-chain alkyl radical.
  • the cotton terry finished with the aqueous liquors prepared in accordance with Example 1 now shows the following effects:
  • an aqueous dispersion is prepared, in addition, 50 parts of glycerol monoisostearate are melted at the beginning and the amount of hot water is increased to 740 parts.
  • the cotton terry cloth finished with this dispersion B) also has a soft, fluffy feel and good to very good hydrophilicity.
  • Example 1 prepares a monomer emulsion and then, as described in Example 1 under A), produces the aqueous dispersion which is compatible with optical brighteners.
  • a light cotton terry towel (240 g / m 2 ) is finished by immersing it in the liquor, squeezing to 100% liquor absorption and drying at 120 ° C. for 10 minutes.
  • the goods treated in this way show a lot soft, fluffy feel and is also characterized by a particularly good hydrophilicity.
  • Example 3 is repeated, but the absence of the acetate of an ethoxylated C-16 fatty amine used there (on average 10 ethylene oxide groups).
  • aqueous dispersion produced in this way is somewhat less filterable, but can also be used very well to equip a wide variety of terry goods.
  • a process for producing these watery dispersions is also disclosed.
  • T water dispersions give to fibrous materials, such as terry cotton fabrics, a specially soft, velvety feel and very good to markable hydrophilic characteristics.
  • Aqueous dispersions for the simultaneous softening and hydrophilizing finishing of fiber materials containing 1) at least one quaternary compound with at least one long-chain alkyl radical, 2) a polymer or copolymer based on alkyl acrylates with alkyl radicals with at least 4 carbon atoms, 3) optionally additionally one from 1) different emulsifier and 4) optionally a hydrophilizing silicone.
  • a drive to produce this aqueous dispersion is claimed.
  • fiber material such as cotton terry toweling is given a particularly soft, fluffy feel and a very good to excellent hydrophilicity.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Inorganic Fibers (AREA)
  • Paper (AREA)
  • Colloid Chemistry (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

Des dispersions aqueuses d'assouplissement et d'hydrophilisation simultanés de matériaux fibreux contiennent 1) au moins un composé quaternaire ayant au moins un résidu alkyle à longue chaîne, 2) un polymérisat ou copolymérisat à base d'alkylacrylates avec des résidus d'alkyle ayant au moins 4 atomes de carbone, 3) le cas échéant un émulsifiant additionnel différent de 1), et 4) le cas échéant un silicone hydrophilisant. L'invention concerne également un procédé de production de ces dispersions aqueuses. Ces dispersions aqueuses rendent des matériaux fibreux, tels que des tissus éponge en coton, particulièrement doux et veloutés au toucher et leur donnent des caractéristiques hydrophiles très bonnes, voire remarquables.Aqueous dispersions of simultaneous softening and hydrophilization of fibrous materials contain 1) at least one quaternary compound having at least one long-chain alkyl residue, 2) a polymer or copolymer based on alkyl acrylates with alkyl residues having at least 4 carbon atoms, 3) if necessary an additional emulsifier other than 1), and 4) if necessary a hydrophilizing silicone. The invention also relates to a process for producing these aqueous dispersions. These aqueous dispersions make fibrous materials, such as cotton terry cloth, particularly soft and velvety to the touch and give them very good, even remarkable, hydrophilic characteristics.

Description

DISPERSIONEN FÜR AUSRÜSTUNG VON FASERMATERIALIEN DISPERSIONS FOR EQUIPMENT OF FIBER MATERIALS
Die vorliegende Erfindung beschreibt wäßrige Dispersionen zur gleichzeitigen weichmachenden und hydrophilisierenden Ausrüstung von Fasermaterialien, die mindestens eine quaternäre Verbindung mit mindestens einem langkettigen Alkylrest und ein Polymerisat bzw. Copolymerisat auf Basis von Alkylacrylaten mit Alkylresten mit mindestens 4 C- Atomen enthalten, ein Verfahren zu deren Herstellung und deren Verwendung.The present invention describes aqueous dispersions for the simultaneous softening and hydrophilizing finishing of fiber materials which contain at least one quaternary compound with at least one long-chain alkyl radical and a polymer or copolymer based on alkyl acrylates with alkyl radicals with at least 4 carbon atoms, a process for their preparation and their use.
Die Verwendung von Copolymeren auf Basis von Alkylacrylaten zur Ausrüstung von Textilien ist längst bekannt (DE-AS 1 119 609 und DE-PS 1 209 989). Der Griff der damit behandelten Fasermaterialien wird günstig beeinflußt. Auch ist es durch Variation der Monomeren und deren Mengenverhältnisse im Copolymerisat durchaus mögelich, andere Effekte wie z.B. eine verringerte Naßanschmutzung, zu erhalten.The use of copolymers based on alkyl acrylates for finishing textiles has long been known (DE-AS 1 119 609 and DE-PS 1 209 989). The grip of the fiber materials treated with it is favorably influenced. By varying the monomers and their proportions in the copolymer it is also possible that other effects such as reduced wet soiling.
Der Stand der Technik hat aber bis heute noch keinen Weg aufgezeigt, auf dieser Basis gleichzeitig einen angenehmen weichen, flauschigen Griff und eine verbesserte Hydrophilität der ausgerüsteten Pasermaterialien, insbesondere von Baumwoll-Frottee-Waren, zu erzielen.To date, however, the prior art has not shown any way of simultaneously achieving a pleasant soft, fluffy feel and improved hydrophilicity of the finished pas materials, in particular cotton terry goods, on this basis.
Aufgabe dieser Erfindung war es deshalb, Mittel aufzufinden, die diesen Mangel des Standes der Technik beheben.The object of this invention was therefore to find means which remedy this deficiency in the prior art.
Erfindungsgemäß gelingt es nunmehr, wäßrige Dispersionen bereitzustellen, die gleichzeitig eine weichmachende und hydrophilisierende Ausrüstung von Pasermaterialien bewirken, wenn die im Patentanspruch 1 näher beschriebenen Bedingungen eingehalten werden. In den Unteransprüchen 2 bis 10 werden detaillierte Einzelheiten der wäßrigen Dispersionen unter Schutz gestellt.According to the invention, it is now possible to provide aqueous dispersions which at the same time bring about softening and hydrophilizing finishing of paser materials if the conditions described in more detail in claim 1 are met. In subclaims 2 to 10 detailed details of the aqueous dispersions are protected.
Die Patentansprüche 11 bis 17 beschreiben Verfahren zur Herstellung der erfindungsgemäßen Dispersionen. Im Patentanspruch 18 wird die Verwendung der wäßrigen Dispersionen beansprucht.Claims 11 to 17 describe processes for producing the dispersions according to the invention. In claim 18, the use of the aqueous dispersions is claimed.
Als Verbindungen (1) wird mindestens eine quaternäre Verbindung mit mindestens einem langkettigen Alkylrest eingesetzt. Diese Verbindungen sind allgemein bekannt und haben als langkettigen Alkylrest mindestens einen gesättigten und/oder ungesättigten Alkylrest mit mindestens 12, insbesondere 16 bis 22 C-Atomen.At least one quaternary compound with at least one long-chain alkyl radical is used as compounds (1). These compounds are generally known and have as the long-chain alkyl radical at least one saturated and / or unsaturated alkyl radical having at least 12, in particular 16 to 22, carbon atoms.
Als Beispiele seien Octadecyloxymethyl-Pyridiniumchlorid und Stearylamido-methyl-pyridiniumchlorid genannt. Besonders geeignet sind aber als Verbindungen (1) quaternäre Imidazoliniumderivate und quaternäre Ammoniumderivate. Für die besonders geeigneten Verbindungen seien als Beispiele nachfolgende aufgeführt:Examples include octadecyloxymethyl-pyridinium chloride and stearylamido-methyl-pyridinium chloride. However, quaternary compounds are particularly suitable as compounds (1) Imidazolinium derivatives and quaternary ammonium derivatives. The following are examples of the particularly suitable compounds:
1-Stearinsäureamidoethyl-2-stearyl-3-methyl-imidazoliniummethosulfat (Verbindung 1 a),1-stearic acid amidoethyl-2-stearyl-3-methyl-imidazolinium methosulfate (compound 1 a),
1-Methyl-2-Talgfettsäureamido-ethylimidazoliniummethosulfat (Verbindung 1 b),1-methyl-2-tallow fatty acid amido-ethyl imidazolinium methosulfate (compound 1 b),
1-Hydroxyethyl-2-heptadecenyl-imidazolinium-ethosulfat (Verbindung 1 c),1-hydroxyethyl-2-heptadecenyl imidazolinium ethosulfate (compound 1 c),
Dimethyl-distearyl-ammoniumchlorid (Verbindung 1 d) undDimethyl-distearyl-ammonium chloride (compound 1 d) and
Diölsäureisopropylester-dimethyl-ammonium-ethosulfat (Verbindung 1 e).Isopropyl diolate dimethyl ammonium ethosulfate (Compound 1 e).
Die verwendeten Mengen an Verbindungen (1) bewegen sich von 20 bis 70 g, insbesondere 30 bis 60 g auf 1000 g wäßrige Dispersion.The amounts of compounds (1) used range from 20 to 70 g, in particular 30 to 60 g, per 1000 g of aqueous dispersion.
Als Verbindungen (2) kommen die bekannten Polymerisate bzw. Copolymerisate auf Basis von Alkylacrylaten mit Alkylresten mit mindestens 4 C-Atomen zur Anwendung. Die Alkylreste in diesen Verbindungen (2) weisen dabei vorzugsweise 4 bis 10, insbesondere 4 bis 8 C-Atome auf. Als Beispiele für derartige Basismonomere, die in Mengen von 60 bis 100 Gew.%, bezogen auf das gesamte Polymerisat, in demselben enthalten sind, seien folgende genannt:The known polymers or copolymers based on alkyl acrylates with alkyl radicals having at least 4 C atoms are used as compounds (2). The alkyl radicals in these compounds (2) preferably have 4 to 10, in particular 4 to 8, carbon atoms. The following may be mentioned as examples of such base monomers, which are contained in the same in amounts of 60 to 100% by weight, based on the total polymer:
2-Ethylhexylacrylat, Decylacrylat und vor allem Butylacrylat. Homopolymere von Butylacrylat sind besonders gut als Verbindungen (2) geeignet, während Ethylacrylat als Basismonomer nicht verwendbar ist. Neben den Alkylacrylathomopolymeren sind als Verbindungen (2) auch auf den entsprechenden Monomeren basierende Copolymerisate verwendbar.2-ethylhexyl acrylate, decyl acrylate and especially butyl acrylate. Homopolymers of butyl acrylate are particularly suitable as compounds (2), while ethyl acrylate cannot be used as the base monomer. In addition to the alkyl acrylate homopolymers, copolymers based on the corresponding monomers can also be used as compounds (2).
Als Comonomere seien ohne Anspruch auf Vollständigkeit folgende genannt (jeweils bezogen auf Summe der Monomeren):The following may be mentioned as comonomers without any claim to completeness (in each case based on the sum of the monomers):
2-Hydroxyethyl- bzw. 3-Hydroxypropyl-(meth)acrylat (2 bis 10 Gew . % ) , Alkylmethacrylate mit mindestens 4 C-Atomen im Alkylrest (2 bis 20 Gew.%), Ethylacrylat (1 bis 40 Gew.%), (Meth)acrylsäure (1 bis 5 Gew.%), Amide oder NMethylolamide bzw. mit Alkoholen mit 1 bis 4 C-Atomen veretherte Methylolamide α , ß-ungesättigter Carbonsäuren oder Gemische solcher Monomeren (0,5 bis 5 Gew./5), Vinylacetat (2 bis 40 Gew . % ) und Acrylnitril (1 bis 10 Gew.%).2-hydroxyethyl or 3-hydroxypropyl (meth) acrylate (2 to 10% by weight), alkyl methacrylates with at least 4 carbon atoms in the alkyl radical (2 to 20% by weight), ethyl acrylate (1 to 40% by weight) , (Meth) acrylic acid (1 to 5 wt.%), Amides or NMethylolamides or methylolamides etherified with alcohols with 1 to 4 carbon atoms α, ß-unsaturated carboxylic acids or mixtures of such monomers (0.5 to 5 wt ), Vinyl acetate (2 to 40% by weight) and acrylonitrile (1 to 10% by weight).
Diese Verbindungen (2) kommen in Form 30 bis 70%iger wäßriger Dispersionen in den Handel, wobei zur Herstellung der erfindungsgemäßen wäßrigen Dispersionen 20 bis 80 g. insbesondere 20 bis 60 g Verbindungen (2), gerechnet als 100%iges Polymerisat, zur Anwendung gelangen.These compounds (2) come in the form of 30 to 70% strength aqueous dispersions, 20 to 80 g of which are used to prepare the aqueous dispersions according to the invention. in particular 20 to 60 g of compounds (2), calculated as a 100% polymer, are used.
Von Fall zu Fall, vor allem wenn relativ geringe Mengen an Verbindungen (1) zum Einsatz gelangen oder wenn erhöhte Anforderungen an die Verträglichkeit mit optischen Aufhellern gestellt werden, ist es notwendig, neben den Ver- bindungen (1) noch einen zusätzlichen Emulgator bei der Herstellung der wäßrigen Dispersionen einzusetzen. Als Emulgatoren werden dabei die bekannten nicht-ionogenen und/oder von (1) verschiedenen kationaktiven Emulgatoren (3) verwendet. Der Fachmann kennt die ethoxylierten Fettalkohole, Fettamide, Fettsäuren, Alkylphenole und Fettamine bzw. deren Salze oder die verwendeten z.B. quaternären Ammoniumverbindungen und wird keine Schwierigkeiten haben, diese Verbindungen entsprechend auszuwählen. Die Mengen an Emulgator (3) können bis zu 100 Gew . % , bezogen auf Verbindung (2), betragen.From case to case, especially if relatively small amounts of compounds (1) are used or if higher requirements are placed on compatibility with optical brighteners, it is necessary to add an additional emulsifier to the (1) Use production of the aqueous dispersions. The known nonionic and / or cationic emulsifiers (3) which are different from (1) are used as emulsifiers. The person skilled in the art knows the ethoxylated fatty alcohols, fatty amides, fatty acids, alkylphenols and fatty amines or their salts or the quaternary ammonium compounds used, for example, and will have no difficulty in selecting these compounds accordingly. The amounts of emulsifier (3) can be up to 100 wt. %, based on compound (2).
Ein besonders angenehmer und weicher Griff der behandelten Fasermaterialien und vor allem eine merklich gesteigerte Hydrophilität wird dann erhalten, wenn die wäßrige Dispersion zusätzlich mindestens ein hydrophilisierend wirkendes Silikon enthält, und zwar in Mengen von 5 bis 70 g, insbesondere 15 bis 55 g auf 1000 g wäßrige Dispersion. Diese zusätzlich verwendeten Verbindungen (4) sind dem Fachmann ebenfalls bekannt. Im allgemeinen handelt es sich um Dimethylpolysiloxane, die Epoxygruppen (a) und/oder Polyethoxy- bzw. Polypropoxy- bzw. Polyethoxy/Propoxy-Gruppen (b) eingebaut enthalten.A particularly pleasant and soft feel of the treated fiber materials and, above all, a noticeably increased hydrophilicity is obtained if the aqueous dispersion additionally contains at least one hydrophilizing silicone, in quantities of 5 to 70 g, in particular 15 to 55 g per 1000 g aqueous dispersion. These additionally used compounds (4) are also known to the person skilled in the art. In general, these are dimethylpolysiloxanes which contain epoxy groups (a) and / or polyethoxy or polypropoxy or polyethoxy / propoxy groups (b) incorporated.
Besonders geeignet sind solche Silikone, die im gleichen Molekül die Gruppen (a) und (b) aufweisen. Ein typischer Vertreter für die Verbindungen (4) ist UCARSIL® EPS (Union Carbide Corp.). Der Fachmann wird keine Schwierigkeiten haben, ähnliche verwendbare Verbindungen aufzufinden.Silicones which have groups (a) and (b) in the same molecule are particularly suitable. A typical representative of the compounds (4) UCARSIL® ® EPS (Union Carbide Corp.). Those skilled in the art will have no difficulty in finding similar useful compounds.
Entscheidend für die Wirksamkeit der erfindungsgemäßen, wäßrigen Dispersionen ist, daß die Herstellung der Verbindungen (2) in Gegenwart der Verbindungen (1) und gegebenenfalls der Verbindungen (4) erfolgt. Gegenstand der Erfindung ist deshalb weiterhin ein Verfahren zur Herstellung der erfindungsgemäßen wäßrigen Dispersionen. Grundsätzlich ist die Herstellung solcher Dispersionen bekannt. Im allgemeinen wird eine Monomerenemulsion be reitet, die neben den Alkylacrylaten mit Alkylresten mit mindestens 4 C-Atomen und gegebenenfalls weiteren Comonomeren und eventuell dem Emulgator (3) die quaternäre Verbindung mit mindestens einem langkettigen Alkylrest und bevorzugt auch die Verbindung (4) enthält.It is crucial for the effectiveness of the aqueous dispersions according to the invention that the compounds (2) are prepared in the presence of the compounds (1) and, if appropriate, the compounds (4). The invention therefore also relates to a process for the preparation of the aqueous dispersions according to the invention. The production of such dispersions is known in principle. In general, a monomer emulsion is rides, which in addition to the alkyl acrylates with alkyl radicals with at least 4 carbon atoms and optionally further comonomers and possibly the emulsifier (3) contains the quaternary compound with at least one long-chain alkyl radical and preferably also the compound (4).
Die eigentliche Polymerisation wird nun in bekannter Weise vorgenommen. Selbstverständlich können der Monomeremulsion und/oder der fertigen wäßrigen Dispersion noch weitere bekannte Textilhilfsmittel, insbesondere Weichmacher und/ oder griffgebende Substanzen in geringer Menge zugesetzt werden, um die Eigenschaften der wäßrigen Dispersion abzurunden.The actual polymerization is now carried out in a known manner. Of course, other known textile auxiliaries, in particular plasticizers and / or substances which give grip, can be added to the monomer emulsion and / or the finished aqueous dispersion in small amounts in order to round off the properties of the aqueous dispersion.
Die erhaltenen wäßrigen Dispersionen dienen zur weichmachenden und hydrophilisierenden Ausrüstung von Fasermaterialien aller Art, insbesondere von Frottee-Waren, vor allem Baumwoll-Frottee-Waren, aber auch von Bettwäsche.The aqueous dispersions obtained serve for the softening and hydrophilizing finishing of fiber materials of all kinds, in particular terry goods, especially cotton terry goods, but also of bed linen.
Dazu werden die Textilien mit Flotten, die 15 bis 80 g/l, insbesondere 20 bis 60 g/l der wäßrigen Dispersion, bezogen auf eine Dispersion mit einem Feststoffgehalt von ca. 20 Gew. % , enthalten, in bekannter Weise behandelt, wodurch eine Auflage von etwa 0,3 bis 3 % Festsubstanz auf dem Fasermaterial resultiert. Durch kurze Nachkondensation kann dabei die Hydrophilität noch gesteigert werden.For this purpose, the textiles are treated in a known manner with liquors which contain 15 to 80 g / l, in particular 20 to 60 g / l, of the aqueous dispersion, based on a dispersion with a solids content of about 20% by weight, so that a A coating of about 0.3 to 3% solid substance results on the fiber material. The hydrophilicity can be increased by brief post-condensation.
Es ist überraschend, daß es auf diese einfache Art und Weise gelingt, einen weichen, flauschigen Griff und gleichzeitig eine gute bis hervorragende Hydrophilität der ausgerüsteten Materialien zu erhalten, nachdem durch einfaches Mischen der Verbindungen (1) und (2) (siehe auch nachfolgende Beispiele) ein solcher Kombinationseffekt nicht erreichbar ist. Die Erfindung wird durch die nachfolgenden Beispiele näher beschrieben, wobei Teile = Gewichtsteile und % = Gewichtsprozent sind.It is surprising that in this simple manner it is possible to obtain a soft, fluffy feel and at the same time a good to excellent hydrophilicity of the finished materials, after simply mixing the compounds (1) and (2) (see also the examples below ) such a combination effect cannot be achieved. The invention is described in more detail by the following examples, parts = parts by weight and% = percent by weight.
Beispiel 1example 1
A) Eine Voremulsion wird durch Vorlegen und Aufschmelzen bei 80 bis 90°C aus 37,5 Teilen 1-Methyl-2-Talgfettsäureamido-ethyl-imidazolinmethosulfat und 20 Teilen des Acetats eines ethoxylierten C-16-Fettamins (insgesamt 10 EO-Gruppen je Mol) als zusätzlicher Emulgator und nachfolgender Zugabe von 550 Teilen 90ºC heißem Wasser, abkühlen auf 40°C und weiterer Zugabe von 2,5 Teilen Phosphorsäure (pH 5 bis 6), 60 Teilen Butylacrylat und 45 Teilen UCARSIL® EPS unter Rühren hergestellt.A) A pre-emulsion is prepared from 37.5 parts of 1-methyl-2-tallow fatty acid amido-ethyl-imidazoline methosulfate and 20 parts of the acetate of an ethoxylated C-16 fatty amine (total of 10 EO groups each Mol) as an additional emulsifier and subsequent addition of 550 parts of 90 ° C hot water, cooling to 40 ° C and further addition of 2.5 parts of phosphoric acid (pH 5 to 6), 60 parts of butyl acrylate and 45 parts of UCARSIL ® EPS with stirring.
Zur Polymerisation werden 100 Teile Wasser und 3 Teile des obengenannten Emulgators vorgelegt , mit 0 , 2 Teilen Phosphorsäure auf einen pH-Wert von 4 eingestellt und 100 Teile der wie oben beschrieben bereiteten Voremulsion zugegeben. Das Gemisch wird nunmehr auf 60ºC erwärmt und mit 3 Teilen Natriumpersulfatlösung (25%.ig) und 2 Teilen Rongalit C-Lösung (10%ig) geimpft. Unter Zulauf des restlichen Monomerengemisches erfolgt bei 65 bis 70°C die Polymerisation während 1 Stunde, wobei gleichzeitig kontinuierlich 3 Teile der Natriumpersulfatlösung und 8 Teile der® Rongalit C-Lösung (BASF) zugegeben werden. Anschließend werden nochmals 2 Teile Natriumpersulfatlösung und 2 Teile Rongalit C-Lösung nachgesetzt und der Ansatz 1 Stunde bei 65 bis 70ºC nachgerührt.For the polymerization, 100 parts of water and 3 parts of the above-mentioned emulsifier are introduced, adjusted to a pH of 4 with 0.2 part of phosphoric acid and 100 parts of the pre-emulsion prepared as described above are added. The mixture is now heated to 60 ° C and inoculated with 3 parts sodium persulfate solution (25%) and 2 parts Rongalit C solution (10%). Under the inlet of the remaining monomer mixture, the polymerization is carried out for 1 hour at 65 to 70 ° C, at the same time continuously, 3 parts of sodium persulfate solution and 8 parts of Rongalit C ® solution (BASF) are added. Then another 2 parts of sodium persulfate solution and 2 parts of Rongalit C solution are added and the mixture is stirred for 1 hour at 65 to 70 ° C.
Abschließend wird durch Zugabe eines Gemisches aus 0,5 g tert.-Butylhydroperoxid und 0,5 g des obengenannten Emulgators (50%ig in Wasser) der Restmonomergehalt auf unterr 0 , 2 % gesenkt .Finally, by adding a mixture of 0.5 g of tert-butyl hydroperoxide and 0.5 g of the above-mentioned emulsifier (50% in water), the residual monomer content is reduced to below 0.2% reduced.
Bei 50ºC wird danach mit 6 Teilen Triethanolamin auf einen pH-Wert von 6 bis 7 eingestellt und abschließend das Produkt in bekannter Weise filtriert. Es wird eine gut kältebeständige, stabile wäßrige Dispersion erhalten.The pH is then adjusted to 6 to 7 with 6 parts of triethanolamine at 50 ° C. and the product is then filtered in a known manner. A good cold-resistant, stable aqueous dispersion is obtained.
B) Zur Herstellung der wäßrigen Dispersion B wird in gleicher Weise wie oben gearbeitet, wobei jedoch in Abwesenheit von UCARSIL® EPS polymerisiert wird.B) The aqueous dispersion B is prepared in the same manner as above, but polymerisation is carried out in the absence of UCARSIL ® EPS.
C) Wie Dispersion B), wobei aber 45 Teile UCARSIL® EPS abschließend kalt eingerührt werden.C) Like dispersion B), but 45 parts of UCARSIL ® EPS are then stirred in cold.
D) Zum Vergleich wird die unter A) beschriebene Arbeitsweise in gleicher Weise in Abwesenheit der Verbindung (1 b) und des UCARSIL® EPS durchgeführt. Dafür werden aber nach erfolgter Polymerisation 37,5 Teile der Verbindüng (1 b) kalt eingerührt.D) For comparison, the procedure described under A) is carried out in the same way in the absence of the compound (1 b) and the UCARSIL ® EPS. However, 37.5 parts of the compound (1 b) are stirred in cold after the polymerization.
Mit 40 g/l der wie oben beschrieben hergestellten wäßrigenWith 40 g / l of the aqueous prepared as described above
Dispersionen A) bis D) wird eine schwere Baumwoll-FrotteeWare (450 g/m2 ) durch Eintauchen in die Flotte, Abquetschen auf 110 % Flottenaufnahme und Trocknen während 15 Minuten bei 120°C ausgerüstet (Feststoffaufläge ca. 1 % ) .Dispersions A) to D) are treated with a heavy cotton terry fabric (450 g / m 2 ) by immersing them in the liquor, squeezing to 110% liquor absorption and drying at 120 ° C. for 15 minutes (solids deposits approx. 1%).
Das ausgerüstete Material weist folgende Effekte auf: Wäßrige Dispersion Griff HydrophilitätThe finished material has the following effects: Aqueous dispersion handle hydrophilicity
A ) ++(+) +++ ) erfindungs- B ) +++ + ) gemäßA) ++ (+) +++) invention B) +++ +) according to
C ) + +++C) + +++
D ) Vergleich +(-)D) comparison + (-)
LegendeLegend
GriffHandle
+++ sehr weicher, flauschiger Griff ++ weicher, flauschiger Griff + weicher Griff +- mäßig weicher Griff - kein Weichgriffeffekt+++ very soft, fluffy handle ++ soft, fluffy handle + soft handle + - moderately soft handle - no soft handle effect
HydrophilitätHydrophilicity
+++ ausgezeichnet hydrophil+++ excellent hydrophilic
++ sehr gut hydrophil++ very good hydrophilic
+ gut hydrophil+ good hydrophilic
+- mäßig hydrophil - nicht hydrophil (hydrophob)+ - moderately hydrophilic - not hydrophilic (hydrophobic)
Die vorstehenden Ergebnisse machen deutlich, daß nur durch die erfindungsgemäßen wäßrigen Dispersionen gleichzeitig ein weicher, angenehmer Griff und eine gute bis sehr gute Hydrophilität erhalten werden.The above results make it clear that only through the aqueous dispersions according to the invention are simultaneously obtained with a soft, pleasant feel and good to very good hydrophilicity.
Beispiel 2Example 2
Das Beispiel 1 wird in gleicher Weise wiederholt, wobei aber als quaternäre Verbindung mit mindestens einem langkettigen Alkylrest die Verbindung (1 d) zum Einsatz kommt. Der mit den entsprechend Beispiel 1 hergestellten wäßrigen Flotten ausgerüstete Baumwoll-Frottee zeigt nunmehr folgende Effekte:Example 1 is repeated in the same way, but using compound (1 d) as the quaternary compound having at least one long-chain alkyl radical. The cotton terry finished with the aqueous liquors prepared in accordance with Example 1 now shows the following effects:
Wäßrige Dispersion Griff Hydrophilität A) ++ ++ ) erfindungs-Aqueous dispersion handle hydrophilicity A) ++ ++) invention
B ) ++ ) gemäß C) ++B) ++) according to C) ++
D ) Vergleich + (-)D) comparison + (-)
Beispiel 3Example 3
Anstelle der in Beispiel 1 verwendeten Verbindung (1 b) wird in diesem Beispiel unter Verwendung der VerbindungInstead of the compound (1 b) used in Example 1, this example uses the compound
(1 e) entsprechend B) eine wäßrige Dispersion hergestellt, wobei zusätzlich gleich zu Beginn 50 Teile Glycerinmonoisostearat mit aufgeschmolzen werden und dafür die Heißwassermenge auf 740 Teile erhöht wird. Die mit dieser Dispersion B) ausgerüstete Baumwoll-Frottee-Ware weist ebenfalls einen weichen, flauschigen Griff und eine gute bis sehr gute Hydrophilität auf.(1 e) in accordance with B) an aqueous dispersion is prepared, in addition, 50 parts of glycerol monoisostearate are melted at the beginning and the amount of hot water is increased to 740 parts. The cotton terry cloth finished with this dispersion B) also has a soft, fluffy feel and good to very good hydrophilicity.
Beispiel 4Example 4
In gleicher Weise wie im Beispiel 1 beschrieben wird unter Verwendung von 40 g eines Emulgator-Gemisches ausIn the same way as described in Example 1, 40 g of an emulsifier mixture are used
250 Teilen Rezinolsäurepolyglykolester (durchschnittlich250 parts of polyvinyl glycol ester (average
12 Ethylenoxideinheiten),12 ethylene oxide units),
200 Teilen Stearylaminethoxylat (durchschnittlich 8 Ethylenoxideinheiten) und200 parts of stearylamine ethoxylate (8 ethylene oxide units on average) and
6 Teilen Eisessig unter Verwendung einer Mischung aus6 parts glacial acetic acid using a mixture of
40 Teilen Butylacrylat,40 parts of butyl acrylate,
10 Teilen 2-Ethylhexylacrylat und10 parts of 2-ethylhexyl acrylate and
10 Teilen Vinylacetat10 parts of vinyl acetate
eine Monomeremulsion bereitet und dann wie im Beispiel 1 unter A) beschrieben, die wäßrige Dispersion hergestellt, die mit optischen Aufhellern verträglich ist.prepares a monomer emulsion and then, as described in Example 1 under A), produces the aqueous dispersion which is compatible with optical brighteners.
Unter Verwendung von 35 g/l dieser wäßrigen Dispersion wird eine leichte Baumwoll-Frottee-Handtuchware (240 g/m2) durch Eintauchen in die Flotte, Abquetschen auf 100 % Flottenaufnahme und Trocknen während 10 Minuten bei 120ºC ausgerüstet. Die so behandelte Ware zeigt einen sehr weichen, flauschigen Griff und ist auch durch eine besonders gute Hydrophilität charakterisiert.Using 35 g / l of this aqueous dispersion, a light cotton terry towel (240 g / m 2 ) is finished by immersing it in the liquor, squeezing to 100% liquor absorption and drying at 120 ° C. for 10 minutes. The goods treated in this way show a lot soft, fluffy feel and is also characterized by a particularly good hydrophilicity.
Beispiel 5Example 5
In gleicher Weise wie im Beispiel 4 wird unter Verwendung des nachfolgend genannten Monomergemisches eine Monomeremulsion hergestellt und dann wie beschrieben, die wäßrige Dispersion bereitet:In the same way as in Example 4, a monomer emulsion is prepared using the monomer mixture mentioned below and then, as described, the aqueous dispersion is prepared:
40 Teile Butylacrylat,40 parts of butyl acrylate,
5 Teile n-Decylacrylat, 8 Teile Acrylnitril und5 parts of n-decyl acrylate, 8 parts of acrylonitrile and
2 Teile N-Methylolacrylamid.2 parts of N-methylolacrylamide.
Wird die in Beispiel 4 beschriebene Frottee-Ware in gleicher Weise unter Verwendung von 50 g/l dieser Dispersion ausgerüstet, so werden ähnlich gute Effekte erhalten.If the terry cloth described in Example 4 is finished in the same way using 50 g / l of this dispersion, similarly good effects are obtained.
Beispiel 6Example 6
Das Beispiel 3 wird wiederholt, wobei aber in Abwesenheit des dort verwendeten Acetats eines ethoxylierten C-16-Fettamins (durchschnittlich 10 Ethylenoxidgruppen) gearbeitet wird.Example 3 is repeated, but the absence of the acetate of an ethoxylated C-16 fatty amine used there (on average 10 ethylene oxide groups).
Die dabei hergestellte wäßrige Dispersion ist etwas schlechter filtrierbar, kann aber ebenfalls sehr gut zur Ausrüstung der verschiedensten Frottee-Waren herangezogen werden. The aqueous dispersion produced in this way is somewhat less filterable, but can also be used very well to equip a wide variety of terry goods.
INTERNATIONALE ANMELDUNG VERÖFFENTLICHT NACH DEM VERTRAG ÜBER DIE INTERNATIONALE ZUSAMMENARBEIT AUF DEM GEBIET DES PATENTWESENS (PCT)INTERNATIONAL APPLICATION PUBLISHED AFTER THE INTERNATIONAL COOPERATION AGREEMENT IN THE PATENT AREA (PCT)
(51) Internationale Patentklassifikation (11) Internationale Veröffentlichungsnummer: WO 88/ 0 D06M 15/263; 15/643, 13/34 A3 (43) Internationales(51) International Patent Classification (11) International Publication Number: WO 88/0 D06M 15/263; 15/643, 13/34 A3 (43) International
Veröffentlichungsdatum : 11. Februar 1988 (11.0Release DATE: February 11, 1988 (11.0
(21) Internationales Aktenzeichen : PCT/EP87/00391 (74) Gemeinsamer Vertreter: CHEMISCHE FAB PFERSEE GMBH; Färberstraße 4, D-8900 Augs(21) International file number: PCT / EP87 / 00391 (74) Common representative: CHEMISCHE FAB PFERSEE GMBH; Färberstrasse 4, D-8900 Augs
(22) Internationales Anmeldedatum : 18. Juli 1987 (18.07.87) (DE).(22) International filing date: July 18, 1987 (July 18, 1987) (DE).
(31) Prioritätsaktenzeichen: P 36 26 051.7 (81) Bestimmungsstaaten: AT (europäisches Patent), BE (europäisches Patent), CH (europäisches Pat(31) Priority reference number: P 36 26 051.7 (81) Destination states: AT (European patent), BE (European patent), CH (European pat
(32) Prioritätsdatum: 1. August 1986 (01.08.86) DE (europäisches Patent), FR (europäisches Pat GB (europäisches Patent), IT (europäisches Pat(32) Priority date: August 1, 1986 (August 1, 1986) DE (European patent), FR (European patent GB (European patent), IT (European patent
(33) Prioritätsland: DE JP, LU (europäisches Patent), NL (europäische tent), SE (europäisches Patent), US.(33) Priority country: DE JP, LU (European patent), NL (European tent), SE (European patent), US.
(71) Anmelder (für alle Bestimmungsstaaten ausser US):(71) Applicant (for all destinations except US):
CHEMISCHE FABRIK PFERSEE GMBH [DE/ Veröffentlicht DE]; Färberstraße 4, D-8900 Augsburg (DE). Mit internationalem Recherchenbericht.CHEMISCHE FABRIK PFERSEE GMBH [DE / Published DE]; Färberstrasse 4, D-8900 Augsburg (DE). With international research report.
Vor Ablauf 'der 'für Änderungen der Ansprüche zugelBefore the 'expires ' for changes in claims
(72) Erfinder ;und(72) inventor; and
(75) Erfinder/Anmelder (nur für US) : SINGER, Heinrich Frist. Veröffentlichung wird wiederholt falls Änderu eintreffen. [DE/DE]; Brachflecken 7, D-8901 Horgau (DE). STE- CHELE, Werner [DE/DE]; Nebelhornstrasse 16, D- 8901 Diedorf (DE). BERNHEIM, Michael [DE/DE]; (88) Veröffentlichungsdatum des internationalen Recherche Sonnenweg 3, D-8901 Aystetten (DE). richts(75) Inventor / applicant (only for US): SINGER, Heinrich Frist. Publication will be repeated if changes occur. [DE / DE]; Brachflecken 7, D-8901 Horgau (DE). STECHELE, Werner [DE / DE]; Nebelhornstrasse 16, D-8901 Diedorf (DE). BERNHEIM, Michael [DE / DE]; (88) Publication date of international research Sonnenweg 3, D-8901 Aystetten (DE). judges
5. Mai 1988 (05.05May 5, 1988 (May 5
(54) Title: DISPERSIONS FOR PREPARING FIBROUS MATERIAL(54) Title: DISPERSIONS FOR PREPARING FIBROUS MATERIAL
(54) Bezeichnung: DISPERSIONEN AUSRÜSTUNG VON FASERMATERIALIEN(54) Name: DISPERSION EQUIPMENT OF FIBER MATERIALS
(57) Abstract(57) Abstract
Watery dispersions for simultaneously softening and providing fibrous materials with a hydrophilic finish contai at least one quatemary compound with at least one long-chain alkyl residue, 2) a polymerisate or copolymerisate on basis of alkylacrylates with alkyl residues having at least 4 C atoms, 3) if necessary one additional emulsifier different f 1), and 4) if necessary one hydrophilising Silicon. A process for producing these watery dispersions is also disclosed. T water dispersions give to fibrous materials, such as terry cotton fabrics, a specially soft, velvety feel and very good to markable hydrophilic characteristics.Watery dispersions for simultaneously softening and providing fibrous materials with a hydrophilic finish contai at least one quatemary compound with at least one long-chain alkyl residue, 2) a polymerisate or copolymerisate on basis of alkylacrylates with alkyl residues having at least 4 C atoms, 3 ) if necessary one additional emulsifier different f 1), and 4) if necessary one hydrophilizing silicone. A process for producing these watery dispersions is also disclosed. T water dispersions give to fibrous materials, such as terry cotton fabrics, a specially soft, velvety feel and very good to markable hydrophilic characteristics.
(57) Zusammenfassung(57) Summary
Wäßrige Dispersionen zur gleichzeitigen weichmachenden und hydrophilisierenden Ausrüstung von Fasermate lien enthaltend 1) mindestens eine quaternäre Verbindung mit mindestens einem langkettigen Alkylrest, 2) ein Polymer bzw. Copolymerisat auf Basis von Alkylacrylaten mit Alkylresten mit mindestens 4 C-Atomen, 3) gegebenenfalls zus lich einen von 1) verschiedenen Emulgator und 4) gegebenenfalls ein hydrophilisierendes Silikon. Außerdem wird ein fahren zur Herstellung dieser wäßrigen Dispersion beansprucht. Mit diesen wäßrigen Dispersionen wird Fasermaterial wie Baumvoll-Frottee- Waren ein besonders weicher, flauschiger Griff und eine sehr gute bis hervorragende Hydrophil verliehen. Aqueous dispersions for the simultaneous softening and hydrophilizing finishing of fiber materials containing 1) at least one quaternary compound with at least one long-chain alkyl radical, 2) a polymer or copolymer based on alkyl acrylates with alkyl radicals with at least 4 carbon atoms, 3) optionally additionally one from 1) different emulsifier and 4) optionally a hydrophilizing silicone. In addition, a drive to produce this aqueous dispersion is claimed. With these aqueous dispersions, fiber material such as cotton terry toweling is given a particularly soft, fluffy feel and a very good to excellent hydrophilicity.
LEDIGLICH ZUR INFORMATIONONLY FOR INFORMATION
Code, die zur Identifizierung von PCT-Vertragsstaaten aufden Kopfbögen der Schriften, die internationale Anmeldungen gemäss dem PCT veröffentlichen.Code used to identify PCT contracting states on the headers of publications that publish international applications under the PCT.
AT Österreich FR Frankreich MR MauritanienAT Austria FR France MR Mauritania
ALAustralien GA Gabun MW MalawiAL Australia GA Gabon MW Malawi
BE Barbados GB Vereinigtes Königreich NL NiederlandeBE Barbados GB United Kingdom NL Netherlands
BE Belgien HU Ungarn NO NorwegenBE Belgium HU Hungary NO Norway
BG Bulgarien rr Italien RO RumänienBG Bulgaria rr Italy RO Romania
BJ Benin JP Japan SD SudanBJ Benin JP Japan SD Sudan
BR Brasilien KP Demokratische Volksrepublik Korea SE SchwedenBR Brazil KP Democratic People's Republic of Korea SE Sweden
CF Zentrale Afrikanische Republik KR Republik Korea SN SenegalCF Central African Republic KR Republic of Korea SN Senegal
CG Kongo U Liechtenstein SU Soviel UnionCG Congo U Liechtenstein SU So much Union
CH Schweiz LK Sri Lanka TD TschadCH Switzerland LK Sri Lanka TD Chad
CM Kamerun LL* Luxemburg TG TogoCM Cameroon LL * Luxembourg TG Togo
DE Deutschland. Bundesrepublik MC Monaco US Vereinigte Staaten von AmerikaDE Germany. Federal Republic of MC Monaco US United States
DK Dänemark MG MadagaskarDK Denmark MG Madagascar
FT Finnland ML Mali FT Finland ML Mali

Claims

Patentansprüche Claims
1. Wäßrige Dispersion zur gleichzeitigen weichmachenden und hydrophilisierenden Ausrüstung von Fasermaterialien enthaltend1. Containing aqueous dispersion for simultaneous softening and hydrophilizing finishing of fiber materials
(1) mindestens eine quaternäre Verbindung mit mindestens einem langkettigen Alkylrest,(1) at least one quaternary compound with at least one long-chain alkyl radical,
(2) ein Polymerisat bzw. Copolymerisat auf Basis von Alkylacrylaten mit Alkylresten mit mindestens 4 C-Atomen,(2) a polymer or copolymer based on alkyl acrylates with alkyl radicals having at least 4 carbon atoms,
(3) gegebenenfalls zusätzlich einen von (1) verschiedenen Εmulgator und(3) optionally, an emulsifier and
(4) gegebenenfalls ein hydrophilisierendes Silikon.(4) optionally a hydrophilizing silicone.
2. Wäßrige Dispersion nach Patentanspruch 1, dadurch gekennzeichnet, daß als Verbindung (1) quaternäre Verbindungen mit mindestens einem gesättigten und/oder ungesättigten Alkylrest mit mindestens 12 C-Atomen enthalten sind.2. Aqueous dispersion according to claim 1, characterized in that quaternary compounds containing at least one saturated and / or unsaturated alkyl radical having at least 12 carbon atoms are present as the compound (1).
3. Wäßrige Dispersion nach den Patentansprüchen 1 und 2, dadurch gekennzeichnet, daß als Verbindung (1) quaternäre Imidazoliniumderivate enthalten sind.3. Aqueous dispersion according to claims 1 and 2, characterized in that quaternary imidazolinium derivatives are contained as compound (1).
4 . Wäßrige Dispersion nach den Patentansprüchen 1 und 2, dadurch gekennzeichnet, daß als Verbindungen (1) quaternäre Ammoniumderivate enthalten sind.4th Aqueous dispersion according to claims 1 and 2, characterized in that quaternary ammonium derivatives are contained as compounds (1).
5. Wäßrige Dispersion nach den Patentansprüchen 1 bis5. Aqueous dispersion according to claims 1 to
4, dadurch gekennzeichnet, daß das griffbildende (Co-)- Polymerisat (2) auf Alkylacrylaten mit Alkylresten von 4 bis 10, insbesondere 4 bis 8 C-Atomen als Basismonomer aufgebaut ist.4, characterized in that the handle-forming (Co -) - Polymer (2) is based on alkyl acrylates with alkyl radicals of 4 to 10, in particular 4 to 8, carbon atoms as the base monomer.
6. Wäßrige Dispersion nach den Patentansprüchen 1 bis 5, dadurch gekennzeichnet, daß 20 bis 70 g Verbindung (1), 20 bis 80 g Verbindung (2) und gegebenenfalls bis zu 100 Gew .% bezogen auf Verbindung (2) an Emulgator6. Aqueous dispersion according to claims 1 to 5, characterized in that 20 to 70 g of compound (1), 20 to 80 g of compound (2) and optionally up to 100% by weight, based on compound (2), of emulsifier
(3) auf 1000 g wäßrige Dispersion enthalten sind.(3) per 1000 g of aqueous dispersion.
7. Wäßrige Dispersion nach den Patentansprüchen 1 bis 6, dadurch gekennzeichnet, daß als Verbindung (4) mindestens ein hydrophilisierendes Dimethylpolysiloxan enthalten ist.7. Aqueous dispersion according to claims 1 to 6, characterized in that at least one hydrophilizing dimethylpolysiloxane is contained as compound (4).
8. Wäßrige Dispersion nach Patentanspruch 7, dadurch gekennzeichnet, daß die Verbindung (4) Epoxygruppen und/ oder Polyethoxy- bzw. Polypropoxy- bzw. Polyethoxy/propoxy-Gruppen enthält.8. Aqueous dispersion according to claim 7, characterized in that the compound (4) contains epoxy groups and / or polyethoxy or polypropoxy or polyethoxy / propoxy groups.
9. Wäßrige Dispersion nach den Patentansprüchen 7 und9. Aqueous dispersion according to claims 7 and
8, dadurch gekennzeichnet, daß 5 bis 70 g Verbindung8, characterized in that 5 to 70 g of compound
(4) auf 1000 g wäßrige Dispersion enthalten sind.(4) are contained per 1000 g of aqueous dispersion.
ιo. Wäßrige Dispersion nach den Patentansprüchen 1 bisιo. Aqueous dispersion according to claims 1 to
9, dadurch gekennzeichnet, daß weiterhin übliche Textilhilfsmittel enthalten sind.9, characterized in that conventional textile auxiliaries are also contained.
11. Verfahren zur Herstellung von wäßrigen Dispersionen nach den Patentansprüchen 1 bis 10, dadurch gekennzeichnet, daß in Gegenwart mindestens einer quaternären Verbindung mit mindestens einem langkettigen Alkylrest (1), gegebenenfalls einem üblichen nicht-ionogenen und/oder von (1) verschiedenen kationaktiven Emulgator (3) und gegebenenfalls mindestens einem hydrophilisierenden Silikon (4) in üblicher Weise Polymerisate bzw. Copolymerisate (2) auf Basis von Alkylacrylaten mit Alkylresten mit mindestens 4 C-Atomen hergestellt werden.11. A process for the preparation of aqueous dispersions according to claims 1 to 10, characterized in that in the presence of at least one quaternary compound having at least one long-chain alkyl radical (1), optionally a customary nonionic and / or from (1) different cationic emulsifier (3) and optionally at least one hydrophilizing silicone (4) in the usual way polymers or copolymers (2) based on alkyl acrylates with alkyl radicals with at least 4 carbon atoms.
12. Verfahren nach Patentanspruch 11, dadurch gekennzeichnet, daß die (Co) polymerisate (2) in Gegenwart quaternärer Verbindungen mit mindestens einem gesättigten und/oder ungesättigten Alkylrest mit mindestens 12 C-Atomen hergestellt werden.12. The method according to claim 11, characterized in that the (co) polymers (2) are prepared in the presence of quaternary compounds with at least one saturated and / or unsaturated alkyl radical having at least 12 carbon atoms.
13. Verfahren nach den Patentansprüchen 11 und 12, dadurch gekennzeichnet, daß die (Co) polymerisate (2) in Gegenwart von quaternären Imidazoliniumderivaten als Verbindung (1) hergestellt werden.13. The method according to claims 11 and 12, characterized in that the (co) polymers (2) are prepared in the presence of quaternary imidazolinium derivatives as compound (1).
14. Verfahren nach den Patentansprüchen 11 und 12, dadurch gekennzeichnet, daß die (Co) polymerisate (2) in Gegenwart von quaternären Ammoniumderivaten als Verbindung (1) hergestellt werden.14. The method according to claims 11 and 12, characterized in that the (co) polymers (2) are prepared in the presence of quaternary ammonium derivatives as the compound (1).
15. Verfahren nach den Patentansprüchen 11 bis 14, dadurch gekennzeichnet, daß zur Herstellung der (Co) -Polymerisate (2) Alkylacrylate mit Alkylresten von 4 bis 10, insbesondere 4 bis 8 C-Atomen als Basismonomere eingesetzt werden.15. The method according to claims 11 to 14, characterized in that for the preparation of the (co) polymers (2) alkyl acrylates with alkyl radicals of 4 to 10, in particular 4 to 8 carbon atoms are used as base monomers.
16. Verfahren zur Herstellung der wäßrigen Dispersionen nach den Patentansprüchen 11 bis 15, dadurch gekennzeichnet, daß die (Co) polymerisate (2) in Gegenwart von 20 bis 70 g Verbindungen (1), gegebenenfalls bis zu 100 Gew.%, bezogen auf Verbindungen (2), an Emul gatoren (3) und gegebenenfalls 5 bis 70 g an Verbindungen (4), jeweils bezogen auf 1000 g wäßriger Dispersion, durch Polymerisation von 20 bis 80 g Monomere, wobei als Basismonomer Alkylacrylate mit Alkylresten von 4 bis 10, insbesondere 4 bis 8 C-Atomen eingesetzt werden, hergestellt werden.16. A process for the preparation of the aqueous dispersions according to claims 11 to 15, characterized in that the (co) polymers (2) in the presence of 20 to 70 g of compounds (1), optionally up to 100% by weight, based on compounds (2), to Emul gators (3) and optionally 5 to 70 g of compounds (4), each based on 1000 g of aqueous dispersion, by polymerization of 20 to 80 g of monomers, alkyl acrylates with alkyl radicals of 4 to 10, in particular 4 to 8, C. Atoms are used to be produced.
17. Verfahren nach den Patentansprüchen 11 bis 16, dadurch gekennzeichnet, daß als Comonomere Vinylacetat, Acrylnitril, N-Methylolacrylamxd, gegebenenfalls verethert mit Alkoholen mit 1 bis 4 C-Atomen, in Mengen von 0,5 bis 40 Gew.%, bezogen auf die Summe der eingesetzten, polymerisierbaren Monomeren, eingesetzt werden.17. The method according to claims 11 to 16, characterized in that as comonomers vinyl acetate, acrylonitrile, N-methylolacrylamxd, optionally etherified with alcohols having 1 to 4 carbon atoms, in amounts of 0.5 to 40% by weight, based on the sum of the polymerizable monomers used.
18. Verwendung der wäßrigen Dispersion nach den PatentanSprüchen 1 bis 10 zur weichmachenden und hydrophilen18. Use of the aqueous dispersion according to claims 1 to 10 for softening and hydrophilic
Ausrüstung von Baumwoll-Frottee-Ware. Equipment of cotton terry goods.
EP87904867A 1986-08-01 1987-07-18 Dispersions for preparing fibrous material Expired - Lifetime EP0436524B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87904867T ATE82337T1 (en) 1986-08-01 1987-07-18 DISPERSIONS FOR FINISHING FIBER MATERIALS.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19863626051 DE3626051A1 (en) 1986-08-01 1986-08-01 AQUEOUS DISPERSIONS FOR THE SIMULTANEOUS SOFTENING AND HYDROPHILIZING EQUIPMENT OF FIBER MATERIALS, METHOD FOR THEIR PRODUCTION AND THEIR USE
DE3626051 1986-08-01

Publications (2)

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EP0436524A1 true EP0436524A1 (en) 1991-07-17
EP0436524B1 EP0436524B1 (en) 1992-11-11

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ID=6306476

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US (1) US4966725A (en)
EP (1) EP0436524B1 (en)
JP (1) JPH01503791A (en)
AT (1) ATE82337T1 (en)
AU (1) AU616157B2 (en)
DE (2) DE3626051A1 (en)
PT (1) PT85462B (en)
WO (1) WO1988000991A2 (en)
ZA (1) ZA875678B (en)

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DE3939549A1 (en) * 1989-11-30 1991-06-06 Henkel Kgaa Lubricant for textiles, partic. for thread during high speed mfr. - or processing contains alkyl acrylate or methacrylate homo-polymer or copolymer of specified min. limiting viscosity
JPH04119174A (en) * 1990-09-10 1992-04-20 Toray Dow Corning Silicone Co Ltd Textile-treatment agent
US5407728A (en) 1992-01-30 1995-04-18 Reeves Brothers, Inc. Fabric containing graft polymer thereon
US5486210A (en) 1992-01-30 1996-01-23 Reeves Brothers, Inc. Air bag fabric containing graft polymer thereon
DE4313085A1 (en) * 1993-04-21 1994-10-27 Stockhausen Chem Fab Gmbh Stable aqueous dispersions of quaternary ammonium compounds and imidazoline derivatives
US5408012A (en) * 1993-05-27 1995-04-18 Comfort Technologies, Inc. Polymers having enhanced durable hydrophilicity and durable rewetting properties and process of producing the same
DE4331642C1 (en) * 1993-09-17 1995-02-16 Peter Dr Kuhnle Impregnation mixture and the use thereof
US5413811A (en) * 1994-03-18 1995-05-09 Kimberly-Clark Corporation Chemical and mechanical softening process for nonwoven web
US5830240A (en) * 1996-10-23 1998-11-03 Solutia Inc. Fibers and textile materials having enhanced dyeability and finish compositions used thereon
US5944852A (en) * 1996-10-23 1999-08-31 Solutia Inc. Dyeing process
GB0029198D0 (en) * 2000-11-30 2001-01-17 Ciba Sc Holding Ag Liquid dispersion polymer compositions their preparation and their use
DE10242762A1 (en) * 2002-09-14 2004-03-18 Cognis Deutschland Gmbh & Co. Kg Aqueous dispersion of copolymerisates and emulsifiers which when combined with fluorinated compounds enable the proportion of these to be decreased without impairing hydrophobization efficiency of fibers and textiles
WO2006023853A1 (en) * 2004-08-23 2006-03-02 Nano-Tex, Inc. Compositions and methods for treating textiles to impart wrinkle resistance, softness and hydrophilicity

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GB1549180A (en) * 1975-07-16 1979-08-01 Procter & Gamble Textile treating compositions
JPS581231B2 (en) * 1975-12-27 1983-01-10 タケモトユシ カブシキガイシヤ Shinkinagoseisen Iyojiyunanshigesai
JPS52132194A (en) * 1976-04-30 1977-11-05 Lion Fat Oil Co Ltd Softening agent composition for fiber article
DE2857180A1 (en) * 1977-07-06 1980-01-31 Procter & Gamble Europ CONCENTRATED LIQUID SOFTENER COMPOSITION
US4155855A (en) * 1977-07-06 1979-05-22 The Procter & Gamble Company Concentrated liquid fabric softener composition
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US4179382A (en) * 1977-11-21 1979-12-18 The Procter & Gamble Company Textile conditioning compositions containing polymeric cationic materials
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GB8428401D0 (en) * 1984-11-09 1984-12-19 Dow Corning Ltd Organosiloxane-oxy-alkylene copolymers

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EP0436524B1 (en) 1992-11-11
PT85462B (en) 1990-06-29
DE3626051A1 (en) 1988-02-11
JPH01503791A (en) 1989-12-21
US4966725A (en) 1990-10-30
ATE82337T1 (en) 1992-11-15
ZA875678B (en) 1988-03-30
PT85462A (en) 1987-08-01
WO1988000991A2 (en) 1988-02-11
AU616157B2 (en) 1991-10-24
AU7784287A (en) 1988-02-24
WO1988000991A3 (en) 1988-05-05
DE3782665D1 (en) 1992-12-17

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