EP2440621A1 - Procédé de production d'un tissu non tissé gonflant - Google Patents

Procédé de production d'un tissu non tissé gonflant

Info

Publication number
EP2440621A1
EP2440621A1 EP10722358A EP10722358A EP2440621A1 EP 2440621 A1 EP2440621 A1 EP 2440621A1 EP 10722358 A EP10722358 A EP 10722358A EP 10722358 A EP10722358 A EP 10722358A EP 2440621 A1 EP2440621 A1 EP 2440621A1
Authority
EP
European Patent Office
Prior art keywords
water
polymer
acid
weight
nonwoven fabric
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.)
Withdrawn
Application number
EP10722358A
Other languages
German (de)
English (en)
Inventor
Bolette Urtel
Christian Krüger
Klaus-Peter Neugebauer
Klaus Haas
Ralf Mossbach
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Priority to EP10722358A priority Critical patent/EP2440621A1/fr
Publication of EP2440621A1 publication Critical patent/EP2440621A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H13/00—Other non-woven fabrics
    • 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
    • D06M15/327—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
    • 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
    • D06M15/347—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated ethers, acetals, hemiacetals, ketones or aldehydes
    • 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
    • D06M15/53—Polyethers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]

Definitions

  • the present invention is a process for producing a nonwoven web by contacting a nonwoven fabric with a water-in-water dispersion of a polymer P, by free-radically initiated polymerization of at least one ethylenically unsaturated monomer MON in the presence of at least one water-soluble polymer A and B polymers in an aqueous medium, wherein the at least one water-soluble polymer A is selected from
  • DE-A 10 2004 058 271 discloses the use of the polymers P as auxiliaries in the production of textile auxiliaries, such as printing pastes, dyeing liquors, coating compositions or equipment liquors.
  • nonwoven webs as waterproofing membranes, for example, for road, tunnel and hydraulic engineering as well as for excavations, flood protection and roof waterproofing, using water-in-water dispersions of Polymers P disclosed.
  • the source nonwovens disclosed in DE-A 10 2004 063 004 are not always fully satisfactory in view of the elution loss of the polymer P from the nonwoven webs.
  • the object of the present invention was to reduce the washout losses of the swelling meadow produced by means of a water-in-water dispersion of a polymer P.
  • the object has been achieved by the source nonwovens produced by the method defined above.
  • Non-woven fabrics are familiar to the expert. Within the scope of this document, this is intended to mean, for example, nonwovens, knitted fabrics, woven or knitted fabrics or combinations thereof.
  • a nonwoven is usually understood to mean a nonwoven and nonwoven fabric which may contain fibers or ribbons.
  • Knitted fabrics are textile structures that are created by forming intertwined meshes that hold each other. Fabrics are textile structures made of perpendicular crossing yarns or tapes, which are produced for example on looms.
  • fiber webs nonwovens, such as, for example, spunbonded nonwovens, needled nonwovens or nonwoven spunbonded with water jet.
  • the solidification of the nonwovens can be carried out mechanically, thermally or chemically in a manner familiar to the person skilled in the art.
  • the fibrous webs which can be used according to the invention are preferably planar structures of any desired thickness, more preferably the thickness of the planar structures is 1 to 300 mm, in particular 1 to 20 mm or 1 to 10 mm.
  • the fiber webs that can be used according to the invention may consist of tapes or of fibers, the latter being preferably used.
  • Suitable tapes are, for example, tapes, in particular those made of textile materials or film tapes of conventional film materials, such as plastics, such as polyethylene and / or polypropylene.
  • fibers staple fibers or filaments (filaments) can be used.
  • the fibers may be, for example, synthetic, mineral or natural, in particular synthetic and / or mineral fibers being used.
  • Examples of synthetic fibers are fibers of polyolefin, such as polyethylene or polypropylene, polyesters, such as polyethylene terephthalate or polybutylene terephthalate, polyamide, polysulfone and / or polyether ketone.
  • Mineral fibers may for example consist of ceramic materials, silicon carbide and / or boron nitride. It is also possible to use fibers made of carbon or glass fibers.
  • polyolefins such as polyethylene, polypropylene, polyesters, such as polyethylene terephthalate, polybutylene terephthalate, polyamides, polysulfones and / or polyether ketones, but especially polyolefins and polyesters.
  • Water-in-water dispersions of the polymer P and the preparation of these dispersions are those skilled in the WO 2005/12378, page 2, line 38 to page 9, line 23 and DE-A 10 2004 063 004, sections [0045] to [0092] known. Both documents are to be expressly referred to in the context of this document and the preparation of the aforementioned water-in-water dispersions are intended to form a part of this document.
  • the water-in-water dispersions of the polymer P are prepared by free-radically induced polymerization of at least one ethylenically unsaturated monomer MON in the presence of at least one water-soluble polymer A and polymer B in an aqueous medium, wherein the at least one water-soluble polymer A is selected from
  • Suitable ethylenically unsaturated monomers MON are preferably water-soluble nitrogen-containing ethylenically unsaturated monomers or water-soluble anionic ethylenically unsaturated monomers.
  • solubility in 100 g of deionized water at 20 0 C and atomic mosphDC Kunststoff (1 atm 1, 013 bar absolute)> 10 g, preferably> 30 g and particularly advantageously> 50 g.
  • Suitable water-soluble nitrogen-containing ethylenically unsaturated monomers are preferably N-vinylformamide, N-vinylacetamide, N-vinylimidazole and N-vinylpyrrolidone or mixtures of at least two of the abovementioned monomers.
  • Suitable water-soluble anionic ethylenically unsaturated monomers are preferably monoethylenically unsaturated C3- to C6-carboxylic acids, for example monoethylenically unsaturated C3- to C6-mono- and dicarboxylic acids, such as acrylic acid, methacrylic acid, ethacrylic acid, crotonic acid, itaconic acid, maleic acid or fumaric acid, and ethylenically unsaturated Sulfonic acids, in particular vinylsulfonic acid, styrenesulfonic acid, in particular para-styrenesulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, and
  • the above-mentioned water-soluble anionic ethylenically unsaturated monomers can be used in each case as the free acid or in the form of their alkali metal or ammonium salts.
  • Preferred water-soluble anionic ethylenically unsaturated monomers used as main monomers include acrylic acid, methacrylic acid, maleic acid, 2-acrylamido-2-methylpropanesulfonic acid and / or vinylsulfonic acid, with acrylic acid being particularly preferred.
  • Water-soluble anionic ethylenically unsaturated monomers can be polymerized to give homopolymers or else mixed with one another or with other comonomers to give copolymers. Examples are the homopolymers of acrylic acid or copolymers of acrylic acid with methacrylic acid and / or maleic acid.
  • Suitable comonomers are, in principle, ethylenically unsaturated comonomers, which may be nonionic or may carry a positive charge, ie are cationic.
  • suitable nonionic or cationic comonomers are (meth) acrylamide, acrylic esters of C 1 -C 4 -alkanols, for example methyl acrylate, ethyl acrylate, n-propyl acrylate, isopropyl acrylate, n-butyl acrylate, acrylic acid iso butyl ester, acrylic acid sec-butyl ester, tert-butyl acrylate, methacrylic acid esters of methanol or ethanol, vinyl acetate, vinyl propionate, mono- or diallyldi- (C 1 -C 4 -alkyl) ammonium salts, especially halides of the formula
  • X is selected from, for example, fluoride, bromide, iodide and in particular chloride, 2- [N, N-di- (C 1 -C 4 -alkyl) amino] ethyl (meth) acrylates, 3- [N 1 N-di- (C 1 -C 4 -alkyl) aminopropyl (meth) acrylates, where C 1 -C 4 -alkyl can each be different or preferably identical and selected from ethyl, n-propyl, isopropyl, n-butyl, isobutyl and preferably methyl, very particularly preferably 2- (N 1 N-dimethylamino) ethyl (meth) acrylate and 3- (N, N-dimethyl) aminopropyl (meth) acrylate.
  • Basic comonomers such as 2- [N, N-di- (C 1 -C 4 -alkyl) amino] ethyl (meth) acrylates and 3- [N, N-di- (C 1 -C 4 -alkyl) aminopropyl (meth) acrylates can both be used in the form of the free bases as well as in partially or fully buffered form in the copolymerization.
  • Nonionic and / or cationic comonomers can be added in the preparation of the polymers P according to the invention preferably in amounts such that the resulting polymers are water-soluble and have overall anionic charge, which may be stabilized, for example, by alkali metal cations or ammonium cations which may be substituted can.
  • the amount of nonionic and / or cationic comonomers may be e.g. 0 to 99, or 0 to 45 wt .-% amount.
  • Preferred polymers are, for example, those which contain 55 to 100% by weight of acrylic acid and / or methacrylic acid in copolymerized form.
  • crosslinked polymers P are used which have been prepared using a so-called ethylenically unsaturated crosslinker.
  • Crosslinked polymers can be prepared by additionally carrying out the polymerization in the presence of at least one ethylenically unsaturated crosslinker. This gives polymers having a higher molecular weight than in the polymerization of at least one ethylenically unsaturated monomer MON in the absence of such a crosslinking agent. Correspondingly prepared crosslinked polymers have a high water absorption capacity.
  • Crosslinkers which can be used are all compounds which have at least two ethylenically unsaturated double bonds in the molecule. Such compounds are familiar to the person skilled in the art and are used, for example, in the preparation of crosslinked polyacrylic acids, such as superabsorbent polymers (cf EP-A 858 478).
  • crosslinkers examples include: triallylamine, pentaerythritol triallether, methylenebis (meth) acrylamide, N, N'-divinylethyleneurea, di- or polyhydric alcohols having 2 to 4 C atoms completely esterified with acrylic acid or methacrylic acid, such as ethylene glycol di (meth) acrylate, 1 , 4-Butandioldi (meth) acrylate, di (meth) acrylates of polyethylene glycols having molecular weights M n of, for example, 300 to 600 g / mol, compounds of general formula I.
  • R 1 is the same or different and selected from methyl and hydrogen; m is an integer from 0 to 2, preferably 1;
  • R 2 selected from Ci-C 4 -AlkVl, such as nC 4 Hg, n-CsH 7 , iso-C3H 7 and preferably C 2 H 5 and CH 3, or phenyl, A 2 , A 3 , A 4 are identical or different and chosen out
  • C 1 -C 20 -alkylene such as, for example, -CH 2 -, -CH (CH 3 ) -, -CH (C 2 H 5 ) -, --CH (C 6 H 5 ) -,
  • Ci-C 2 o-alkylene in which from one to seven, respectively, not adjacent
  • C atoms are replaced by oxygen, such as -CH 2 -O-CH 2 -, -CH 2 -CH 2 -O, - (CH 2 J 2 -O-CH 2 -, - (CH 2 J 2 -O - (CH 2 J 2 -, - [(CH 2 J 2 -O] 2 - (CH 2 J 2 -, - [(CH 2 J 2 -O) 3 - (CH 2 J 2 -;
  • crosslinker in the preparation of polymers P of at least one ethylenically unsaturated monomer MON, the amounts of crosslinker used in each case are, for example, 0.001 to 5.0% by weight, preferably 0.01 to 1.0% by weight %, based on the total amount of ethylenically unsaturated monomers MON used in the polymerization.
  • polymerization initiators which are familiar to the person skilled in the art and which form radicals under the reaction conditions are used.
  • Suitable polymerization initiators are, for example, peroxides, hydroperoxides, hydrogen peroxide, persulfates, such as, for example, sodium, potassium or ammonium persulfate, redox catalysts and azo compounds, such as 2,2'-azobis (N, N-dimethyleneisobutyramidines) dihydrochloride, 2,2'-azobis (4- methoxy-2,4-dimethylvaleronitrile), 2,2'-azobis (2,4-dimethylvaleronitrile) and 2,2'-azobis (2-amidinopropane) dihydrochloride).
  • Polymerization initiators are used in quantities customary in emulsion polymerizations (from 0.1 to 5% by weight, based on the sum of the ethylenically unsaturated monomers MON used for the polymerization).
  • azo initiators or persulfates are used as polymerization initiators.
  • the free-radical polymerization reaction can also be initiated with the aid of energy-rich radiation such as electron beams or by irradiation with UV light.
  • the water-in-water dispersions of the polymers P used according to the invention have a polymer concentration of, for example, 1 to 70, preferably 5 to 50 and in particular 15 to 25,% by weight, based in each case on the sum of the total amounts of monomers MON, polymers A and polymers B.
  • the polymer concentration can also be referred to as solids content.
  • Water-in-water dispersions of the polymers P used according to the invention are prepared by free-radically initiated polymerisation of at least one ethylenically unsaturated monomer MON in the presence of at least one water-soluble polymer A and polymer B, wherein the at least one water-soluble polymer A is selected
  • Water-in-water dispersions of polymers P used according to the invention can also be prepared in the presence of at least two different of the abovementioned water-soluble polymers A and B.
  • the water-in-water dispersions of the polymers P obtained after the polymerization reaction have, for example at a pH of 4, a dynamic viscosity in the range of 100 to 12,000 mPas, preferably 150 to 6,000 mPas (measured in a Brookfield viscometer at 23 0 C).
  • Water-soluble polymers A of group (a1) are graft polymers of vinyl propionate or of mixtures of vinyl propionate and vinyl acetate, preferably of vinyl acetate on polyalkylene glycol, preferably polyethylene glycol or polyalkylene glycol substituted on one or both sides with alkyl, carboxyl or amino groups, preferably polyethylene glycol consideration.
  • Polyalkylene glycols suitable as a graft base are described, for example, in WO 03/046024, page 4, line 37 to page 8, line 9.
  • 10 to 10,000, preferably 30 to 300 parts by weight of vinyl propionate, mixture of vinyl propionate and vinyl acetate or preferably vinyl acetate are grafted onto 100 parts by weight of the grafting base.
  • Very particular preference is given to using polyethylene glycol having a molar mass average molecular weight M n of from 1000 to 100 000 g / mol as the grafting base.
  • Suitable water-soluble polymers A of group (a2) are copolymers of alkylpolyalkylene glycol (meth) acrylates and (meth) acrylic acid, preferred are copolymers of alkylpolyalkylene glycol acrylates and (meth) acrylic acid.
  • Such compounds are known, for example, as dispersants for cement. They are made, by first esterifying addition products of ethylene oxide and / or propylene oxide onto, for example, C 1 - to C 6 -alkoxy alcohols with acrylic acid and / or methacrylic acid and then copolymerizing the resulting esters with acrylic acid and / or methacrylic acid.
  • water-soluble polymers of group (a2) contain, for example, from 5 to 60, preferably from 10 to 35,% of copolymerized units of alkylpolyalkylene glycol (meth) acrylates and from 95 to 40, preferably from 90 to 65,% of copolymerized units of (meth) acrylic acid. They usually have a number-average molecular weight M n in the range from 2,000 to 50,000, preferably 5,000 to 20,000 g / mol.
  • Water-soluble polymers of group (a2) can be used in the form of the polyacids or else in completely or partially neutralized form in the preparation of aqueous dispersions used according to the invention.
  • Carboxylic groups of the water-soluble polymers of group (a2) can preferably be neutralized with sodium hydroxide solution, potassium hydroxide solution or ammonia.
  • Suitable water-soluble polymers A of group (a3) are polyalkylene glycols, preferably polyethylene glycols.
  • polyalkylene glycols and in particular polyethylene glycols used as water-soluble polymers A of group (a3) can have a number average molecular weight M n in the range from 100 to 100,000, preferably from 300 to 80,000, more preferably from 600 to 50,000 and in particular from 1000 to 50,000 g / mol, wherein the molecular structure of polyalkylene glycols is defined above.
  • Preferred polyalkylene glycols (a3) are polyethylene glycol, polypropylene glycol and block copolymers of ethylene oxide and propylene oxide.
  • the block copolymers may contain in copolymerized form ethylene oxide and propylene oxide in any desired amounts and in any desired order and have two or more blocks.
  • Suitable water-soluble polymers A of group (a4) are polyalkylene glycols substituted on one or both sides with alkyl, carboxyl or amino groups and in particular polyethylene glycols, for example having number-average molecular weights M n in the range from 100 to 100,000, preferably from 300 to 80,000, more preferably from 600 to 50,000 and in particular from 1000 to 50,000 g / mol.
  • Preferred water-soluble polymers A of group (a4) are polyethylene glycols, polypropylene glycols and block copolymers of ethylene oxide and propylene oxide which are substituted on one or both sides with alkyl copolymers containing ethylene oxide and propylene oxide in copolymerized form in any desired amounts and in any order may have two or more blocks.
  • Suitable alkyl groups are C 1 -C 20 -alkyl, in particular unbranched C 1 -C 20 -alkyl.
  • Suitable carboxyl groups are, for example, pivalate and propionate and in particular acetate, furthermore benzoate.
  • Amino groups may be selected from NH 2, and mono- and di-C 1 -C 4 -alkylamino groups and cyclic amino groups such as
  • Aqueous polymer systems used according to the invention comprise at least one water-soluble polymer A of the groups (a1), (a2), (a3) or (a4), for example in amounts of 2 to 15, preferably 5 to 12,% by weight, based on the resulting aqueous polymer system ,
  • the water-soluble polymers B of group (b1) are preferably used partially or quantitatively hydrolyzed copolymers of vinyl alkyl ethers, such as vinyl-Ci-C4-alkyl ethers, and maleic anhydride.
  • C 1 -C 4 -alkyl is selected from methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl and preferably methyl or ethyl.
  • Water-soluble polymers B of group (b1) are obtainable by copolymerizing vinyl alkyl ethers with maleic anhydride and subsequent partial or quantitative hydrolysis of the anhydride groups to carboxyl groups and optionally partial or complete neutralization of the carboxyl groups.
  • Particularly preferred water-soluble polymers B of group (b1) are hydrolyzed copolymers of vinyl methyl ether and maleic anhydride as free polyacid and in the form of at least partially neutralized with sodium hydroxide, potassium hydroxide or ammonia salts.
  • Suitable water-soluble polymers B of group (b2) are starch, modified starch, preferably cationic or anionic modified.
  • modified starches are cationically modified potato starch, anionically modified potato starch, minced potato starch and maltodextrin.
  • cationically modified potato starches are the commercial products Amylofax 15 and Perlbond 970.
  • a suitable anionically modified potato starch is Perfectamyl A 4692. Here the modification consists essentially in a carboxylation of potato starch, for example benzoate, pivalate and in particular acetate.
  • C * Pur 1906 is an example of an enzymatically degraded potato starch and maltodextrin C 01915 for a hydrolytically degraded potato starch.
  • water-soluble polymers B are synthetic, preferably random copolymers (b3) obtainable by copolymerization of
  • ( ⁇ 1) at least one monomer selected from (meth) acrylamide, N-vinylformamide, N-vinylpyrrolidone and N-vinylcaprolactam, very particularly preferred are acrylamide and N-vinylpyrrolidone, and
  • one or more cationic monoethylenically unsaturated monomers selected from di-C 1 -C 4 -alkylamino-C 2 -C 4 -alkyl (meth) acrylate, for example 2- (N 1 N-dimethylamino) ethyl (meth) acrylate, 3 dimethylamino) propyl (meth) acrylate, 2- (N 1 N-diethylamino) ethyl (meth) acrylate, 3-diethylamino) propyl (meth) acrylate, each partially or quantitatively neutralized, for example, with hydrogen halide acids such as hydrochloric acid, with sulfuric acid, para-toluenesulfonic acid, formic acid or acetic acid, or quaternized partially or quantitatively with Ci-C 4 -AlkVl or benzyl, for example by reaction with Ci-C4-alkyl halide such as C1-C4 Alkyl bromine
  • anionic monoethylenically unsaturated monomers selected from (meth) acrylic acid, vinylsulfonic acid, vinylphosphonic acid, maleic acid, fumaric acid, itaconic acid, crotonic acid, in each case as free acid or as alkali metal or ammonium salt, where the molar Proportion of in (b3) polymerized cationic monoethylenically unsaturated monomers (ß2) is higher than the proportion of copolymerized anionic monoethylenically unsaturated monomers (ß3).
  • Polymers B of group (b3) can have a K value in the range from 15 to 200, preferably 30 to 150 and particularly preferably in the range from 45 to 110, determined according to H. Fikentscher (Cellulose-Chemie, Volume 13, pages 58 to 64 and 71 to 74, 1932) in 3 wt .-% aqueous NaCl solution at 25 0 C, a pH of 7 and a polymer concentration of 0.1 wt .-%.
  • synthetic preferably random polymers B of group (b3) are composed of
  • From 2 to 90 preferably from 20 to 80 and more preferably from 30 to 70 mol% of at least one monomer ( ⁇ 1), and
  • synthetic preferably random polymers B of group (b3) are composed of
  • the solubility of comonomers ( ⁇ 1) in water at 25 0 C is at least 100 g / l, most preferably they are miscible with water in any ratio.
  • Suitable examples of polymers B of the group (b3) are those prepared by copolymerizing acrylamide and 2- (N, N-dimethylamino) ethyl acrylate methochloride, acrylamide and 2- (N, N-dimethylamino) ethyl methacrylate metrochloride, methacrylamide and 2- (N, N-dimethylamino) ethyl acrylate methochloride, methacrylamide, and 2- (N, N-dimethylamino) ethyl methacrylate methochloride, acrylamide, 2- (N 1 N-dimethylamino) ethyl acrylate methochloride and acrylic acid, acrylamide, 2- (N 1 N-dimethylamino) ethyl methacrylate methochloride and acrylic acid.
  • a particularly suitable water-soluble polymer B of group (b2) is enzymatically degraded starch, in particular maltodextrin.
  • the total amount of the water-soluble polymers B is 1 to 100% by weight, preferably 2 to 80% by weight, and particularly preferably 10 to 50% by weight, based on the total amount Monomers MON.
  • the ratio of the total amounts of water-soluble polymers A and water-soluble polymers B in the water-in-water dispersions used according to the invention is generally from 1:10 to 10: 1, preferably from 1: 5 to 5: 1 and particularly preferably from 1: 2 to 2: 1.
  • Aqueous water-in-water dispersions used according to the invention preferably contain a combination of
  • (b1) at least one hydrolyzed copolymer of vinyl methyl ether and maleic anhydride as polyacid or in at least partially neutralized form with sodium hydroxide, potassium hydroxide or ammonia.
  • the water-in-water dispersion of the polymer P which can be used according to the invention, it has a content of inorganic salts in the range from 0.001 to 15% by weight, preferably 0.1 to 5% by weight, based on the total amount of the polymer P (corresponding to the sum of the total amounts of monomers MON, polymers A and polymers B).
  • a content of inorganic salts in the range from 0.001 to 15% by weight, preferably 0.1 to 5% by weight, based on the total amount of the polymer P (corresponding to the sum of the total amounts of monomers MON, polymers A and polymers B).
  • from 1 to 300 parts by weight, preferably from 10 to 200 parts by weight, and more preferably from 50 to 150 parts by weight, of polymer P, based on 100 parts by weight non-woven fabric are used.
  • Essential for the process according to the invention is that at least one organic compound V which has at least two functional groups selected from the group comprising hydroxyl, epoxy, primary and secondary amino groups, the water-in-water dispersion of the polymer P in advance and / or admixed with the nonwoven fabric during contacting and / or applied to the impregnated nonwoven fabric after contacting and prior to the drying step.
  • any organic compound which has at least two functional groups selected from the group comprising hydroxyl, epoxy, primary and secondary amino groups can be used as compound V.
  • the average molecular weight of the compound V can be> 1000 g / mol, but preference is given to organic compounds V which have an average molecular weight of ⁇ 1000 g / mol.
  • organic compounds V having an average molecular weight> 1000 g / mol are polyethylene glycols, polypropylene glycols, polytetramethylene diols, polyethylene glycol diglycidyl ethers, polypropylene glycol diglycidyl ethers, polyether amines, such as polyalkylene glycol diamines, for example polyethylene glycol diamine or polypropylene glycol diamine and polyethyleneimines.
  • organic compounds V which have an average molecular weight of ⁇ 1000 g / mol.
  • Suitable compounds V are in particular linear or cyclic di- or polyol compounds, alkanolamine compounds, di- or polyamine compounds, mono-, di- or polysaccharides as well as di- or polyepoxy compounds.
  • Preferred compounds according to the invention are those compounds V which are selected from the group comprising ethanolamine, diethanolamine, triethanolamine, 3-aminopropanol-1, 1-aminopropanol-2, 5-aminopentanol-1,2-2-aminoethoxy) ethanol, N- (2-aminoethyl) ethanolamine, BiS- (N-hydroxyethyl) -propanediamine-1,3-diisopropanolamine, triisopropanolamine, N-methyldiethanolamine, N-butyldiethanolamine, ethylene glycol, diethylene glycol, triethylene glycol, propanediol 1, 2, propanetriol 1, 2,3, butanediol-1, 2, butanediol-1, 4, butanediol-2,3, neopentyl glycol, trimethylolpropane, pentanediol-1, 2, pentanediol-1, 5, hexanedio
  • the organic compounds V are used in a total amount of 0.001 to 10 parts by weight, preferably 0.001 to 5 parts by weight and more preferably 0.01 to 2 parts by weight, based in each case on 100 parts by weight of polymer P, used.
  • At least one organic compound V in addition to the at least one organic compound V, additionally at least one phosphorus- or boron-containing inorganic compound B is admixed with the water-in-water dispersion of the polymer P in advance and / or during the contacting with the nonwoven fabric and / or after the incon - bring clock and can be applied to the impregnated nonwoven fabric before the drying step.
  • inorganic phosphorus or boron compounds which are capable of accelerating the crosslinking reaction of the polymer P with the organic compound V in the drying step are suitable as the phosphorus- or boron-containing inorganic compounds B.
  • Preference according to the invention is given to phosphoric acid, polyphosphoric acid, alkylphosphinic acids, alkylphosphonic acids with alkyl equal to methyl, ethyl, propyl, isopropyl, n-butyl or tert-butyl, hypophosphorous acid, phosphorous acid or tetrafluoroboric acid and their alkali metal salts, especially their sodium salts. and / or potassium salts, for example alkali metal hypophosphites, alkali metal phosphites, alkali metal polyphosphates, alkali metal phosphates, alkali metal dihydrogen phosphates and / or alkali metal tetrafluoroborate.
  • inorganic compounds B are used, they are used in a total amount of from 0.0001 to 10 parts by weight, preferably from 0.01 to 7 parts by weight and more preferably from 0.1 to 5 parts by weight, based on 100% by weight .
  • Parts Polymer P used.
  • At least one organic compound V is admixed with the water-in-water dispersion of the polymer P in advance and / or during the contacting with the nonwoven fabric and / or applied to the impregnated nonwoven fabric after the contacting and before the drying step. If the at least one organic compound V is added to the water-in-water dispersion in advance of contacting with the fiber fleece, optionally a partial or total amount of the compound V in the preparation of the water-in-water dispersion can be initially charged and any remaining residue - or total quantities after their preparation are added.
  • a subset of the compound V it is also possible for a subset of the compound V to be mixed in advance with the water-in-water dispersion and for the remaining amount or total amount to be mixed with the nonwoven fabric during incontacting.
  • the organic compound V is preferably admixed with the water-in-water dispersion of the polymer P before and / or during the contacting with the fiber fleece.
  • inorganic compounds B in addition to inorganic compounds B, it is also possible to use further optional auxiliaries known to the person skilled in the art, for example so-called thickeners, liquefiers, defoamers, neutralizing agents, buffer substances or preservatives. If such optional compounds are used in the process according to the invention, they can be added to the water-in-water dispersion of the polymer P beforehand and / or during the contacting with the nonwoven fabric and / or after contacting and applied to the impregnated nonwoven fabric before the drying step. The amounts of these optionally used compounds are familiar to the person skilled in the art or can be determined from this in routine tests.
  • the manner in which the water-in-water dispersion of the polymer P is brought into contact with the nonwoven fabric is of subordinate importance, provided that the water-in-water dispersion is applied uniformly to the nonwoven fabric or into the nonwoven fabric.
  • the contacting takes place by spraying the water-in-water dispersion of the polymer P on the nonwoven fabric or by impregnating the nonwoven fabric with the water-in-water dispersion.
  • the water-in-water dispersion of the polymer P is used in such an amount that 1 to 300 parts by weight, preferably 10 to 200 parts by weight and particularly preferably 50 to 150 parts by weight, when being brought into contact with the fiber web.
  • the impregnated nonwoven fabric obtained after contacting with the water-in-water dispersion of the polymer P, the organic compound V and the optionally further optional auxiliaries is prepared in a manner familiar to the person skilled in the art Way at a temperature> 120 0 C with formation of the swelling nonwoven dried or cured.
  • drying the resultant impregnated fiber fleece under training is carried fertil a source fleece into two drying stages, the first drying stage at a temperature ⁇ 120 0 C, preferably> 20 0 C and ⁇ 1 10 0 C, and most preferably> 40 and ⁇ 100 0 C and the second drying step at a temperature> 120 0 C, preferably> 130 0 C and ⁇ 250 0 C and particularly preferably> 140 0 C and ⁇ 220 0 C takes place.
  • the first drying step is advantageously carried out such that is dried at a temperature ⁇ 120 0 C until the obtained Rohquellvlies, which often does not yet have its final shape (so-called semi-finished) a residual moisture ⁇ 15 wt .-%, preferably ⁇ 12 Wt .-% and particularly preferably ⁇ 10 wt .-% has up.
  • the residual moisture is determined in general in the context of this document by first weighed about 1 g of the obtained (crude) source web at room temperature, subsequently dried this for 10 minutes at 110 0 C and subsequently cooled and is re-weighed at room temperature.
  • the residual moisture corresponds to the weight difference of the (raw) source web before and after the drying process, based on the weight of the (raw) source web before the drying process multiplied by a factor of 100.
  • the resulting semi-finished product is still deformable after heating to a temperature> 100 and can be brought at this temperature in the final form of the desired swellable nonwoven.
  • the subsequent second drying step is advantageously carried out such that the semi-finished product at a temperature> 120 0 C is heated until the formation of the source of this web has a residual moisture ⁇ 1 wt .-%, preferably ⁇ 0.5 wt .-% and in particular preferably ⁇ 0.1 wt .-%, wherein the polymer P and the organic compound V crosslink and cure usually as a result of a chemical condensation reaction.
  • the production of the swellable nonwoven takes place in that the semi-finished product is brought into the final shape in a molding press in the aforementioned temperature ranges and cured.
  • first (drying) and the second drying stage (curing) of the swellable nonwoven take place in one step, for example in a molding press. If the drying takes place in one working step, it takes place at a temperature> 120 ° C.
  • the source nonwovens obtainable by the process according to the invention advantageously have a planar form, such as flat sheets, webs or strips or even an elongated shape whose ratio of length (L) to maximum extension of the cross section (D) L / D >2,>5,>10,>100,> 1000 or ⁇ 100000 and whose cross-section may have any imaginable shape, such as a round shape, in particular a circular or ellipsoidal shape or even an angular shape, such as in particular a triangular, quadrangular, such as a square or a rectangular shape.
  • the swellable nonwoven webs according to the invention have a lower washout loss with aqueous media compared to the swellable webs of the prior art and are therefore advantageously suitable for water sealing, for example in waterproofing membranes or joint sealing tapes for moisture regulation, such as in interior moisture webs or moisture webs in air conditioning systems, for the separation of heavy metals from aqueous media, such as in ion exchangers, for water absorption, such as in absorbent towels or Absorbtionsbahnen and / or use as a moisture barrier.
  • the polymerization mixture was allowed to stir for 2 hours at 64 0 C and then added another 0.16 g Wako V 50, dissolved in 31, 4 g of deionized water. Then allowed the aqueous polymer dispersion for 1 hour at 64 0 C to react further and then gave 0.6 g of L (+) - ascorbic acid and 1, 1 g of a 70 wt .-% strength skyssri- tert-butyl hydroperoxide solution. Then allowed the resulting water-in-water polymer dispersion for 1 hour at 64 0 C to react further.
  • the water-in-water polymer dispersion was cooled to 45 0 C and 125 g of a 50 wt .-% aqueous solution of a copolymer of acrylic acid and maleic anhydride in the weight ratio 42/58 with a weight average molecular weight of 3000 g / mol (Sokalan CP ® 12S BASF SE) company and 12.5 g of a 30% strength by weight aqueous solution of a sodium salt Fettalkoholpolyglykolethersulfat (E- mulphor ® FAS 30 from BASF SE) was added and the resulting water-in-water polymer dispersion at that temperature for Stirred for 5 minutes.
  • Sokalan CP ® 12S BASF SE Sokalan CP ® 12S BASF SE
  • the solids content was generally determined by drying a defined amount of the water-in-water polymer dispersion (about 1 g) in an aluminum crucible with an inner diameter of about 5 cm at 120 ° C. in a drying oven to constant weight (about 2 g) hours). Two separate measurements were carried out in each case. The values given in the examples represent the mean value of the respective two measurement results.
  • the viscosity was determined in general, at a given solids content of the respective water-in-water polymer dispersion according to DIN EN ISO 2555 using a Brookfield viscometer "Brookfield RVT", spindle 3, 20 rpm for minutes te, at a temperature of 23 0 C.
  • Example 2 The preparation of Example 2 was carried out analogously to the preparation of Example 1 with the difference that 12.6 g of triethanolamine were added instead of 6.3 g of triethanolamine.
  • Comparative Example 1 The preparation of Comparative Example 1 was carried out analogously to the preparation of Example 1 with the difference that no triethanolamine was added.
  • Example 3 The preparation of Example 3 was carried out analogously to the preparation of Example 1 with the difference that 328 g of deionized water instead of 203 g of deionized water were submitted that no copolymer of acrylic acid and maleic anhydride in the weight ratio 42/58 and no 30 wt. % aqueous solution of a fatty alcohol polyglycol ether sulfate sodium salt were added and that after cooling, only 0.6 g of triethanolamine instead of 6.3 g of triethanolamine were added.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 24.3% by weight and the viscosity to 2020 mPas.
  • Comparative Example 2 was carried out analogously to the preparation of Example 3 with the difference that no triethanolamine was used.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 24.1% by weight and the viscosity to 2225 mPas.
  • Example 4 The preparation of Example 4 is carried out analogously to the preparation of Example 1 with the difference that 264 g of deionized water were introduced instead of 203 g of deionized water, that 0.9 g of ethylene glycol diglycidyl ether (Decanol ® EX-810 Fa. Nagase Chemtex) instead of 0.6 g Trimethylolpropanethoxilattriacrylat were used and 62.5 g instead of 125 g copolymer of acrylic acid and maleic anhydride in a weight ratio 42/58 were added and that after cooling len no triethanolamine was added.
  • ethylene glycol diglycidyl ether Decanol ® EX-810 Fa. Nagase Chemtex
  • Trimethylolpropanethoxilattriacrylat were used and 62.5 g instead of 125 g copolymer of acrylic acid and maleic anhydride in a weight ratio 42/58 were added and that after cooling len no triethanolamine was added.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 26.2% by weight and the viscosity to 1050 mPas.
  • Example 5 The preparation of Example 5 was carried out analogously to the preparation of Example 4, with the difference that 2.3 g of ethylene glycol diglycidyl ether were used instead of 0.9 g of ethylene glycol diglycidyl ether.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 26.1% by weight and the viscosity to 1060 mPas.
  • Example 6 was prepared analogously to the preparation of Example 4 with the difference that 3.7 g of ethylene glycol diglycidyl ether were used instead of 0.9 g of ethylene glycol diglycidyl ether.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 26.5% by weight and the viscosity to 1070 mPas.
  • Example 7 was prepared analogously to the preparation of Example 4 with the difference that 5.1 g of ethylene glycol diglycidyl ether were used instead of 0.9 g of ethylene glycol diglycidyl ether.
  • the solids content of the obtained water-in-water polymer dispersion was determined to be 26.7% by weight and the viscosity to 1090 mPas.
  • Example 8 The preparation of Example 8 was carried out analogously to the preparation of Example 4, with the difference that 6.0 g of ethylene glycol diglycidyl ether were used instead of 0.9 g of ethylene glycol diglycidyl ether.
  • the solids content of the obtained water-in-water polymer dispersion was determined to be 26.4% by weight and the viscosity to 1150 mPas.
  • Comparative Example 3 was carried out analogously to the preparation of Example 4 with the difference that no Ethylenglykoldiglycidylether was used.
  • the solids content of the obtained water-in-water polymer dispersion was determined to be 26.0% by weight and the viscosity to 1050 mPas.
  • Example 9 The preparation of Example 9 was carried out analogously to the preparation of Comparative Example 3, with the difference that, after cooling to room temperature, 28.5 g of D-glucose and 28.5 g of sodium hypophosphite were added to the water-in-water polymer dispersion.
  • the solids content of the resulting water-in-water polymer dispersion was determined to be 29.2% by weight and the viscosity to 780 mPas.
  • the water-in-water polymer dispersions obtained in Examples 1 to 9 and Comparative Examples 1 to 3 were diluted at room temperature by addition of deionized water with stirring to a solids content of 24% by weight and are referred to below as binder liquors B1 to B9 and also V1 to V3.
  • each polypropylene (PP) needle fleeces 29.7 x 21, 0 cm [A4] with a basis weight of 280 g / m 2 ) in the longitudinal direction over an endless PES wire belt with a tape speed of 60 cm in each case passed through the aforementioned aqueous binder liquors B1 to B9 and V1 to V3 per minute.
  • the wet application was set at 1165 g / m 2 (corresponding to 280 g / m 2 of binder as a solid).
  • the impregnated PP needled webs thus obtained were dried on a plastic net carrier for 14 minutes at 150 ° C.
  • the source nonwovens thus obtained will be referred to as QB1 to QB9 and QV1 to QV3.
  • the source nonwovens thus obtained will be referred to as QB1 to QB9 and QV1 to QV3.
  • round test specimens having a diameter of 105 mm were cut out of the obtained source webs QB1 to QB9 and QV1 to QV3.
  • the test specimens obtained were then stored for 24 hours at 23 0 C and 50% relative humidity in a climate chamber.
  • the results obtained are listed in Table 1. The lower the corresponding washout loss, the better the results obtained.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

L'invention concerne un procédé de production de tissus non tissés gonflants à perte au lavage réduite.
EP10722358A 2009-06-08 2010-06-01 Procédé de production d'un tissu non tissé gonflant Withdrawn EP2440621A1 (fr)

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EP10722358A EP2440621A1 (fr) 2009-06-08 2010-06-01 Procédé de production d'un tissu non tissé gonflant
PCT/EP2010/057603 WO2010142568A1 (fr) 2009-06-08 2010-06-01 Procédé de production d'un tissu non tissé gonflant

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