EP1597425A1 - Procede d'impermeabilisation de matieres textiles - Google Patents

Procede d'impermeabilisation de matieres textiles

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Publication number
EP1597425A1
EP1597425A1 EP04706158A EP04706158A EP1597425A1 EP 1597425 A1 EP1597425 A1 EP 1597425A1 EP 04706158 A EP04706158 A EP 04706158A EP 04706158 A EP04706158 A EP 04706158A EP 1597425 A1 EP1597425 A1 EP 1597425A1
Authority
EP
European Patent Office
Prior art keywords
organic
optionally
liquor
weight
water
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
EP04706158A
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German (de)
English (en)
Other versions
EP1597425B1 (fr
Inventor
Harald Keller
Jürgen Reichert
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BASF SE
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BASF SE
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Publication of EP1597425A1 publication Critical patent/EP1597425A1/fr
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Publication of EP1597425B1 publication Critical patent/EP1597425B1/fr
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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
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • 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
    • 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
    • D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • 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
    • D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • D06M15/233—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated aromatic, e.g. styrene
    • 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
    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
    • 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
    • D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
    • 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
    • D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/33—Esters containing fluorine
    • 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
    • D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • 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
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties

Definitions

  • the present invention relates to a process for finishing textile materials by treatment with at least one aqueous liquor which contains at least one organic polymer and at least one organic or inorganic solid in particulate form, the organic or inorganic solids in the liquor in one proportion of at least 5.5 g / l.
  • Finishing textiles is an area of increasing economic importance. It is particularly interesting to make textiles water and dirt repellent. In some cases, modern measures use the so-called Lotus-Effect® and give textiles a water-repellent behavior by applying a rough surface.
  • WO 96/04123 describes self-cleaning surfaces which have an artificial surface structure which has elevations and depressions, the structure being characterized in particular by its structural parameters.
  • the structures are produced, for example, by embossing a structure on a thermoplastic deformable hydrophobic material or by applying Teflon powder to a surface treated with UHU®. From US 3,354,022 similarly produced water-repellent surfaces are known.
  • WO 02/84013 proposes hydrophobicizing fibers made of polyester, for example, by pulling them through a decalin bath heated to 80 ° C., in which 1% hydrophobic Aerosil® 8200 silica gel has been suspended.
  • WO 02/84016 proposes to make polyester fabrics hydrophobic by pulling them through a bath of DMSO (dimethyl sulfoxide) heated to 50 ° C., in which 1% of Aeroperl® 8200 hydrophobic silica gel has been suspended. Both methods of hydrophobization have in common that the solvent is selected so that the fibers are partially dissolved. To do this, it is necessary to use large amounts of organic solvent, which is undesirable in many cases. In addition, the mechanical strength of the fibers can be influenced by treatment with organic solvents.
  • DMSO dimethyl sulfoxide
  • WO 01/75216 proposes to make textile fibers and fabrics repel water and dirt by providing them with a two-component layer, one of which is a dispersing agent and the other is, for example, a colloid.
  • finishing layers are produced in which the colloids are anisotropically distributed in the dispersant, an accumulation of the colloids being observed at the interface between the finishing layer and the surrounding surface.
  • the process uses equipment liquors that contain up to 5 g / l Aerosil 812 S.
  • the object was therefore to provide a process for finishing textile materials which does not have the disadvantages outlined above and at the same time has a very good water and dirt-repellent effect. There was still the task of providing dirt and water-repellent textiles. Furthermore, the task was to provide fleets for the protection and water-repellent finishing of textile materials.
  • textile materials are to be understood as fibers, roving, yarn, twine on the one hand and textile fabrics on the other hand, such as, for example, woven goods, knitwear, nonwovens and clothing.
  • Textile fabrics which are used, for example, for the production of textile in the exterior are particularly preferred. Examples include sails, sunshades and umbrellas, tarpaulins, tent sheets, tablecloths, awning fabrics and furniture coverings, for example for chairs, swings or benches.
  • Textile materials in the sense of the present invention can consist of different substances. Natural fibers and synthetic fibers as well as mixed fibers are mentioned. Natural fibers include silk, wool and cotton. Synthetic fibers include polyamide, polyester, polypropylene, polyacrylonitrile, polyethylene terephthalate and viscose. Also leave modified natural fibers coat by the process according to the invention, for example cellulose acetate.
  • aqueous liquors are understood to mean those liquors which can contain at least 5% by weight of water.
  • Aqueous liquors preferably contain at least 25% by weight of water, particularly preferably at least 50% by weight and very particularly preferably at least 75% by weight.
  • the maximum water content is 99% by weight, preferably 97% by weight, particularly preferably 95% by weight.
  • aqueous liquors used according to the invention can contain organic solvents, for example methanol, ethanol, isopropanol, acetone, methyl ethyl ketone, methyl isobutyl ketone, ethylene glycol mono-n-butyl ether, ethylene glycol mono-isobutyl ether, acetic acid, n-butanol, iso- Butanol, n-hexanol and isomers, n-octanol and isomers, n-dodecanol and isomers.
  • Organic solvents can make up 1 to 50% by weight, preferably 2 to 25% by weight, of the aqueous liquor used according to the invention.
  • At least one of the liquors used in the process according to the invention contains at least one organic polymer.
  • Organic polymers can serve as binders.
  • the effect of a binder can be such that the organic polymer forms a film and connects the particles to one another and to the textile material to be coated.
  • At least one organic polymer is a polymer or copolymer of ethylenically unsaturated hydrophobic monomer which has a solubility in water of less than 1 g / l, determined at 25 ° C.
  • hydrophobic monomers make up at least 50% by weight, preferably at least 75% by weight, of the copolymer.
  • Preferred monomers are selected from the groups of
  • C 2 -C 24 olefins in particular ⁇ -olefins having 2 to 24 C atoms, for example ethylene, propylene, 1-butene, isobutene, 1-hexene, 1-octene, 1-decene, 1-dodecene, 1-hexadecene or 1-octadecene;
  • Vinyl aromatics for example styrene, ⁇ -methylstyrene, cis-stilbene, trans-stilbene, diolefins such as, for example, 1,3-butadiene, cyclopentadiene, chloroprene or isoprene, C 5 -C 18 -cycloolefins such as, for example, cyclopentene, cyclohexene, norbornene, dimeric cyclopentadiene, Vinyl esters of linear or branched CC 2 o-alkane carboxylic acids such as, for example, vinyl acetate, vinyl propionate, vinyl n-butyrate, vinyl n-hexanoate, vinyl n-octanoate, vinyl laurate and vinyl stearate,
  • (Meth) acrylic acid esters of C 1 -C 4 alcohols for example methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, iso-propyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate), tert-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, n-decyl (meth) acrylate, n-dodecyl (meth) acrylate , n-eicosyl (meth) acrylate and very particularly preferably from the groups of the halogenated monomers and the monomers with siloxane groups.
  • Halogenated monomers include chlorinated olefins such as vinyl chloride and vinylidene chloride.
  • halogenated monomers are fluorine-containing olefins such as, for example, vinylidene fluoride, trifluorochloroethylene, tetrafluoroethylene, hexafluoropropylene, vinyl esters of fluorinated or perfluorinated Cs-C ⁇ -carboxylic acids, as described, for example, in US Pat. No. 2,592,069 and US Pat. No. 2,732,370
  • (Meth) acrylic acid esters of fluorinated or perfluorinated alcohols such as fluorinated or perfluorinated C 3 -C 14 alkyl alcohols, for example (meth) acrylate esters of HO-CH 2 -CH 2 -CF 3 , HO-CH 2 -CH 2 -C 2 F 5 ,
  • HO-CH 2 -CH 2 -nC 3 F 7 HO-CH 2 -CH 2 -iso-C 3 F 7 , HO-CH 2 -GH 2 -n- C ⁇ F-js, HO-CH 2 -GH2-n-CaF ⁇ , HO-GH2-GH 2 -n-G'joF2i > HO-CH 2 -CH2-n-Ci2F25 for example in US 2,642,416, US 3,239,557, BR 1,118,007, US 3,462,296.
  • R 1 is hydrogen, CH 3 , C 2 H 5 , R CH 3 , C 2 H 5 , x is an integer in the range from 4 to 12, very particularly preferably 6 to 8 y is an integer Number in the range from 1 to 11, preferably 1 to 6,
  • Suitable copolymers are copolymers of (meth) acrylic acid esters fluorinated or perfluorinated C 3 -C 12 alkyl alcohols such as HO-CH 2 -CH 2 -CF 3 , HO-CH 2 -CH 2 -C 2 F 5 , HO-CH 2 -CH 2 -nC 3 F 7 , HO-CH 2 -CH 2 -iso-C 3 F 7 , HO-CH 2 -CH 2 -nC 4 F 9 , HO-CHs-CHz-n-CsFn, HO-CH 2 -CH 2 -nC 6 F 13 , HO-CH 2 -CH 2 -nC 7 F 15 ; with (meth) acrylic acid esters non-halogenated CrC 20 alcohols, for example methyl (meth) acrylate, ethyl (meth) acryl
  • olefins with siloxane groups are, for example, olefins of the general formulas II a to II c
  • R 3 is selected from d-Ci ⁇ -alkyl, for example methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, sec-butyl, tert.
  • n-pentyl iso-pentyl, sec.-pentyl, neo-pentyl, 1,2-dimethylpropyl, iso-amyl, n-hexyl, iso-hexyl, sec.-hexyl, n-heptyl, iso-heptyl , n-octyl, n-nonyl, n-decyl, n-dodecyl, n-tetradecyl, n-hexadecyl, n-octadecyl; preferably CC 6 alkyl such as methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, sec-butyl, tert-butyl, n-pentyl, isopentyl, sec-pentyl, neo -Pent
  • C e -C 14 aryl for example phenyl, 1-naphthyl, 2-naphthyl, 1-anthryl, 2-anthryl, 9-anthryl, 1-phenanthryl, 2-phenanthryl, 3-phenanthryl, 4-phenanthryl and 9 -Phenanthryl, preferably phenyl, 1-naphthyl and 2-naphthyl, particularly preferably phenyl C 3 -C 12 cycloalkyl, for example cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, cyclononyl, cyclodecyl, cycloundecyl and cyclododecyl; cyclopentyl, cyclohexyl and cycloheptyl or Si (CH 3 ) 3 are preferred.
  • R 1 is defined as above.
  • n is an integer in the range from 0 to 6, in particular 1 to 2;
  • m is an integer in the range from 2 to 10,000, in particular up to 100.
  • Suitable polymers are also: polyethers such as polyethylene glycol, polypropylene glycol, polybutylene glycols, polytetrahydrofuran; Polycaprolactone, polycarbonates, polyvinylbutyrai, partially aromatic polyesters from aliphatic or aromatic dicarboxylic acids and / or aliphatic or aromatic dialcohols, e.g.
  • Polyester composed of aliphatic dialcohols with 2 to 18 carbon atoms such as, for example, ethylene glycol, propanediol, 1,4-butanediol, 1,6-hexanediol, 1,8-octanediol or bisphenol A, and aliphatic dicarboxylic acids with 3 to 18 carbon atoms such as succinic acid, glutaric acid, adipic acid and ⁇ , ⁇ -decanedicarboxylic acid; Polyester composed of terephthalic acid and aliphatic dialcohols with 2 to 18 carbon atoms, such as ethylene glycol, propanediol, 1, 4-butanediol, 1,6-hexanediol or 1,8-octanediol.
  • aliphatic dialcohols with 2 to 18 carbon atoms such as, for example, ethylene glycol, propanediol, 1,4-butanediol, 1,6-he
  • polyesters can, for example, be terminated with monoalcohols such as 4 to 12 carbon atoms, for example n-butanol, n-hexanol, n-octanol, n-decanol or n-dodecanol.
  • monoalcohols such as 4 to 12 carbon atoms, for example n-butanol, n-hexanol, n-octanol, n-decanol or n-dodecanol.
  • polyesters mentioned above can be terminated, for example, with monocarboxylic acids, such as, for example, stearic acid.
  • Suitable polymers are melamine-formaldehyde resins, urea-formaldehyde resins, N, N-dimethylol-4,5-dihydroxyethyleneureas, which can be etherified with CrC 5 alcohols.
  • the molecular weight of the organic polymer or polymers can be selected in a wide range.
  • the molecular weight can be in the range from 1000 to 10,000,000 g / mol, preferably in the range from 2500 to 5,000,000 g / mol, determined by at least one of the following methods: light scattering, gel permeation chromatography (GPG), viscometry , If a polymer from the group of polyolefins is used, for example polyethylene, polypropylene or polyisobutene and copolymers of ethylene with propylene, butylene or 1-hexene, the molecular weight is advantageously in the range from 30,000 to 5,000,000 g / mol.
  • the breadth of the molecular weight distribution is not critical per se and can be in the range from 1.1 to 20. It is usually in the range from 2 to 10.
  • the proportion of the organic polymer or polymers described above can be at least 0.1 g / l of the liquor, preferably at least 1 g / l and particularly preferably at least 10 g / l.
  • the maximum proportion is, for example, 500 g / l, preferably 250 g / l and particularly preferably 100 g / l.
  • the organic polymer (s) is not soluble in the liquor, wherein insoluble in connection with organic polymers in the sense of the present invention means that less than 1 g / l are soluble in the liquor at room temperature, preferably less than 0.1 g / l.
  • At least two different organic polymers are used.
  • At least one organic polymer can be in the form of particles with an average grain diameter of 0.1 to 50 ⁇ m, preferably 0.5 to 30 ⁇ m and particularly preferably up to 20 ⁇ m (median value, number average).
  • At least one of the aqueous liquors used in the process according to the invention contains at least one hydrophobic solid in particulate form, which is different from the polymer or polymers described above, in a proportion of at least 5.5 g / l, preferably at least 7 g / l , particularly preferably at least 10 g / l. If it is desired to use a mixture of at least two hydrophobic solids in particulate form, at least one is preferably present in a proportion of at least 5.5 g / l.
  • the maximum proportion of the hydrophobic solids in particulate form can be a total of 150 g / l.
  • the hydrophobic solid in particulate rer form can be inorganic or organic in nature, it is preferably inorganic.
  • suitable materials are polyethylene, polypropylene, polyisobutylene and polystyrene and copolymers thereof with one another or with one or more further olefins such as, for example, styrene, methyl acrylate, ethyl acrylate, methyl methacrylate, butyl acrylate, butyl methacrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate or maleic anhydride -Methylmaleinimid.
  • a preferred polyethylene or polypropylene is described for example in EP-A 0761 696.
  • Particularly suitable materials are inorganic materials, in particular solid inorganic oxides, carbonates, phosphates, silicates or sulfates from groups 3 to 14 of the Periodic Table of the Elements, for example calcium oxide, silicon dioxide or aluminum oxide, calcium carbonate, calcium sulfate or calcium silicate, aluminum oxide and silicon dioxide being preferred , Silicon dioxide in its modification as silica gel is particularly preferred. Fumed silica gels are very particularly preferred.
  • Solid inorganic oxides can be thermally hydrophobicized by heating to 400 to 800 ° C or preferably by physisorbed or chemisorbed organic or organometallic compounds.
  • particles are reacted before the coating step, for example with organometallic compounds which contain at least one functional group, for example alkyl-lithium compounds such as methyl lithium, n-butyl lithium or n-hexyl lithium; or silanes such as hexamethyldisilazane, octyltrimethoxysilane and in particular halogenated silanes such as trimethylchlorosilane or dichlorodimethylsilane.
  • organometallic compounds which contain at least one functional group, for example alkyl-lithium compounds such as methyl lithium, n-butyl lithium or n-hexyl lithium; or silanes such as hexamethyldisilazane, octyltrimethoxysilane and in particular halogenated silanes such as trimethylchlorosilane or dichlorodimethylsilane.
  • hydrophobic In connection with the hydrophobic solid or particles in particulate form, hydrophobic is understood to mean that its solubility is below 1 g / l, preferably below 0.3 g / l, determined at room temperature.
  • Inorganic solids can preferably be porous in nature.
  • the porous structure can best be characterized by the BET surface area, measured according to DIN 66131.
  • Inorganic solids used can preferably have a BET surface area in the range from 5 to 1000 m / g, preferably from 10 to 800 m 2 / g and particularly preferably from 20 to 500 m 2 / g.
  • At least one of the hydrophobic solids is in particulate form.
  • the average particle diameter (median, number average) is at least 1 nm, preferably at least 3 n and particularly preferably at least 6 nm.
  • the maximum particle diameter (median, number average) is 350 nm, preferably 100 nm. You can use common methods such as transmission electron microscopy.
  • the weight ratio of organic polymer to organic or inorganic solid in particulate form is generally 9: 1 to 1: 9, preferably 4: 1 to 1.4 and particularly preferably 7: 3 to 4: 6.
  • At least one of the hydrophobic solids is in the form of spherical particles, which should include those particulate solids, of which at least 75% by weight, preferably at least 90% by weight in spherical form and further particles in granular form.
  • At least one of the hydrophobic solids can form agglomerates. If one or more hydrophobic solids are present in the form of agglomerates, which can consist of 2 to several thousand primary particles and which in turn can have a spherical shape, the information relating to the shape and size of the particles relates to the primary particles.
  • At least one liquor used in the process according to the invention can contain at least one surface-active agent, selected for example from the group of ionic and nonionic emulsifiers.
  • Suitable nonionic emulsifiers are, for example, ethoxylated mono-, di- and tri-alkylphenols (degree of ethoxylation: 3 to 50, alkyl radical: C 4 -C 12 ) and ethoxylated fatty alcohols (degree of ethoxylation: 3 to 80; alkyl radical: C 8 -C) 36 ).
  • ethoxylated mono-, di- and tri-alkylphenols degree of ethoxylation: 3 to 50, alkyl radical: C 4 -C 12
  • ethoxylated fatty alcohols degree of ethoxylation: 3 to 80; alkyl radical: C 8 -C
  • Suitable anionic emulsifiers are, for example, alkali metal and ammonium salts of alkyl sulfates (alkyl radical: G 8 to C 12 ), of sulfuric acid semiesters of ethoxylated alkanols (degree of ethoxylation: 4 to 30, alkyl radical: C 2 -C 18 ) and ethoxylated alkylphenols (ethoxylation Grade: 3 to 50, alkyl radical: C 4 -C 12 ), of alkyl sulfonic acids (alkyl radical: Ci2-C 18 ) and of alkylarylsulfonic acids (alkyl radical: C 9 -C 18 ).
  • Suitable cationic emulsifiers are usually a C 6 -C 1 ⁇ alkyl, aralkyl or heterocyciischen containing primary, secondary, tertiary or quaternary ammonium salts, alkanolammonium salts, pyridinium salts, imidazolinium salts, oxazolinium salts, morpholinium salts, thiazolinium salts and also salts of amine oxides, quinolinium , Isoquinolinium salts, tropylium salts, sulfonium salts and phosphonium salts.
  • Examples include dodecylammonium acetate or the speaking hydrochloride, the chlorides or acetates of the various 2- (N, N, N-trimethylammonium) ethyl paraffinates, ⁇ / -cetylpyridinium chloride, N-lauryl-pyridinium sulfate and ⁇ / -cetyl- ⁇ /, ⁇ /, ⁇ / -trimethylammonium bromide, ⁇ -Dodecyl- ⁇ /, ⁇ /, ⁇ / - trimethylammonium bromide, ⁇ /, ⁇ / -distearyl- ⁇ /, ⁇ -dimethylammonium chloride and the gemini surfactant W, W- (lau ⁇ yldimethyl) ethylenediamine dibromide.
  • Very particularly suitable emulsifiers are, for example, copolymers of ethylene and at least one ⁇ , £ -unsaturated mono- or dicarboxylic acid or at least one anhydride of a ⁇ -unsaturated mono- or dicarboxylic acid, for example acrylic acid, methacrylic acid, crotonic acid, maleic acid, fumaric acid, methylene malonic acid, maleic anhydride, itaconic acid anhydride ,
  • the carboxyl groups can be partially or preferably completely neutralized, for example with alkali metal ions, alkaline earth metal ions, ammonium or amines, for example amines such as triethylamine, diethylamine, ethylamine, trimethylamine, dimethylamine, methylamine, ethyldiisopropyfamine, ethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine , N- (n-butyl) diethanolamine or N, N
  • the proportion of emulsifier in the liquor can be selected within wide limits and can be 0.1 to 100 g / l, preferably 0.2 to 10 g / l.
  • the process according to the invention is carried out by treating textile material with at least one aqueous liquor. It is also possible to carry out several treatment steps with the same or different liquors.
  • the process according to the invention is carried out by first treating the textile to be treated with a liquor which contains at least one organic polymer and furthermore an organic or preferably inorganic solid in particulate form and then a further treatment with a new liquor, which contains the organic polymer, but no further organic or inorganic solid in particulate form.
  • the process according to the invention is carried out by first treating the textile to be treated with a liquor which contains at least one organic polymer and furthermore an organic or preferably inorganic solid in particulate form, and then a further one Treatment with a new fleet that uses a different organic ⁇ polymer contains, but no other organic or inorganic solid in particulate form.
  • the process according to the invention is carried out by first treating the textile to be treated with a liquor which contains at least one organic polymer and furthermore an organic or preferably inorganic solid in particulate form and then a further treatment with a new liquor, which contains no further polymer, but the particulate inorganic solid already used in the first step.
  • the temperature for carrying out the method according to the invention is not critical per se.
  • the liquor temperature can be in the range from 10 to 60 ° C., preferably 15 to 30 ° C.
  • the process parameters of the process according to the invention can be selected such that the process according to the invention usually results in a liquor absorption of 25% by weight to 85% by weight, preferably 40 to 70% by weight.
  • the method according to the invention can be carried out in conventional machines which are used for finishing textiles, for example foulards.
  • Foulards with vertical textile feed are preferred, which contain two pressed rollers as an essential element, through which the textile is guided.
  • the liquid is filled in above the rollers and wets the textile.
  • the textile is squeezed off by the pressure and a constant application is guaranteed.
  • the speed of the textile intake of the foulards is 1 to 40 m / min, preferably 1 to 30 m / min.
  • the treated textile can be dried by methods customary in the textile industry.
  • annealing can be carried out, continuously or discontinuously.
  • the duration of the tempering can be selected within wide limits. Usually one can anneal over a period of about 0 seconds to about 30 minutes, in particular 30 seconds to 5 minutes.
  • the mixture is heated to temperatures of up to 180 ° C., preferably up to 150 ° C.
  • a suitable method for tempering is, for example, hot air drying.
  • the textile material is provided with an adhesive layer before the treatment according to the invention.
  • a so-called primer can be used for this.
  • the application of a primer is preferred if you want to finish synthetic fibers.
  • one or more polymers can be applied to the textile material to be treated as an adhesive layer, wherein the polymer synthesis can also be carried out on the textile material.
  • Polymers which are particularly suitable are those which have crosslinked or crosslinkable groups, for example natural or synthetic polymers with free hydroxyl groups, carbonyl groups, primary or secondary amino groups or thiol groups.
  • suitable polymers are lignin, polysaccharides, polyvinyl alcohol and polyethylene imine.
  • Crosslinking can be achieved, for example, by subsequent reaction with, for example, isocyanates, dimethylolurea or N, N-dimethylol-4,5-dihydroxyethyleneurea (DMDHEU).
  • Other particularly preferred crosslinkers are melamine-formaldehyde resins, which can be etherified with methanol.
  • 0.01 to 1% by weight, preferably 0.1 to 0.5% by weight, of the textile is saponified by partial saponification with strong alkalis such as aqueous sodium hydroxide solution or potassium hydroxide solution.
  • Another object of the present invention are textile materials finished by the method according to the invention.
  • the finishing according to the invention provides the textiles according to the invention with one or more layers.
  • the textile materials according to the invention show particularly good dirt and water-repellent behavior.
  • textile materials according to the invention show very good mechanical strength.
  • the or the solids used are isotropically or largely isotropically distributed over the finishing layer, i.e. no concentration is found in the boundary layer between the equipment layer and the surrounding atmosphere.
  • the textiles according to the invention contain 0.5 to 50 g / m 2 layer, preferably 1 to 20 g / m 2 and particularly preferably 1.5 to 10 g / m 2 .
  • the present invention further relates to aqueous liquors for finishing textile materials, comprising at least one organic polymer and at least one organic or inorganic solid in particulate form, the organic or inorganic solids in the liquor being added in one batch. of at least 5.5 g / l.
  • the liquors according to the invention can contain further components, for example one or more organic solvents or one or more emulsifiers.
  • Another object of the present invention is the use of the fleets according to the invention for finishing textile materials.
  • Another object of the present invention is a process for the production of aqueous liquors, hereinafter also called the production process according to the invention.
  • the production process according to the invention comprises mixing the following components: at least one organic polymer, at least one organic or inorganic solid in particulate form,
  • the production process according to the invention can usually be carried out at temperatures from room temperature to about 100 ° C., room temperature being preferred.
  • the manufacturing method according to the invention generally comprises a homogenization step, for example by mechanical or pneumatic stirring, shaking, ultrasound treatment or a combination thereof. In some cases, however, the homogenization step can be omitted.
  • the order in which the components are added can be chosen as desired.
  • a water- and solvent-free mixture of polymer and organic or inorganic solid can first be prepared and then the dry mixture can be dispersed in organic solvent or a mixture of water and organic solvent or in water.
  • formulations are first prepared which contain organic polymer, organic or inorganic solid in particulate form, optionally one or more organic solvents and optionally one or more emulsifiers and optionally water. Before carrying out the treatment of textile len materials are then produced in a liquor according to the invention by diluting the formulation with water. It is preferred that the formulations according to the invention contain a maximum of 15% by weight, preferably about 0.1 to 10% by weight, particularly preferably up to 5% by weight, of water.
  • the formulations according to the invention can also be anhydrous.
  • the present invention further relates to formulations which contain organic polymer, organic or inorganic solid in particulate form, optionally one or more organic solvents and optionally one or more emulsifiers and optionally water, the proportion of water being about 0.1 to 10% by weight .-%, preferably up to 5 wt .-%.
  • Example 1.1 Production of the fleet 1.1
  • Example 1.2 Production of the fleet 1.2
  • Example 1.4 Production of the fleet 1.4
  • a polyester fabric with a basis weight of 220 g / m 2 was treated with liquor 1.1 on a foulard (manufacturer Mathis, type no. HVF12085). The contact pressure of the rollers was 2.6 bar. A fleet uptake of 60% resulted. The application speed was 2 m / min. The treated polyester fabric was then dried at 120 ° C. on a tenter. The final taring took place over a period of 3 min at 50 ° G in circulating air. The treated polyester fabric 2.1 was obtained.
  • a polyamide fabric with a basis weight of 160 g / m 2 was treated with liquor 1.1 on a foulard (manufacturer Mathis, type Mr. HVF12085). The contact pressure of the rollers was 2.6 bar. The result was a fleet uptake of 65%. The application speed was 2 m / min. The treated polyamide fabric was then dried at 120 ° C. on a tenter. The final tempering was carried out over a period of 3 min at 150 ° C. in circulating air. The treated polyamide fabric 2.2 was obtained.
  • a polyacrylic fabric with a basis weight of 295 g / m 2 was treated with liquor 1.1 on a foulard (manufacturer Mathis, type no. HVF12085). The contact pressure of the rollers was 2.6 bar. A fleet absorption of 50% resulted. The application speed was 2 m / min. The treated polyacrylic fabric was then dried at 120 ° C. on a tenter. The final tem was carried out over a period of 3 min at 150 ° C in circulating air. The treated polyacrylic fabric 2.3 was obtained.
  • a polyester fabric with a basis weight of 220 g / m 2 was treated with liquor 1.2 on a pad (manufacturer Mathis, type no. HVF12085). The contact pressure of the rollers was 2.6 bar. A fleet uptake of 60% resulted. The application speed was 2 m / min. The treated polyester fabric was then dried at 120 ° C on a tenter. The final tempering was carried out over a period of 3 minutes at 150 ° C. under circulating air. The treated polyester fabric 2.4 was obtained.
  • a polyamide fabric with a basis weight of 160 g / m 2 was treated with liquor 1.2 on a padder (manufacturer Mathis, type no. HVF12085). The contact pressure of the rollers was 2.6 bar. The result was a fleet uptake of 65%. The application speed was 2 m / min. The treated polyamide fabric was then dried at 120 ° C. on a tenter. The final tempering was carried out over a period of 3 minutes at 150 ° C. under circulating air. The treated polyamide fabric 2.5 was obtained.
  • a polyacrylic fabric with a basis weight of 295 g / m 2 was treated with liquor 1.2 on a padder (manufacturer Mathis, type no. HVF12085). The contact pressure of the rollers was 2.6 bar. A fleet absorption of 50% resulted. The application speed was 2 m / min. The treated polyacrylic fabric was then dried at 120 ° C. on a tenter. The final tempering was carried out over a period of 3 minutes at 150 ° C. under circulating air. The treated polyacrylic fabric 2.6 was obtained.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatment Of Fiber Materials (AREA)
EP04706158A 2003-02-18 2004-01-29 Procede d'impermeabilisation de matieres textiles Expired - Lifetime EP1597425B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10306893 2003-02-18
DE10306893A DE10306893A1 (de) 2003-02-18 2003-02-18 Verfahren zur Hydrophobierung von textilen Materialien
PCT/EP2004/000776 WO2004074568A1 (fr) 2003-02-18 2004-01-29 Procede d'impermeabilisation de matieres textiles

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EP1597425A1 true EP1597425A1 (fr) 2005-11-23
EP1597425B1 EP1597425B1 (fr) 2010-12-01

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EP (1) EP1597425B1 (fr)
JP (1) JP4531039B2 (fr)
AT (1) ATE490369T1 (fr)
DE (2) DE10306893A1 (fr)
ES (1) ES2356143T3 (fr)
WO (1) WO2004074568A1 (fr)

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JP4584308B2 (ja) * 2004-05-19 2010-11-17 ビーエーエスエフ ソシエタス・ヨーロピア 吸収材料を仕上げ処理する方法
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BRPI0807871A2 (pt) * 2007-03-30 2014-06-17 Basf Se Processo para a produção de um produto têxtil revestido, produtos têxteis, uso de produtos têxteis, toldo, capuz ou encerado, e, licor aquoso.
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CA2882179A1 (fr) 2012-08-23 2014-02-27 Gary S. Selwyn Procede de finissage chimique a l'aide d'un baton et appareil correspondant
US9790640B2 (en) 2014-02-24 2017-10-17 Gary S Selwyn Composition and process for applying hydrophobic coating to fibrous substrates
JP6789567B2 (ja) * 2016-05-16 2020-11-25 明成化学工業株式会社 繊維製品のはっ水処理用水系分散体及びその製造方法、はっ水加工方法及びはっ水性繊維製品
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DE502004011953D1 (de) 2011-01-13
US7955518B2 (en) 2011-06-07
WO2004074568A1 (fr) 2004-09-02
ES2356143T3 (es) 2011-04-05
US20100305256A1 (en) 2010-12-02
EP1597425B1 (fr) 2010-12-01
ATE490369T1 (de) 2010-12-15
JP4531039B2 (ja) 2010-08-25
US7790238B2 (en) 2010-09-07
US20060174418A1 (en) 2006-08-10
DE10306893A1 (de) 2004-08-26

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