EP0935019A1 - Beschichtungsmittel für Fasern - Google Patents

Beschichtungsmittel für Fasern Download PDF

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Publication number
EP0935019A1
EP0935019A1 EP99101835A EP99101835A EP0935019A1 EP 0935019 A1 EP0935019 A1 EP 0935019A1 EP 99101835 A EP99101835 A EP 99101835A EP 99101835 A EP99101835 A EP 99101835A EP 0935019 A1 EP0935019 A1 EP 0935019A1
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EP
European Patent Office
Prior art keywords
weight
fibers
particularly preferably
sulfosuccinate
agglomeration inhibitor
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.)
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EP99101835A
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German (de)
English (en)
French (fr)
Inventor
Stephan Dr. Hütte
Bernd Klinksiek
Andreas Dr. Endesfelder
Hans-Joachim Dr. Wollweber
Hans-Josef Behrens
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Bayer AG
Asahi Kasei Spandex Europe GmbH
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Bayer AG
Bayer Faser GmbH
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Publication of EP0935019A1 publication Critical patent/EP0935019A1/de
Withdrawn legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/70—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyurethanes
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
    • D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
    • D04B1/18—Other fabrics or articles characterised primarily by the use of particular thread materials elastic threads
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/285—Phosphines; Phosphine oxides; Phosphine sulfides; Phosphinic or phosphinous acids or derivatives 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/288—Phosphonic or phosphonous acids or derivatives 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • D06M13/295—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing polyglycol moieties; containing neopentyl moieties
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/38—Polyurethanes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material

Definitions

  • the invention relates to coating compositions for fibers and a method for their Manufacturing.
  • the invention relates in particular to preparation agents for elastanes Basis of a dispersion of fatty acid metal salts and agglomeration inhibitors in Polyorganosiloxanes and mineral oils.
  • the preparations are made through a precipitation process made from fine-grained and sedimentation-stable dispersions result in a narrow grain size distribution and are free of agglomerates.
  • the Coating agents reduce the electrical resistance of elastanes, whereby neither in the application nor in the processing of the elastane, even with one deposits of coating agents on machine parts for a long period of time. Elastanes treated with the coating agents stick even after a long time Storage time not and remain processable.
  • fiber used in the present invention includes fiber Staple fibers and / or continuous filaments.
  • the fibers e.g. Elastane can by spinning processes known in principle, such as the dry spinning process, the wet spinning process or the melt spinning process.
  • Elastane i.e. elastic polyurethane fibers made from long-chain synthetic polymers, which are at least 85% segmented polyurethanes based on e.g. Polyethers, polyesters and / or polycarbonates are well known. Yarns made from such fibers are used to manufacture fabrics or fabrics or fabrics that are used for the manufacture of corsetry, Linen, stockings, sportswear and ribbons are suitable. Polyurethane fibers have considerable compared to other, non-elastic textile fibers Stickiness. Bonding of the elastanes occurs particularly when elastanes be wound on a spool or a partial warp beam. A sticking of the Spandex or the increased adhesion of the fibers to one another is particularly then observed when the fibers are stored for a long time before further processing were. This effect is exacerbated if the storage of the material is elevated Temperature.
  • the stickiness or the adhesion of elastanes to spools or partial warp beams can be used when processing the polyurethane fibers with, for example, polyamide fibers or cotton by a warp or circular knitting process or automatic hosiery lead to strong tension in the fiber during unwinding, which can lead to thread breakage can lead and in extreme cases bobbins or partial warp beams made of such fibers no longer processable.
  • magnesium stearate with organic solvents such as Isopropanol, chloroform, Acetone or heptane made into a paste with polyorganosiloxane or mineral oil mixed and ground in a mill.
  • organic solvents such as Isopropanol, chloroform, Acetone or heptane made into a paste with polyorganosiloxane or mineral oil mixed and ground in a mill.
  • the disadvantage of this manufacturing process is that magnesium stearate is finely divided into the silicone oil by a complex grinding process is incorporated.
  • organic solvents the time-consuming recovery of the solvents is necessary depending on the type of solvent, there is still a risk of ignition or explosion of the solvent.
  • JP-188 875 is used to reduce the adhesion of polyurethane fibers described a preparation.
  • This consists of a polydimethylsiloxane, a higher alcohol, its ether or a fatty acid ester consisting of a Fatty acid with at least 12 carbon atoms, a modified silicone and the, metal salt of a fatty acid with at least eight carbon atoms.
  • the disadvantage however, the preparation mentioned is similar to that of the others described above known preparation.
  • the dispersed metal soaps list during application Polyurethane fibers to build up deposits in the preparation system, for example can lead to the blockage of preparation lines. Associated with it the running time of the spinning machines is shortened. The cleaning effort for cleaning the spinning machines and the preparation system is increased considerably. A safe and even preparation of the polyurethane fiber over a long period of time is not achieved with such preparations.
  • JP-60-67 442 describes the preparation of finely divided particles of fatty acid metal salts in polydimethylsiloxane for the preparation to reduce the adhesion of elastanes.
  • Magnesium stearate or calcium oleate is dissolved in a pressure-stable vessel in hexane or benzene at 140 or 130 ° C and precipitated by rapid cooling at 10 0 C / min. Entering this dispersion in low-viscosity polydimethylsiloxane and then distilling off hexane or benzene finally leads to the ready-to-use preparation.
  • the disadvantage of this preparation is the complex and costly preparation process for the preparation caused by the distillation of hexane or benzene.
  • DD-251 578 is used to reduce the adhesion of elastanes be prepared by the wet spinning process, the use of an aqueous Suspension with finely divided magnesium and / or calcium stearate and optionally Polydimethylsiloxane described as a preparation.
  • the disadvantage of this invention is however. that to remove the water from the dispersion after application the polyurethane fiber requires special drying of the fiber. So that's a additional processing step connected, which increases the cost of the product leads.
  • the invention has for its object a preparation for fibers, in particular for elastanes, to be made available, for example, during application Roll, thread guide or spray technology is easy to process and those in the application and especially in the processing of elastanes with, for example Cotton or polyamide fibers for surface goods not for deposits in the preparation system or on processing machines.
  • the stickiness Elastane is said to be reduced by the preparation and the processability of using the preparation coated elastane guaranteed even after a long storage period be.
  • Further requirement for preparations for elastane, if they are solids contained, in the form of dispersions, is to ensure a uniform Preparation order and coupled with it an even application of solids by stabilizing the preparation against sedimentation.
  • the stability of dispersions depends on many factors such as the particle size and shape, polarity, charge and density. However, among all these factors is the Particle size is the most important factor influencing sedimentation stability. Therefore it must be a primary goal in the production of suitable dispersions, set the grain size of the solid in the preparation as low as possible. the primary particles must not agglomerate into clusters.
  • Another object of the invention is an improved Processes for making preparations for fibers are available too make grinding unnecessary.
  • the preparation oils according to the invention for fibers in particular Polyurethane fibers. in the form of dispersions.
  • Mineral oil is understood here as a liquid distillation product (e.g. from petroleum), which consists essentially of a mixture of saturated hydrocarbons.
  • the coating compositions according to the invention contain linear and / or branched Polyorganosiloxanes, preferably linear polyorganosiloxanes and particularly preferred linear polydimethylsiloxanes with a viscosity of 2 to 150 mPas (25 ° C) ⁇ preferably with a viscosity of 2.5 to 50 mPas (25 ° C) and particularly preferred with a viscosity of 2.5 to 20 mPas (25 ° C).
  • the content of linear, or branched Polyorganosiloxane, preferably linear polyorganosiloxane and especially preferably linear polydimethylsiloxane is from 30 to 98.97% by weight, preferably 50 to 96.9% by weight and particularly preferably 70 to 94.8% by weight, based on the Weight of the preparation according to the invention.
  • metal salts used to produce the preparations according to the invention of fatty acids are those whose metal is a metal of the first to the third main group of the periodic table or zinc.
  • the fatty acids are saturated or unsaturated, from at least six and at most 30 carbon atoms constructed and are mono- or bifunctional.
  • the metal salts of fatty acids it is particularly lithium, magnesium, calcium, aluminum and Zinc salts of oleic, palmitic or stearic acid, particularly preferably around magnesium stearate, Calcium stearate or aluminum stearate.
  • the content of metal salts from Fatty acids in the preparation according to the invention is from 0.01 to 20% by weight preferably from 0.05 to 8% by weight, particularly preferably from 0.1 to 4% by weight, entirely particularly preferably from 0.1 to 2% by weight, based on the weight of the preparation.
  • the mineral oils of the coating composition according to the invention have a viscosity of 2 to 500 mPas (25 ° C), preferably 3 to 300 mPas (25 ° C) and particularly preferably 3 to 200 mPas (25 ° C).
  • the mineral oils are further characterized by a density of 800 to 900 kg / m 3 (15 ° C) and a viscosity-density constant (VDK, determination according to DIN 51378) of 0.770 to 0.825.
  • the mineral oil content in the preparation according to the invention is from 1 to 69% by weight, preferably from 3 to 50% by weight and particularly preferably from 5 to 30% by weight. based on the weight of the preparation.
  • the preparations according to the invention contain cation-active, anion-active or nonionic antistatic compounds, if appropriate also in a mixture.
  • cation-active, anion-active or nonionic antistatic compounds if appropriate also in a mixture.
  • An overview of possible antistatic compounds is given in the book "Kunststoffadditive" by R. Gumbleter and H. Müller, Carl Hanser-Verlag Kunststoff, Vol. 3, 1990, pages 779 to 805.
  • Examples of cationic agglomeration inhibitors are ammonium compounds, for anionic agglomeration inhibitors salts of sulfonic or phosphoric acids and for nonionic agglomeration inhibitors fatty or phosphoric acid esters, alkoxylated fatty alcohols, polyaminosiloxanes or alkoxylated polyorganosiloxanes.
  • Suitable anionic agglomeration inhibitors are: fatty alcohols such as sodium lauryl sulfate or ammonium lauryl sulfate, fatty alcohol ether sulfates of the formula R- (O-CH 2 -CH 2 ) n-OSO 3 Na, where R is hydrogen or an alkyl group having 1 to 30 hydrocarbon atoms and n is a number from 1 to 20, Sodium alkylsulfoacetate of the formula RO-CO-CH 2 -SO 3 Na, where R represents an alkyl group with 1 to 30 hydrocarbon atoms, Alkylolamide sulfates of the formula R-CONH- (CH 2 ) n -OSO 3 Na, where R is an alkyl group with 1 to 30 hydrocarbon atoms and n is a number from 1 to 6 or Fatty alcohol ether phosphates of the formula RO- (CH 2 -CH 2 -O) n -PO (ONa) 2 , where R is hydrogen or an
  • Suitable cationic agglomeration inhibitors are: quaternary ammonium salts of the formula R 1 R 2 R 3 R 4 N + Cl - , where R 1 R 2 , R 3 and R 4 independently of one another are identical or different and represent hydrogen or an alkyl group having 1 to 30 carbon atoms.
  • Suitable nonionic agglomeration inhibitors are: Polyoxyethylene fatty alcohol ethers, polyoxyethylene fatty acid esters, polyoxyethylene glycol fatty acid esters, diethylene glycol monofatty acid esters, fatty acid alkanolamides of the formula R-CO-NH- (CH 2 -CH 2 ) n -OH, where R is an alkyl group with 1 to 30 hydrocarbon atoms and n is a number from 1 to 20, sucrose esters , for example sucrose palmiat, pentaerythritol partial esters, for example pentaerythritol monostearate, ethoxylated pentaerythritol partial esters, for example pentaerythritol monostearate polyglycol ether, sorbitan fatty acid esters or ethoxylated sorbitan fatty acid esters.
  • Anion-active and / or non-ionic agglomeration inhibitors are preferably added to the preparation according to the invention; agglomeration inhibitors from the groups of the sulfonic acids and the fatty and phosphoric acid esters are particularly preferred. Agglomeration inhibitors from the groups of the dialkyl sulfosuccinates, the nonionic phosphoric acid esters and the sugars esterified with fatty acids are very particularly preferred.
  • dialkyl sulfosuccinates can be prepared, for example, as in the magazine C.R. Carly, Ind. Eng. Chem., Vol. 31, page 45, 1939.
  • dialkyl sulfosuccinates are sodium bistridecyl sulfosuccinate, Sodium dioctyl sulfosuccinate, sodium dihexyl sulfosuccinate. Sodium diamyl sulfosuccinate, Sodium diisobutyl sulfosuccinate and sodium dicyclohexyl sulfosuccinate.
  • dialkyl sulfosuccinates are sodium bistridecyl sulfosuccinate, Sodium dioctyl sulfosuccinate and sodium dihexyl sulfosuccinate.
  • Particularly preferred examples of the phosphoric acid esters are those in which R 1 represents an alkyl group having 14 to 20 carbon atoms, R 2 represents hydrogen or a methyl group and x and y correspond to 1 or 2 and z corresponds to 3 to 10.
  • the content of agglomeration inhibitor D) in the preparation according to the invention is from 0.02 to 15% by weight, preferably 0.05 to 5% by weight and particularly preferred 0.1 to 3 wt .-%, based on the weight of the preparation.
  • the invention also relates to a process for producing coating compositions for fibers based on a dispersion of fatty acid metal salts and an agglomeration inhibitor in a mixture of polyorganosiloxane and mineral oil, which is characterized in that from 0.01 to 20% by weight, preferably from 0.05 to 8% by weight, particularly preferably from 0.1 to 4% by weight, very particularly preferably from 0.1 to 2% by weight, metal salt B) of a saturated or unsaturated, mono- or bifunctional C 6 -C 30 fatty acid in from 1 to 69% by weight, preferably from 3 to 50% by weight, particularly preferably from 5 to 30% by weight, of a mineral oil C) with heating to from 70 to 170 ° C.
  • the warm solution in a mixing device intensively and quickly with from 30 to 98.97 wt .-%, preferably from 50 to 96.9 wt .-%, particularly preferably from 70 to 94.8% by weight, polyalkylsiloxane A) is mixed in such a way that the resulting dispersion may be directly connected nd is homogenized, and that the mineral oil C) or the polyalkylsiloxane A) before mixing or the resulting dispersion before or preferably after the homogenization from 0.02 to 15% by weight, preferably from 0.05 to 5% by weight , particularly preferably from 0.1 to 3% by weight of agglomeration inhibitor D) are added.
  • the homogenization is preferably carried out by entering shear energy with an energy density of at least 10 6 J / m 3 based on the volume of the preparation. particularly preferably at least 3x10 6 J / m 3 , very particularly preferably of at least 4x10 6 J / m 3 . This promotes fine particle size and sedimentation stability.
  • the preparation of the preparations according to the invention in the form of dispersions are present, is carried out by a precipitation process by dissolving fatty acid metal salts in hydrocarbons in the heat and combining this phase with the polyorganosiloxane-containing phase.
  • the precipitation can consist of a precipitation device from a two- or multi-stage dispersing device with an optional subsequent one Honiogenization stage are carried out.
  • the preparation of the invention Preparations can also be made by entering the metal salt Phase in the polyorganosiloxane-containing phase in a boiler with subsequent Monogenization done by a homogenizer.
  • the addition of Agglomeration inhibitor can in all cases in the preparation of the preparation anywhere.
  • a suitable multi-stage dispersing device and a homogenizing nozzle will in U.S. Patent No. 5,302,660.
  • the apparatus described is used to achieve a rapid mixing of two material flows, the to be brought together to a chemical reaction.
  • the implementation a precipitation process in the above-mentioned apparatus with, if necessary, a subsequent one Homogenization leading to fine-grained and sedimentation-stable dispersions leads with narrow grain size distribution, which are free of agglomerates, however not described.
  • the known dispersion devices enable two material flows very much to mix quickly with each other. It was found that due to the entry high shear energy when using such devices for manufacturing of preparation oils for fibers according to the precipitation process according to the invention the fatty acids Metal salts to form a good and narrow grain size distribution incorporated into polyorganosiloxanes free of agglomerates and stable to sedimentation can be.
  • the method for producing the preparations according to the invention by means of a two- or multi-stage dispersing device with optionally subsequent Homogenization is compared to a precipitation process in the boiler with subsequent Homogenization preferred because this process is operated continuously can.
  • the invention further relates to fibers, in particular polyurethane fibers, which are coated with the coating agent according to the invention.
  • the polyurethane fibers coated with the coating agent according to the invention order especially from segmented polyurethane polymers, for example those based on polyethers, polyesters, polyether esters and / or polycarbonates. Fibers of this type can be produced by processes which are known in principle such as those described in US 2,929,804, 3 097 192, 3 428 711, 3 553 290 and 3 555 115 and in the publication WO-9 309 174 to be discribed. Furthermore, the polyurethane fibers made of thermoplastic Order polyurethanes, their production, for example, in writing US 5,565,270. The polyurethane is based in particular on organic Diisocyanates and a chain extender with several active hydrogens, such as.
  • Di- and polyols di- and polyamines, hydroxylamines, hydrazines, Semicarbazides, water or a mixture of these components.
  • Preferred Diols are glycol, butanediol and hexanediol.
  • Preferred diamines are ethylenediamine, 1,2-propanediamine, 2-methyl-1,5-diaminopentane, 1,3-diaminocyclohexane and 1-methyl-2,4-diaminocyclohexane.
  • the fibers can contain a variety of different other additives for different purposes, such as antioxidants. Stabilizers against heat, light and UV radiation, pigments and matting agents. Dyes, lubricants and lubricants. Examples of antioxidants, stabilizers against heat, light and UV radiation are stabilizers from the group of sterically hindered phenols, HALS stabilizers (h indered a mine l ight s tabilizer), the triazines, the benzophenones and the benzotriazoles. Examples of pigments and matting agents are titanium dioxide, zinc oxide and barium sulfate. Examples of dyes are acidic disperse and pigment dyes and optical brighteners. Examples of lubricants and lubricants are metal salts of fatty acids and silicone and mineral oils. The additives mentioned are dosed in such a way that they show no effects contrary to the preparation oil applied to the outside of the fiber and produced by a precipitation process.
  • the coating compositions according to the invention for fibers in the form of dispersions available and by a compared to a conventional grinding process simple and economical precipitation process in a mixing nozzle or in a boiler with subsequent homogenization can have, as in Example 1 is shown, the surprising advantage that it has a medium Grain size of D50 ⁇ 3 ⁇ m are very fine, with a very narrow grain size distribution have a very low proportion of coarse-grained with a D90 of ⁇ 10 ⁇ m Have particles.
  • the coating agents are free from agglomerates and are good against sedimentation with a sedimentation rate of ⁇ 20% per 10 days stable.
  • the coating composition according to the invention has only 2 wt .-% and less fatty acid metal salt, remain the excellent Preserve properties of the coating agent.
  • Example 3 When applying the coating compositions of the invention to polyurethane fibers is also surprisingly found, as shown in Example 3, that already by the small amount of a fatty acid salt in the coating agent the strengthening of the adhesion over a longer storage period of the fibers even with increased Temperature, and with it the stickiness of the polyurethane fiber is greatly reduced and the processing of the fibers e.g. good on a circular knitting machine and runs without deposits on knitting needles.
  • Example 3 it was found to be particularly surprising. that the coating compositions of the invention also in long-term tests during application no deposits or on polyurethane fibers via a preparation roll Blockages in the pipes of the coating material or in preparation trays showed. As a result, application of the coating agent is carried out via a enables a long period of time. The uniformity of the application is also improved and an interruption of a production process due to necessary Cleaning work unnecessary.
  • the measurements to determine the grain size distributions are carried out with Mastersizer M20, company Malvern Instruments about laser light diffraction and laser light scattering. Polydimethylsiloxane with a viscosity of 10 mPas (25 ° C) are used.
  • the grain size of the particles is given in micrometers ( ⁇ m) depending on the volume distribution of the particles at 10, 50 and 90% before and after treatment with ultrasound for 180 s.
  • the difference between the grain size distributions before and after the ultrasound treatment a measure of the presence of agglomerates. If the difference is small, there are none Agglomerates present.
  • the viscosity of the preparation oils is determined using a Haake viscometer, model CV 100 at a temperature of 20 ° C. and a viewing speed of 300 s -1 .
  • the adhesion of the thread to a bobbin is determined by first of all Thread from a bobbin weighing 500 g up to 3 mm above the bobbin tube is cut off. Then a weight is hung on the thread and determines the weight with which the load rolls off the spool.
  • the so certain liability is a measure of the processability of the coils. Is liability too high, can be difficult to process into flat goods due to thread breaks become.
  • the determination of liability after a storage period of 8 weeks at an elevated temperature of 40 ° C describes an aging process and is a measure for the development of liability after a long storage period at RT. Warehousing the coils take place at 40 ° C in a heating cabinet with a rel. humidity of 60%. After storage, liability becomes as described above measured.
  • Deposits in the preparation system are determined by using the preparation oil in a long-term test over 14 days without interruption due to roller technology is applied to a polyurethane fiber. At the end of the experiment it is assessed how much solid is deposited from the dispersion in the preparation system Has. The more deposits there are, the less suitable the preparation is, because the preparation system with storage container, piping and preparation tubs and rolls or thread guides or spray nozzles cleaned more often, and thus a production process has to be interrupted more often.
  • Fig. 1 shows an example of the flow diagram of the process for the precipitation of fatty acid Metal salt in polyorganosiloxane.
  • the two material flows, e.g. in Mineral oil dissolved fatty acid metal salts and polyorganosiloxanes using the metering pumps 8 and 9 dosed from the batch containers 6 and 7 and the finished preparation oil drained into the product container 12.
  • the agglomeration inhibitor can in the batch containers 6 or 7, or in the product container 12 in a suitable form be added.
  • the pre-pressure in front of the mixing device is via pressure gauge 10 and 11 checked.
  • FIG. 2 shows the flow diagram of a variant of the method according to the invention.
  • the Phase of fatty acid metal salt and mineral oil from the batch container 6 is in the Polyorganosiloxane entered in the mixing container 7 and mixed.
  • the mixture is conveyed through the homogenizer 15 by means of the metering pump 9 and the finished Preparation oil drained into the product container 12.
  • the agglomeration inhibitor D can be in the batch containers 6 or 7 or in the Product container 12 can be added in a suitable form.
  • polyurethane fibers to check the processing properties of fibers with the new preparations was made by implementing Polytetrahydrofuran (PTHF) with an average molecular weight of 2000 g / mol with methylene bis (4-phenyl diisocyanate) (MDI) in a molar ratio from 1 to 1.8.
  • PTHF Polytetrahydrofuran
  • MDI methylene bis (4-phenyl diisocyanate
  • the prepolymer thus produced was treated with dimethylacetamide diluted and then with a mixture of ethylenediamine (EDA) and diethylamine (DEA) (97: 3 ratio) chain extended in dimethylacetamide.
  • EDA ethylenediamine
  • DEA diethylamine
  • the molar ratio from chain extender and chain terminator to unreacted isocyanate in the prepolymer was 1.075.
  • the solids content of the segmented so produced Polyurethane was 30% by weight.
  • the polyurethane urea solution has one Viscosity of 120 Pas (50 ° C) and the polymer has an intrinsic viscosity of 0.98 g / dl (measurement at 25 ° C in dimethylacetamide with a concentration of 0.5 g Polymer in 100 ml of dimethylacetamide).
  • the polyurethane-urea spinning solution (percentages in relation on the weight of the finished fiber): (a) 1.0% 1, ⁇ 3,5-tris (4-tert-butyl-3-hydroxy-2,5-dimethylbenzyl) - 1,3,5-triazine 2,4,6- (1H, 3H, 5H) -trione (Cyanox 1790, Cytec), (b) 0.05% titanium dioxide (type RKB 2, Bayer AG), (c) 0.15% magnesium stearate.
  • Preparations 1-1 to 1-3 contain low-viscosity silicone oil and polyamylsiloxane Mg stearate, which is obtained by a milling process with a pearl mill (type MS 12, Fryma) was registered.
  • the grain size distribution shows that the particles not in the form of agglomerates, the proportion of coarse particles Particles, however, even after 5 grinding cycles with a D90 value of> 10 ⁇ m.
  • Stabilization against sedimentation improves with decreasing Grain size (tests 1-1 and 1-2), however, deteriorates, as in experiment 1-3, with decreasing content of Mg stearate in the preparation. The reason for this can be a weak interaction of the individual particles be with each other.
  • Preparations 1-4 to 1-8 were produced by the precipitation process described schematically in FIG. 1 in a mixing nozzle 1.
  • a 130 ° C. hot stream of hydrocarbon and Mg stearate in experiments 1-7 and 1- 8 additionally phosphoric acid ester as agglomeration inhibitor) with a stream of low-viscosity silicone oil (in experiment 1-6 additionally polyamylsiloxane) at 20 ° C with a pressure of 50 bar in the mixing nozzle 1 and then homogenized with an energy density of 5x10 6 J / m 3 .
  • the ratios of the material flows corresponded to those of the composition of the finished preparation.
  • Preparations 1-9 and 1-10 were produced by the precipitation process described schematically in FIG. 2 in a kettle with subsequent homogenization.
  • a 120 ° C hot stream of mineral oil, Mg stearate and fatty alcohol EO adduct or phosphoric acid ester was added with stirring to a kettle with silicone oil at 20 ° C and then through a homogenizer 15 (see Fig. 2) at an energy density homogenized of 5x10 6 J / m 3 .
  • the preparations contain agglomerates and show an increased coarse fraction but with good stabilization against sedimentation in experiment 1-9. Homogenization breaks the agglomerates in the preparation and improves stabilization against sedimentation.
  • the preparations made by precipitation in the kettle with subsequent honing contain no agglomerates, with a very small coarse fraction with D90 values of ⁇ 10 ⁇ m, have a narrow grain size distribution and a sedimentation rate of ⁇ 20% / 10 d a good stabilization against sedimentation.
  • Experiment 1-11 shows the result of the characterization of a preparation, which according to the patent specification JP-60-67 442 by a precipitation process of Mg stearate in Hexane in a kettle followed by the addition of silicone oil and polyamylsiloxane and removal of hexane by distillation.
  • the preparation shows good stabilization against sedimentation, but is due to the strong Tendency to agglomeration and the increased viscosity, probably due to strong interactions between the solid particles in the preparation, not as a preparation oil for the production of fibers, especially polyurethane fibers, suitable.
  • Experiment 2-2 shows that polyamylsiloxane is part of the preparation Electrical volume resistance of polyurethane fibers reduced, this branched So siloxane increases electrical conductivity. This result corresponds the observation made in U.S. Patent 3,296,063.
  • the volume resistance of phosphoric acid ester and / or Na dioctyl sulfosuccinate was increased however, the polyurethane fibers are further lowered, i.e. the electrical Conductivity increased further.
  • Na dioctyl sulfosuccinate is in front of the phosphoric acid ester and this in turn is the most effective before polyamylsiloxane Means for reducing volume resistance.
  • Experiments 3-1 and 3-2 show that when applying preparations based on silicone oil or silicone oil with polyamylsiloxane the increase in Adhesion of polyurethane fibers with a storage time of 8 weeks and a temperature of 40 ° C, as is often the case during transport, in warehouses or subtropical countries occurs, is very strong and the processability of the coils is often not possible is.
  • the adhesion values obtained in these experiments are above 1 cN, which is a limit for successful processability of polyurethane fibers on a circular knitting machine, for example. Liability of more than 1 cN when processing the bobbins into thread breaks, with the consequence of Machine downtime. In extreme cases, even a thread of the Be pulled out.
  • the preparations used in experiments 3-1 and 3-2 based on silicone oil or silicone oil with polyamylsiloxane are therefore not suitable for the preparation of polyurethane fibers.
  • Mg stearate in the preparations for reducing the Tackiness of polyurethane fibers is, however, among those who go through a milling process were produced, less than those produced by precipitation in the Mixing nozzle or precipitation in the boiler with subsequent homogenization were. This is enough for preparations caused by the case processes described were produced, 1 wt .-% Mg stearate from the stickiness of polyurethane fibers to reduce to the desired level.
  • the one produced by a precipitation process Preparation is to set the same behavior regarding liability behavior a Mg stearate content of 4% by weight is necessary.

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  • Chemical Kinetics & Catalysis (AREA)
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  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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WO2001036720A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for regulating agglomeration of elastic material
WO2001036721A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for regulating strength degradation in elastic strand
WO2001036726A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for improving creep resistance of a substrate composite
WO2001086054A1 (de) * 2000-05-09 2001-11-15 Henkel Kommanditgesellschaft Auf Aktien Mit uv-strahlenfiltern ausgerüstete gewebe
US6531085B1 (en) 1999-11-19 2003-03-11 Kimberly-Clark Worldwide, Inc. Method for improving strength of elastic strand
WO2003072873A1 (fr) * 2002-02-28 2003-09-04 Sanyo Chemical Industries, Ltd. Lubrifiant pour le traitement de fibre elastique

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JP4747255B2 (ja) * 2000-12-27 2011-08-17 Ｊｎｃ株式会社 帯電性を有するトウおよびそれを用いた積層体
KR20030070190A (ko) * 2002-02-21 2003-08-29 주식회사 효성 사간 점착성을 향상시킨 스판덱스 방사유제 조성물
US7297395B2 (en) * 2002-07-30 2007-11-20 Kimberly-Clark Worldwide, Inc. Superabsorbent materials having low, controlled gel-bed friction angles and composites made from the same
US20040023589A1 (en) * 2002-07-30 2004-02-05 Kainth Arvinder Pal Singh Superabsorbent materials having high, controlled gel-bed friction angles and composites made from the same
US20040023579A1 (en) * 2002-07-30 2004-02-05 Kainth Arvinder Pal Singh Fiber having controlled fiber-bed friction angles and/or cohesion values, and composites made from same
US20040044321A1 (en) * 2002-08-27 2004-03-04 Kainth Arvinder Pal Singh Superabsorbent materials having controlled gel-bed friction angles and cohesion values and composites made from same
US20040044320A1 (en) * 2002-08-27 2004-03-04 Kainth Arvinder Pal Singh Composites having controlled friction angles and cohesion values
US20040253890A1 (en) * 2003-06-13 2004-12-16 Ostgard Estelle Anne Fibers with lower edgewise compression strength and sap containing composites made from the same
US20040253440A1 (en) * 2003-06-13 2004-12-16 Kainth Arvinder Pal Singh Fiber having controlled fiber-bed friction angles and/or cohesion values, and composites made from same
US7259206B2 (en) * 2003-09-04 2007-08-21 Nippon Paint Co., Ltd. Water-borne resin composition and electrocoating composition
DE102008026264A1 (de) * 2008-06-02 2009-12-03 Emery Oleochemicals Gmbh Antistatikmittel enthaltend Fettalkoholethersulfat und Polyethylenglycolfettsäureester
CN102465447B (zh) * 2010-11-05 2013-08-28 浙江尤夫高新纤维股份有限公司 海式缆绳用聚酯纤维表面涂敷材料及其生产工艺
JP5895312B2 (ja) * 2011-05-27 2016-03-30 東レ・オペロンテックス株式会社 弾性布帛

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WO2001036720A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for regulating agglomeration of elastic material
WO2001036721A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for regulating strength degradation in elastic strand
WO2001036726A1 (en) * 1999-11-19 2001-05-25 Kimberly-Clark Worldwide, Inc. Method for improving creep resistance of a substrate composite
US6531085B1 (en) 1999-11-19 2003-03-11 Kimberly-Clark Worldwide, Inc. Method for improving strength of elastic strand
US6540951B1 (en) 1999-11-19 2003-04-01 Kimberly-Clark Worldwide, Inc. Method for regulating agglomeration of elastic material
US6962749B2 (en) 1999-11-19 2005-11-08 Kimberly-Clark Worldwide, Inc. Method for improving strength of elastic strand
WO2001086054A1 (de) * 2000-05-09 2001-11-15 Henkel Kommanditgesellschaft Auf Aktien Mit uv-strahlenfiltern ausgerüstete gewebe
WO2003072873A1 (fr) * 2002-02-28 2003-09-04 Sanyo Chemical Industries, Ltd. Lubrifiant pour le traitement de fibre elastique

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JPH11269770A (ja) 1999-10-05
KR100544544B1 (ko) 2006-01-24
IL128388A0 (en) 2000-01-31
HU9900286D0 (en) 1999-04-28
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PL186551B1 (pl) 2004-01-30
KR19990072496A (ko) 1999-09-27
US6391953B1 (en) 2002-05-21
HUP9900286A2 (en) 2003-05-28
TW440632B (en) 2001-06-16
SG82598A1 (en) 2001-08-21
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CO5060553A1 (es) 2001-07-30
AR015229A1 (es) 2001-04-18

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