EP1907621A1 - Substrats textiles a structure d'appret en couche - Google Patents

Substrats textiles a structure d'appret en couche

Info

Publication number
EP1907621A1
EP1907621A1 EP06760528A EP06760528A EP1907621A1 EP 1907621 A1 EP1907621 A1 EP 1907621A1 EP 06760528 A EP06760528 A EP 06760528A EP 06760528 A EP06760528 A EP 06760528A EP 1907621 A1 EP1907621 A1 EP 1907621A1
Authority
EP
European Patent Office
Prior art keywords
agent
finishing treatment
chemical layer
textile substrate
stain release
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Withdrawn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
EP06760528A
Other languages
German (de)
English (en)
Inventor
Yunzhang Wang
Daike Wang
Simon X. Zhang
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.)
Milliken and Co
Original Assignee
Milliken and Co
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
Priority claimed from US11/145,337 external-priority patent/US7485588B2/en
Priority claimed from US11/145,389 external-priority patent/US7407899B2/en
Application filed by Milliken and Co filed Critical Milliken and Co
Publication of EP1907621A1 publication Critical patent/EP1907621A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/04—Processes in which the treating agent is applied in the form of a foam
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/18—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials
    • D06N3/183—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials the layers are one next to the other
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/18—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials
    • D06N3/186—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials one of the layers is on one surface of the fibrous web and the other layer is on the other surface of the fibrous web

Definitions

  • This invention relates to textile substrates to which a finishing treatment has been applied during the manufacturing process.
  • a finishing treatment provides improved water and/or oil repellency and stain and soil resistance.
  • the finishing treatment generally includes a repellent agent, a stain release agent, and a particulate component.
  • Other compounds may be added to the treatment, such as stain-blocking agents, crosslinking agents, coupling agents, antimicrobial agents, and pH adjusting agents.
  • the components of the finishing treatment are generally applied to the textile substrate using an application process that results in layered structures on the surface of the treated substrate, which has been found to greatly improve the durability of the treatment.
  • Such treated textile substrates thus exhibit excellent stain and soil resistance and water and/or oil repellency properties. Furthermore, it has been found that application of such a finishing treatment to the textile substrates is durable and provides improved cleanability to the treated substrates.
  • any significant reduction in either oil or water repellency consequently reduces stain repellency as well.
  • the ability to effectuate proper stain release may likewise be diminished, particularly upon exposure to greater degrees of staining and wherein the surface energy profile needed for proper stain release function (which is similar to that needed to impart the aforementioned water and oil repellency properties) is compromised (e.g., is not wash or abrasion durable).
  • floorcovering articles particularly the pile portion of such articles (e.g., the portion which is designed to be in contact with pedestrians' footwear, such as tufted fibers, cut pile fibers, loop pile fibers, and the like), are highly susceptible to staining, dirt accumulation, liquid spills, and the like.
  • floorcovering manufacturers With pedestrians walking on such surfaces, it has been extremely challenging for floorcovering manufacturers to provide floorcovering articles that resist such attacks and maintain their original appearance after long-term use. Attempts by others to provide finishing treatments to floorcovering articles have included applying fluorochemical compounds to the surface of the article, for example, by spray coating.
  • Figure 1 is a graphical representation of the ratio of fluorine to oxygen as determined by X-ray Photoelectron Spectroscopy (XPS) analysis on treated polyester fabric.
  • XPS X-ray Photoelectron Spectroscopy
  • fluorochemicals may be used interchangeably and each represents polymeric materials containing at least one fluorinated segment, preferably containing -CF 3 groups.
  • fluorocarbons may be used interchangeably and each represents polymeric materials containing at least one fluorinated segment, preferably containing -CF 3 groups.
  • fluoropolymers may be used interchangeably and each represents polymeric materials containing at least one fluorinated segment, preferably containing -CF 3 groups.
  • Fluorochemical generally refers to an organic compound in which some or all of the hydrogen atoms directly attached to the carbon atoms have been replaced by fluorine.
  • Fluorocarbon generally refers to a class of organic compounds, similar to hydrocarbons, in which fluorine atoms replace some or all of the hydrogen atoms.
  • Fluoropolymer generally refers to a polymer composed of linear repeating units in which some or all of the hydrogen atoms are replaced with fluorine.
  • Hydrophilic is generally defined as having a strong affinity for or the ability to absorb water.
  • Hydrophilic is generally defined as lacking affinity for or the ability to absorb water.
  • Water repellency and “oil repellency” are generally defined as the ability of a substrate to block water and oil, respectively, from penetrating into the substrate.
  • the substrate may be a textile substrate which is capable of blocking water and oil from penetrating into the fibers of the textile substrate.
  • a water repellent agent typically refers to a compound that, when applied to a textile substrate, provides a water repellency rating of at least 1.0 when tested by the 3M Water Repellency Test Il (May 1992).
  • a water and oil repellent agent typically refers to a compound that, when applied to a textile substrate, provides a water repellency rating of at least 1.0 when tested by the 3M Water Repellency Test Il (May 1992) and an oil repellency rating of at least 1.0 when tested by AATCC Test Method 118-2000.
  • Stain release is generally defined as the degree to which a stained textile substrate approaches its original, unstained appearance as a result of a care procedure.
  • high levels of stain resistance means an oil repellency rating of at least 3.0 when tested by AATCC Test Method 118 - 2000, a water repellency rating of at least 3.0 when tested by the 3M Water Repellency Test Il (May, 1992), and a spray rating of at least 50 when tested by AATCC Test Method 22-2000.
  • Acceptable stain release as described herein, means a rating for corn oil and mineral oil release of at least 3.0 when tested by modified AATCC Test Method 130 -2000.
  • the term "padding” describes an application process used for application of the finishing treatment to the textile substrate. It generally refers to a process wherein a liquid coating is applied to a textile substrate by passing the substrate through a bath and subsequently through squeeze rollers.
  • floorcovering article is intended to describe a textile substrate which comprises face fibers and which are utilized to cover surfaces on which people are prone to walk.
  • carpets broadloom, tile, or otherwise
  • floor mats outdoor, indoor, and the like are specific types of floorcovering articles.
  • face fiber portion encompasses any standard fibers and composites thereof, which are utilized within floorcovering articles.
  • the face fiber portion may be comprised of monofilament fiber, core-sheath fiber, and the like, or may be present as loop pile, cut pile, or any other type of carpet face.
  • nylon, polyethylene, polypropylene, polyester, cotton, polyvinylacetate, and the like fibers may be tufted through a fabric (such as a woven, non-woven, or knit fabric of any fiber type, such as those listed previously).
  • This fabric segment is generally referred to as the primary backing portion of a floorcovering article.
  • layered structure is intended to describe a structure formed on a textile substrate to which a multi-component finish (i.e. at least two components) has been applied. Two or more components of the multi-component finish, instead of being entirely intermixed together, are substantially separate from each other in a layered arrangement, thus forming a layered structure.
  • the boundary between the layers may be distinct or they may be intermixed.
  • Textile substrates of the current invention may be of any known construction including a knit construction, a woven construction, a nonwoven construction, and the like, or combinations thereof. Textile substrates may have a weight of between about 1 and about 55 ounces/square yard. Textile substrates such as fabrics may more preferably have a weight of between about 2 and about 12 ounces/square yard, whereas textile substrates such as floorcovering articles may more preferably have a weight of between about 20 and about 50 ounces/ square yard.
  • the material of the textile substrate can be synthetic fiber, natural fiber, man-made fiber using natural constituents, inorganic fiber, glass fiber, or a blend of any of the foregoing.
  • synthetic fibers may include polyester, acrylic, polyamide, polyolefin, polyaramid, polyurethane, or blends thereof. More specifically, polyester may include polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, polylactic acid, or combinations thereof.
  • Polyamide may include nylon 6, nylon 6,6, or combinations thereof.
  • Polyolefin may include polypropylene, polyethylene, or combinations thereof.
  • Polyaramid may include poiy-p-phenyleneteraphthalamide (i.e., Kevlar®), poly-m- phenyleneteraphthalamide (i.e., Nomex®), or combinations thereof.
  • Exemplary natural fibers include wool, cotton, linen, ramie, jute, flax, silk, hemp, or blends thereof.
  • Exemplary man-made materials using natural constituents include regenerated cellulose (i.e., rayon), lyocell, or blends thereof.
  • the textile substrate may be formed from staple fiber, filament fiber, slit film fiber, or combinations thereof.
  • the fiber may be exposed to one or more texturing processes.
  • the fiber may then be spun or otherwise combined into yarns, for example, by ring spinning, open-end spinning, air jet spinning, vortex spinning, or combinations thereof.
  • the textile substrate will generally be comprised of interlaced fibers, interlaced yarns, loops, or combinations thereof.
  • the textile substrate may be comprised of fibers or yarns of any size, including microdenier fibers or yarns (fibers or yarns having less than one denier per filament).
  • the fibers or yarns may have deniers that range from less than about 0.1 denier per filament to about 2000 denier per filament or, more preferably, from less than about 1 denier per filament to about 500 denier per filament.
  • the textile substrate may be partially or wholly comprised of multi-component or bi-component fibers or yarns in various configurations such as, for example, islands-in- the-sea, core and sheath, side-by-side, or pie configurations.
  • the fibers or yarns may be splittable along their length by chemical or mechanical action.
  • the fibers comprising the textile substrate may include additives coextruded therein, may be precoated with any number of different materials, including those listed in greater detail below, and/or may be dyed or colored to provide other aesthetic features for the end user with any type of colorant, such as, for example, poly(oxyalkylenated) colorants, as well as pigments, dyes, tints, and the like.
  • additives may also be present on and/or within the target fiber or yarn, including antistatic agents, brightening compounds, nucleating agents, antioxidants, UV stabilizers, fillers, permanent press finishes, softeners, lubricants, curing accelerators, and the like.
  • the textile substrate may be printed or dyed, for example, to create aesthetically pleasing decorative designs on the substrate or to print informational messages on the substrate.
  • the textile substrate may be colored by a variety of dyeing and/or printing techniques, such as high temperature jet dyeing with disperse dyes, thermosol dyeing, pad dyeing, transfer printing, screen printing, digital printing, ink jet printing, flexographic printing, or any other technique that is common in the art for comparable, equivalent, traditional textile products.
  • the fibers or yarns comprising the textile substrate of the current invention may be dyed by suitable methods prior to substrate formation, such as for instance, via package dyeing, solution dyeing, or beam dyeing, or they may be left undyed.
  • the textile substrate may be printed with solvent-based dyes rather than water based dyes
  • a textile substrate composite material may be formed by combining one or more layers of textile substrate together. For example, it may be desirable to combine several layers of an open weave textile substrate together to form a textile substrate composite material.
  • the composite material may also include adhesive material or one or more layers of film.
  • the composite material may then be treated with the chemical composition of the present invention to achieve a material that exhibits durable stain repellency and stain release performance characteristics.
  • the textile substrates comprising the composite material may be treated with the chemical composition before being combined into a composite material.
  • any standard carpet yarn or fiber may be utilized as the substrate for topical treatment thereof within this application.
  • natural (cotton, wool, and the like) or synthetic fibers may constitute the target substrate, either by itself or in any combinations or mixtures of synthetics, naturals, or blends or both types.
  • polyolefins such as polyethylene, polypropylene, and polybutylene
  • halogenated polymers such as polyvinyl chloride
  • polyesters such as polyethylene terephthalate, polyester/polyethers
  • polyamides such as nylon 6 and nylon 6,6, polyurethanes, as well as homopolymers, copolymers, or terpolymers in any combination of such monomers, and the like
  • polyamide fibers are commonly used to create floorcovering articles because of their strength, flexibility, toughness, elasticity, abrasion resistance, washability, ease of drying, and resistance to attack by microorganisms.
  • the floorcovering articles may be manufactured according to a variety of standard processes known to those skilled in the art. Generally, prior to integration with any other components, the face fiber portion is sewn, tufted, needled, and the like, through the primary backing fabric to form a composite which can then be simply adhered to a further portion. Alternatively, the primary backing fabric may be contacted with a secondary backing fabric and the face fiber portion may then be created by needling, etc., through the primary backing fabric. Examples of carpet and carpet tile production are disclosed within U.S. Patent Nos. 5,929,145 to Higgins et al.; 5,948,500 to Higgins et al.; 5,545,276 to Higgins et al.; and 5,540,968 to Higgins etal. Examples of floor mat production are present within U.S. Patent Nos. 5,902,662 to Kerr; 5,928,446 to Kerr et al.; and 5,305,565 to Nagahama et al. Finishing Treatment
  • the finishing treatment useful for rendering a textile substrate with improved stain and soil resistance and water and/or oil repellency is typically comprised of a repellent agent, a stain release agent and a particulate component. It has been unexpectedly discovered that superior water and oil repellency and stain release is achieved when the finishing treatment is applied using a process comprising at least two steps such that the components of the finishing treatment are layered on the textile substrate. Generally, these unexpected results are achieved by applying a first layer of chemicals comprising a repellent agent to the textile substrate and then subsequently applying a second layer of chemicals to the first layer.
  • the second layer of chemicals includes a stain release agent or both a repellent agent and a stain release agent.
  • a particulate component may be added to the chemical mixture of either the first layer, the second layer, or both layers. It is believed that these results are unexpected because one having ordinary skill in the art would not expect that after application of a water and oil repellent layer to a textile substrate that one could then add a stain-releasing layer of chemistry that would adhere to this first repellent layer and would not compromise the repellent properties of the first repellent layer. However, it has been found, through the use of certain processing steps, that such an arrangement can be achieved and that the resulting treated substrate exhibits improved repellency, stain release, and soil resistance characteristics.
  • additives may be included in the treatment in order to impart various desirable attributes to the textile substrate. These include, without limitation, stain-blocking agents, crosslinking agents, coupling agents, antimicrobial agents, and pH adjusting agents.
  • Chemical components may be optimized to achieve the desired level of performance for different target applications within a single finishing treatment. Further, the relative ratio of each component to the other components may vary depending upon the target application.
  • Water repellent agents typically include waxes, silicones, certain hydrophobic resins, and the like, or combinations thereof.
  • Compounds which generally provide both water and oil repellency to a textile substrate include fluorochemicals.
  • repellent fluorochemicals useful in the present invention include any of the fluorochemical compounds and polymers known in the art to impart dry soil resistance and water- and oil-repellency to fibrous substrates.
  • These repellent fluorochemical compounds and polymers typically comprise one or more fluorochemical radicals that contain a perfluorinated carbon chain having from about 3 to about 20 carbon atoms, more preferably from about 6 to about 14 carbon atoms.
  • These fluorochemical radicals can contain straight chain, branched chain, or cyclic fluorinated allcylene groups, or any combination thereof.
  • the fluorochemical radicals are preferably free of polymerizable olefinic unsaturation but can optionally contain catenary heteroatoms such as oxygen, divalent or hexavalent sulfur, or nitrogen. Fully fluorinated radicals are preferred, but hydrogen or chlorine atoms may also be present as substituents, although, preferably, no more than one atom of either is present for every two carbon atoms. It is additionally preferred that any fluorochemical radical contain from about 40% to about 80% fluorine by weight, and more preferably, from about 50% to about 78% fluorine by weight.
  • the terminal portion of the radical is preferably fully fluorinated, preferably containing at least 7 fluorine atoms, e.g., CF 3 CF 2 CF 2 -, (CF 3 ) 2 CF-, and CF 5 CF 2 — .
  • Perfluorinated aliphatic groups i.e., those of the formula C n F 2n+1 - are the most preferred fluorochemical radical embodiments.
  • Representative repellent fluorochemical compounds useful in finishing treatment of the present invention include, without limitation, fluorochemical urethanes, ureas, esters, ethers, alcohols, epoxides, allophanates, amides, amines (and salts thereof), acids (and salts thereof), carbodiimides, guanidines, oxazolidinones, isocyanurates, and biurets. Blends of these compounds are also considered useful.
  • fluorochemical polymers useful in treatments in the present invention include fluorochemical acrylate and substituted acrylate homopolymers or copolymers containing fluorochemical acrylate monomers interpolymerized with monomers free of non-vinylic fluorine such as methyl methacrylate, butyl acrylate, acrylate and methacrylate esters of oxyalkylene and polyoxyalkylene polyol oligomers (e.g., oxyethylene glycol dimethacrylate, polyoxyethylene glycol dimethacrylate, methoxy acrylate, and polyoxyethylene acrylate), glycidyl methacrylate, ethylene, butadiene, styrene, isoprene, chloroprene, vinyl acetate, vinyl chloride, vinylidene chloride, vinylidene fluoride, acrylonitrile, vinyl chloroacetate, vinylpyridine, vinyl alkyl ethers, vinyl alkyl ketones, acrylic acid, methacrylic acid
  • the relative amounts of various non-vinylic fluorine-free comonomers used are generally selected empirically depending on the textile substrate to be treated, the properties desired, and the mode of application onto the textile substrate.
  • Useful fluorochemical treatments also include blends of the various repellent fluorochemical polymers described above as well as blends of the aforementioned fluorochemical compounds with these repellent fluorochemical polymers.
  • water and oil repellent fluorochemicals that can be used in conjunction with the current invention include, but are not limited to, the ScotchgardTM family of repellent fluorochemicals by 3M, the ZonylTM family of repellent fluorochemicals by Dupont, the RepearlTM family of repellent fluorochemicals by Mitsubishi International Corporation. Repearl® F-8025, Repearl F-7105, and Repearl F-7000 by Mitsubishi are particularly useful in the practice of the current invention.
  • Other fluorochemicals such as the UnidyneTM products distributed by Daikin America, Inc. or products distributed by OMNOVA Solutions may also be employed. Fluorochemical based water and oil repellent agents may be preferred for use in the present invention.
  • a stain release agent is generally a compound that assists in the release of stains that are present on, or are present within, a textile substrate that has been treated with a stain release agent.
  • the stain release agent may be a fluorochemical based compound, or it may be non-fluorochemical based compound.
  • Fluorochemical based stain release agents generally comprise fluorinated stain release fluoropolymers. Many of these types of stain release agents are hybrid polymeric materials that have oleophobic and hydrophilic moieties combined in a copolymer so that the respective moieties have mobility under various conditions of temperature and environment. The chemistry of these materials is taught in numerous patents, for example, US Patent No. 3,574,791 to Sherman et al. and US Patent No. 3,944,527 to McCown. Exemplary oleophobic fluorochemical parts of the hybrid polymeric material are described in these patents.
  • the hydrophilic groups include, but are not limited to, alkoxylates, especially ethoxylates; and carboxyl, hydroxyl, sulfonate, sulfate, phosphate and phosphonate groups.
  • fluorochemical based stain release component examples include Unidyne® TG- 992 and Unidyne® TG-993, both available from Daikin Corp., Repearl® SR1100, available from Mitsubishi Corp., as well as Zonyl® 7910, available from DuPont.
  • non-fluorochemical based stain release agents include ethoxylated polyesters, sulfonated polyesters, ethoxylated nylons, carboxylated acrylics, cellulose ethers or esters, hydrolyzed polymaleic anhydride polymers, polyvinylalcohol polymers, polyacrylamide polymers, ethoxylated silicone polymers, polyoxyethylene polymers, polyoxyethylene- polyoxypropylene copolymers, and the like, or combinations thereof.
  • the stain release agent may be a blend of a non-fluorochemical based hydrophilic agent and a fluorochemical repellent agent as described above and as taught in commonly owned US Patent No. 6,818,253 to Kimbrell.
  • Fluorochemical based stain release agents may be preferred stain release agents.
  • Fluorochemical based stain release agents comprised of hybrid oleophobic and hydrophilic moieties may be most preferred.
  • particulate materials inorganic or organic, may be used in conjunction with the present invention.
  • the particulate component increases the repellency of the textile substrate and may even act synergistically with a repellent agent to improve repellency upon application of both materials to a textile substrate.
  • the particulate component may also provide other functions to the treated textile substrate, such as soil resistance, ultraviolet stability, abrasion resistance, etc.
  • the particles are comprised of at least one material selected from the group consisting of silicates, doped silicates, minerals, silicas, polymers, carbon, graphite, metal salts, metal powders, silica-coated metal powders, inorganic oxides (such as metal oxides), and the like, and combinations thereof. More specifically, examples of particles that may be employed include, but are not limited to, silica, colloidal silica, alumina, zirconia, titania, zinc oxide, precipitated calcium carbonate, polytetrafluoroethylene (PTFE), perfluorinated copolymers, copolymers with tetrafluoroethylene, polyvinylpyrrolidone (PVP), and the like. Such particles can also be surface modified, for instance by grafting.
  • PTFE polytetrafluoroethylene
  • PVP polyvinylpyrrolidone
  • the size of the selected particles should be taken into consideration for several reasons.
  • Particles that are too small may not provide appropriate surface roughness to trap air on the substrate surface or may require high loading with subsequent agglomeration to achieve the desired effect. Particles that are too large may give a frosty, white appearance to dyed textiles or may be removed easily during use or routine maintenance of the textile substrate.
  • particle sizes of between about 1 nm and about 50 ⁇ m are believed to be capable of providing good results in various applications of the invention.
  • Particle sizes in the range of between about 5 nm and about 1 ⁇ m are particularly useful, and particle sizes in the range of between about 10 nm and about 50 nm have been found to work well in some applications.
  • the terms "inorganic oxide” or “metal oxide” refer to a general class of materials comprising at least one species of metal cation combined with oxygen anions or hydroxyl anions, or mixtures of oxygen and hydroxyl ions.
  • This material can additionally contain water in bound or adsorbed form and can further comprise small amounts, for example less than 5% by weight, stabilized counter ions such as sodium ion, carboxylate ion, chloride ion, nitrate ion, or the like.
  • stabilized counter ions such as sodium ion, carboxylate ion, chloride ion, nitrate ion, or the like.
  • the sol has a pH of 9, an average particle size of 20 nm in diameter;
  • the sol has a pH of 9, an average particle size of 5 nm in diameter;
  • the sol has a pH of 9, an average particle size of 20 nm in diameter.
  • the sol has a pH of 9, an average particle size of 75 nm in diameter;
  • Nalco 1056TM Aluminized Silica-a 30% by weight solids aqueous colloidal suspension of aluminized silica particles (26% silica and 4% alumina) available commercially from Nalco;
  • the dispersion has a pH of 9.5, and an average agglomerated primary particle size of about 100 nm in diameter;
  • the dispersion has an average particle size of about 100nm in diameter;
  • the sol has a pH of 9, an average particle size of 22 nm in diameter;
  • the sol has a pH of 9, an average particle size of 12 nm in diameter;
  • Ludox® CL-P Colloidal Alumina Coated Silica a 40% by weight solids aqueous sol, available from Grace Davison.
  • the sol has a pH of 4, an average particle size of 22 nm in diameter;
  • Ludox® CL Colloidal Alumina Coated Silica a 30% by weight solids aqueous sol, available from Grace Davison.
  • the sol has a pH of 4.5, an average particle size of 12 nm in diameter;
  • Ludox® TMA Colloidal Silica - a 34% by weight solids aqueous colloidal silica sol available from Grace Davison.
  • the sol has a pH of 4.7 and an average particle size of 22 nm in diameter;
  • Ludox SM Colloidal Silica - a 30% by weight solids aqueous dispersion available from Grace Davison. It has an average particle size of about 20nm in diameter;
  • Aerosil® R7200 Hydrophobic Fumed Silica available from Degussa Corporation of Germany.
  • the material has an average pH of 5.5 and an average particle size of approximately 12 nm in diameter;
  • Aeroxide® AIu C Hydrophilic Fumed Alumina Oxide available from Degussa Corporation of Germany.
  • the material has an average pH of 5 and an average particle size of 13 nm in diameter;
  • the average aggregated particle size is 4.5 Dm in diameter;
  • the average aggregated particle size is 4.5 Dm in diameter;
  • particles having other functional properties may be used. Such particles may provide additional attributes beyond the structural building feature described herein.
  • AlphaSan® antimicrobial particles available from Milliken & Company of
  • Spartanburg, South Carolina, may provide antimicrobial features to the textile substrate.
  • Zinc oxide particles may offer odor-absorbing properties.
  • ZelecTM particles also available from Milliken & Company, may provide antistatic properties.
  • Zinc borate particles or antimony pentoxide may provide flame retardant and fungicide properties.
  • Iron-based microparticles may provide magnetic and microwave-absorbing properties.
  • Stain-Blocking Agents One class of stain-blocking agents suitable for this invention includes anionic surfactants having a relatively low molecular weight (MW in the range of 500 to 50,000) and containing sulfonic groups that react with nylon under low pH conditions.
  • suitable stain- blocking agents are sold by Minnesota Mining and Manufacturing Company (3M) of St. Paul, Minnesota, under the tradename Stainblocker FC661 and by Milliken & Company of Spartanburg, South Carolina, under the tradenames FS2 and FS7.
  • crosslinking agents may be suitable for incorporation into the finishing treatment of the present invention.
  • One group of crosslinking agents includes hydrophobic crosslinking agents.
  • Hydrophobic crosslinking agents include those crosslinking agents which are insoluble in water. More specifically, hydrophobic crosslinking agents may include monomers containing blocked isocyanates (such as blocked diisocyanates), polymers containing blocked isocyanates (such as blocked diisocyanates), epoxy containing compounds, and the like, or combinations thereof. Diisocyanate containing monomers or diisocyanate containing polymers may be the preferred crosslinking agents. However, monomers or polymers containing two or more blocked isocyanate compounds may be the most preferred crosslinking agents.
  • Repearl® MF also available from Mitsubishi Corp.
  • Others include Arkophob® DAN, available from Clariant, Epi-Rez® 5003 W55, available from Shell, and Hydrophobol® XAN, available from Dupont, and Milliguard® MRX, available from Milliken & Company.
  • Coupling agents are generally used to provide a stable bond between organic polymer compounds and inorganic materials, which would otherwise be incompatible.
  • One non- limiting class of coupling agents includes silane-containing coupling agents.
  • Silane coupling agents are a class of organofunctional silanes that have the generic structure: Y-R-Si-X 3 , where X is a hydrolysable group such as methoxy, ethoxy, or acetoxy, and Y is an organofunctional group attached to silicon by an alkyl bridge, R. Examples of the Y groups are vinyl, epoxy, amino, ureido, mercapto, methacrylate, and the like.
  • Silane coupling agents are generally used for coupling inorganic particulate materials to organic resins.
  • the Y component then allows for reaction to a variety of resin systems.
  • silane coupling agents include the Silquest® A- series of silanes available from GE silicones-OSi Specialties and the Dow Corning Z- series of silanes available from Dow Coming.
  • attributes other than durable stain and soil resistance, stain release, and repellency are desirable.
  • attributes include static protection, wrinkle resistance, shrinkage reduction or elimination, desirable hand (or feel) requirements, dyefastness requirements, odor control, flammability requirements, and the like.
  • antimicrobial agents such as antimicrobial agents, antibacterial agents, antifungal agents, flame retardants, UV inhibitors, antioxidants, coloring agents, lubricants, thickeners, durable press resins (such as dimethyloldihydroxyethyleneurea), other types of resins (such as Kymene 450), catalysts (such as Catalyst 531 ), antistatic agents, fragrances, and the like, or combinations thereof.
  • antimicrobial and/or antifungal agents may be utilized in order to inhibit microbial and/or fungal growth and even to help control odor.
  • antimicrobial and/or antifungal agents examples include colloidal silver; AlphaSan® RC-5000 and AlphaSan® RC-2000 (both available from Milliken & Company); Ultrafresh NM, Ultrafresh DM-50, and Ultrafresh DM-25 (all available from Thompson Associates); Chitosante (available from VAG Bioscience); Kathon LM (available from Rohm and Haas); Reputex (available from Avecia); AM 5700 (available from Dow Corning); Amical 48 (available from Dow Chemical); zinc omadine (available from Arch Chemicals, Inc.); and combinations thereof.
  • Potentially preferred are the AlphaSan® antimicrobial products and zinc omadine.
  • the textile substrate may also be treated by mechanical finishing techniques.
  • mechanical treatment such as calendering, embossing, etching, rainbow or hologram embossing, film or metal foil hologram embossing, fabric metallization, heat setting, hydroentanglementwith water or air, sanforizing, glazing, schreinering, sueding, sanding, emorizing, napping, shearing, tigering, decating, fabric patterning through the use of water, air, laser, or patterned rolls, and the like, or combinations thereof.
  • mechanical treatments typically provide desirable effects to the textile substrate which affect such properties as the appearance, strength, and/or hand of the fabric.
  • advantages may be obtained by treatment either before or after the finishing treatment of the current invention is applied.
  • benefits from sanding prior to application of the finishing treatment and calendaring after application of the finishing treatment may be envisioned.
  • bleach resistance agents include, without limitation, bleach resistance agents, color safe agents, foaming agents, and the like.
  • bleach resistant formulations are preferably aqueous in nature (although short-chain alcohols, such as methanol, ethanol, isopropanol, and the like, may also be utilized as the solvent therein) and may be in the form of a shampoo, coating, spray, atomized dispersion, and the like.
  • Foaming agents may include any of various anionic or nonionic surfactants, including, without limitation, fatty aryl-sulfonates, -phosphates (preferably dodecylbenzenesulfonic acid), ethoxylated fatty alcohols (preferably Syn Lube® 728 from Milliken & Company), coconut oil, and the like, and mixtures thereof.
  • anionic or nonionic surfactants including, without limitation, fatty aryl-sulfonates, -phosphates (preferably dodecylbenzenesulfonic acid), ethoxylated fatty alcohols (preferably Syn Lube® 728 from Milliken & Company), coconut oil, and the like, and mixtures thereof.
  • the total amount of the finishing treatment applied to the textile substrate may vary over a wide range.
  • the total amount of finishing treatment applied to the textile substrate will depend generally on the composition of the article, the level of durability required for a given end-use application, and the cost of the chemical composition.
  • the total amount of chemical solids applied to the textile substrate will be found in the range of about 0.25% to about 10.0% on weight of the textile substrate. More preferably, the total amount of chemical solids applied to the substrate may be found in the range of about 0.5% to about 5.0% on weight of the substrate.
  • Typical solids proportions and concentration ratios of repellent agent to stain release agent may be found in the range of about 10 : 1 and about 1 : 10, including all proportions and ratios that may be found within this range.
  • solids proportions and concentration ratios of repellent agent to stain release agent may be found in the range of about 5 : 1 and about 1 : 5.
  • the total amount of particulate component applied to the textile substrate is preferably less than about 10% on weight of the textile substrate.
  • the ratio of repellent agent to stain release agent to crosslinking agent may be found in the range of about 10 : 1 : 0.1 and about 1 : 10 : 5, including all proportions and ratios that may be found within this range.
  • solids proportions and concentration ratios of repellent agent to stain release agent to particulate component may be found in the range of about 5 : 1 : 0.1 and about 1 : 5 : 2.
  • the proportion of repellent agent to stain release agent and the amount of particulate component applied to the textile substrate may likewise be varied based on the relative importance of each property being modified. For example, higher levels of repellency may be required for a given end-use application. As a result, the amount of repellency agent, relative to the amount of stain release agent, may be increased. Alternatively, higher levels of stain release may be deemed more important than high levels of stain repellency. In this instance, the amount of stain release agent may be increased, relative to the amount of stain repellency agent. The amount of particulate component may be adjusted accordingly.
  • the type of repellent agent, stain release agent, and particulate component may be varied based on the end-use of the treated textile substrate.
  • a treated floorcovering article may be produced that is not expected to encounter oil based stains.
  • more economical repellency agents, such as silicones may be utilized as one component of the finishing treatment.
  • finishing treatment to the textile substrate may be accomplished by a variety of application methods which include, without limitation, spraying, foaming, padding, steaming, or by any other technique whereby one can apply a controlled amount of a liquid suspension to a textile substrate. Employing one or more of these application techniques may allow the finishing treatment to be applied to the textile substrate in a uniform manner.
  • the finishing treatment is generally applied to the textile substrate using a multi-layered application process.
  • the first step of the process involves the application of a first chemical composition comprising a repellent agent to the substrate. This method of application generally results in the first chemical layer being proximal to or contiguous with the surface of the textile substrate. This structural layering effect is demonstrated in Figure 1.
  • the textile substrate may then be exposed to a controlled drying step, in order to evaporate the desired amount of liquid from the substrate leaving the solid active components on the surface of the treated substrate. Drying can be accomplished by any technique typically used in manufacturing operations, such as dry heat from a tenterframe, microwave energy, infrared heating, steam, superheated steam, autoclaving, or the like, or any combination thereof. Alternatively, the textile substrate may not be exposed to a drying step in which case, the substrate will generally remain wet for step two of the application process.
  • the second step of the process involves the application of a second chemical composition comprising a stain release agent or both a repellent agent and a stain release agent.
  • the repellent agent may be the same or it may be different from the repellent agent applied in the first step of the application process.
  • the second chemical composition may be applied simultaneously with or sequentially to the first chemical layer, for example, by spraying, foaming, or padding techniques. This method of application generally results in the second chemical layer being proximal to or contiguous with the first chemical layer on the surface of the textile substrate. This structural layering effect is demonstrated in Figure 1.
  • the treated substrate After application of the finishing treatment to the textile substrate, the treated substrate is generally exposed to a drying step to evaporate excess liquid, leaving the solid active components on the surface of the treated substrate. Additionally, it may be desirable to expose the treated substrate to an additional heating step to further enhance the performance or durability of the chemical agents. This step may be referred to as a curing step.
  • additional heating may (a) enable certain discreet particles of the active components of the chemical agents to melt-flow together, resulting in uniform, cohesive film layers; (b) induce preferred alignment of certain segments of the chemical agents; (c) induce crosslinking reactions between the chemical agents or between the chemical agents and the substrate; or (d) combinations thereof. Description of the Preferred Embodiments
  • test sample was placed on a flat, horizontal surface. 3 small drops of the test liquid, approximately 5 mm in diameter, were placed gently in three different areas on the test sample using a dropper or pipette. The drops were allowed to stand undisturbed for 10 seconds. If after 10 seconds, two of the three drops are still visible as spherical to hemispherical, the sample passes the test.
  • the reported water repellency rating corresponds to the highest IPA containing blend for which the treated substrate passes the test.
  • Water repellency forfloorcovering textile substrates was tested according to the 3M Water Repellency Test V (February, 1994).
  • the rating scale of 0 - 10 is the same as that described in "a" above with regard to water repellency for fabric textile substrates.
  • the reported water repellency rating corresponds to the highest IPA-containing blend that resulted in a pass designation for the treated floorcovering substrate.
  • Oil Repellency for fabric textile substrates was tested according to the AATCC (American Association of Textile Chemists and Colorists) Test Method 118-2000.
  • the rating scale is 0 - 8, with "0" indicating the poorest degree of repellency (substrates having higher surface energy) and "8” indicating the best degree of repellency (substrates having lower surface energy).
  • the oil repellency scale is:
  • test sample was placed on a flat, horizontal surface. Beginning with the lowest numbered test liquid, a small drop of the test liquid, approximately 5 mm in diameter, was placed gently in several different areas on the test sample using a dropper or pipette. The drops were allowed to stand undisturbed for 30 seconds and observe the drop at a 45° angle. If after 30 seconds, no penetration or wetting of the sample substrate at the liquid-substrate interface and no wicking around the drop occurs, the sample passes the test. The numerical Oil Repellency Rating given to the sample is the highest numbered test liquid which will not wet the substrate within a period of 30 seconds.
  • Oil repellency for floorcovering articles which have pile surfaces is the same as that described above in "c" for fabric textile substrates, except for the following modifications:
  • the Spray Rating Test was conducted in accordance with AATCC Test Method 22-2000.
  • the rating scale is as follows:
  • the Martindale Abrasion Test was performed according to ASTM D4966-98 modified using a Mark III Abrasion Tester BS5690 (Shirley Developments Ltd.). A 7 inch x 7 inch sample was mounted onto the test station. A woven wool fabric, which was placed on the abrasion cylinder (with a 12 kpa weight), was used as the abrasive material. The sample was then exposed to a pre-determined number of abrasion cycles.
  • the Stain Release Test procedure used here is a modification of AATCC Method 130-2000 such that a spot removal method was used to clean the stains instead of a laundering process.
  • Stains such as corn oil (CO), burned motor oil (BMO), ketchup, mustard are applied to a test fabric according to the AATCC Method 130.
  • the stained fabric was set aside for 24 hours at 70 +/- 2 degrees F and 65 +/- 2% RH before cleaning.
  • the following procedures were used to spot clean the stains:
  • This test method describes a procedure for the accelerated soiling of carpets. It can be used to compare the soiling propensity of two or more carpets, or it can be used to soil carpets as a preliminary step in measuring either the ability of a carpet to be cleaned or the efficiency of a cleaning process.
  • This accelerated carpet soiling method has been found to give results similar to floor service soiling, but its use is recommended only as a screening method and not as a replacement for floor testing.
  • the synthetic soil (available from Textile Innovators) is composed of the following components: 38% peatmoss, 17% kaolin, 17% portland cement, 17% silica, 1.75% carbon black, 0.5% red iron oxide, 8.75% mineral oil (medical grade).
  • Soiling levels are predetermined on an arbitrarily selected carpet (control sample) soiled to give light, medium and heavy degrees of soil preferably by exposure to a service soiling test (5.0 grams of soil was used for each test). Soiling times in the ball mill are determined by soiling unsoiled specimens of the control sample to match the levels of soiling established with soiled control specimens. The carpet specimens under evaluation are soiled for 1 minute.
  • the soiling procedure is as follows:
  • the three L * , a * , b* color coordinates of the soiled carpet samples may be measured using a Minolta 310 Chroma Meter with a D65 illumination source.
  • the color difference value, ⁇ Ecmc, of each soiled carpet sample is calculated relative to its unsoiled counterpart.
  • This ⁇ Ecmc measurement is in accordance with industry procedures, as set forth for example in US Patent No. 5,908,663 to Wang et al.
  • the ⁇ Ecmc values calculated from these colorimetric measurements have been shown by others to be qualitatively in agreement with values from previously used visual evaluations such as the soiling evaluation suggested by the AATCC.
  • ⁇ Ecmc values have the additional advantages of higher precision, and they are largely unaffected by environment variations or operator subjectivities.
  • the color shade differential is provided below as ⁇ Ecmc, and the larger the number reported below corresponds to poor soil removal.
  • ⁇ Ecmc means that the unsoiled and soiled textile articles are closer in color shade, and therefore, more soil has been removed.
  • ⁇ Ecmc will be different depending on the color or pattern of the carpet and the color or amount of the soil used. Light colors will show greater color change after soiling with a dark soil. Therefore, the value given in the specification and claims much be adjusted from the values given for white carpet, if another carpet color or pattern is evaluated.
  • AATCC Test Method 171-2000 was used to determine stain release for the floorcovering substrates, with the exceptions described below:
  • test sample Place the test sample flat on a smooth, horizontal surface. Then 10 drops of red Kool-Aid stain are applied to the test sample and rubbed into the carpet for 30 seconds with a circular motion of a gloved finger. The stains are allowed to dry overnight (approximately 16 hours).
  • a piece of fabric was immersed into a bath containing the chemical composition comprising the desired chemical agents.
  • the fabric was removed from the treatment bath and run between squeeze rolls at a desired pressure to obtain a uniform pickup generally between about 30 and about 100%.
  • the fabric was pulled taut and pinned to a frame to retain the desired dimensions.
  • the pinned fabric was either put in a Dispatch oven or run through a tenter at a temperature of between about 300 and about 380 degrees F for between about 0.5 and 10 minutes to dry and to cure the finish.
  • a piece of fabric was immersed into a first bath containing the chemical composition comprising the desired chemical agents.
  • the fabric was removed from the treatment bath and run between squeeze rolls at a desired pressure to obtain a uniform pickup generally between about 30 and about 100%.
  • the fabric was pulled taut and pinned to a frame to retain the desired dimensions.
  • the pinned fabric was either put in a Dispatch oven or run through a tenter at a temperature of between about 300 and about 380 degrees F for between about 0.5 and 10 minutes to dry and to cure the finish.
  • Multi-layer floorcovering application procedure includes the following steps:
  • the treated textile substrates were tested for water and oil repellency, spray rating, and stain release according to the methods described previously for the as-received samples. These test results are provided in Table 1.
  • the treated textile substrates were also tested for water and oil repellency, spray rating, and stain release after 10000 cycles of Martindale abrasion (with 12kpa weight). These test results are provided in Table 2.
  • the treated floorcovering articles were tested for dry soil resistance, carpet cleanability, and water and oil repellency according to the methods described previously for floorcovering substrates.
  • N/A indicates that a given sample was not tested for a particular parameter.
  • a woven 100% polyester fabric (approximately 8 oz/yd 2 ) was obtained from Milliken & Company of Spartanburg, South Carolina. The fabric was woven, using 2 ply 150 filament textured polyester yarns in each the warp and filling, to provide a fabric having approximately 60 ends per inch and 45 pick per inch.
  • the woven fabric was treated according to the multi-layer pad/pad application procedure described previously.
  • the first chemical bath contained the following components:
  • Milliguard® MRX 1 an isocyanate-containing crosslinking agent available from Milliken & Company.
  • the second chemical bath contained the following components:
  • Aerosil® R7200 hydrophobic fumed silica particles available from Degussa Corporation of Germany.
  • AlphaSan® RC5000 a silver based antimicrobial agent available from Milliken & Company.
  • the squeeze roll pressures were set to achieve a total wet pick up of approximately 100%.
  • the treated fabric was dried and cured in a tenter at 325 degrees F for approximately 5 minutes.
  • Example 1 was repeated except that the 100% woven polyester fabric was replaced by a polyester double needle bar knit fabric (approximately 12 oz/yd 2 ) obtained from Milliken & Company.
  • Example 1 was repeated except that the second chemical bath contained the following components:
  • Example 3 was repeated except that the 100% woven polyester fabric was replaced by a polyester double needle bar knit fabric (approximately 12 oz/yd 2 ) obtained from Milliken & Company.
  • the fabric was removed from the treatment bath and run between squeeze rolls at 40 psi to obtain a uniform pickup of about 60%.
  • the fabric was again run between squeeze rolls at 40 psi and pulled taut and pinned to a frame and dried in a Dispatch oven at 350 degrees F for 5 minutes to cure the finish.
  • Example 1 100% woven polyester fabric described in Example 1 was treated according to the one- step pad application procedure as described previously.
  • the chemical bath contained the following components:
  • the squeeze roll pressures were set to achieve a wet pick up of approximately 100%.
  • the treated fabric was dried and cured in a dispatch oven at 325 degrees F for approximately 5 minutes.
  • Comparative Example 2 Comparative Example 1 was repeated except that the 100% woven polyester fabric was replaced by the polyester double needle bar knit fabric (approximately 12 oz/yd 2 ).
  • Example 1 100% woven polyester fabric described in Example 1 was treated according to the one- step pad application procedure as described previously.
  • the chemical bath contained the following components:
  • the squeeze roll pressures were set to achieve a wet pick up of approximately 100%.
  • the treated fabric was dried and cured in a dispatch oven at 325 degrees F for approximately 5 minutes.
  • Comparative Example 3 was repeated except that the 100% woven polyester fabric was replaced by the polyester double needle bar knit fabric (approximately 12 oz/yd 2 ).
  • Example 5 The 100% woven polyester fabric used in Example 5 was treated according to the one-step pad application procedure as described previously.
  • the chemical bath contained the following components:
  • the squeeze roll pressures were set to achieve a wet pick up of approximately 60%.
  • the treated fabric was dried and cured in a dispatch oven at 350 degrees F for approximately 5 minutes.
  • Tables 1 and 2 illustrates the advantage of applying the finishing treatment using a multi-layer application process.
  • Table 1 clearly shows that improved repellency and stain release is unexpectedly achieved by applying a first layer comprised of a repellent agent followed by a second layer comprised of a repellent agent and a stain release agent.
  • the results in Table 2 show that the finishing treatment is durable to abrasion.
  • Example 5 In order to demonstrate the formation of layered structures on the textile substrate, the polyester fabric used in Example 5 and Comparative Example 5 was treated according to the multi-layer pad/pad application procedure, with the following modifications described below.
  • a piece of fabric was immersed into a first chemical bath containing the following chemicals:
  • the fabric was removed from the treatment bath and run between squeeze rolls at 40 psi to obtain a uniform pickup of about 60%.
  • the fabric was again run between squeeze rolls at 40 psi and pulled taut and pinned to a frame and dried in a Dispatch oven at 350 degrees F for 5 minutes to cure the finish.
  • the sputter-profile XPS analysis clearly demonstrates the formation of layered structure in the surface treatment.
  • the F/O ratio is high at the very outer surface of the treated fabric due to the existence of a large number of -CF3 groups that are present in the second chemical layer, which is comprised of the stain release agent.
  • the F/O ratio decreases as the profile analysis moves from the outer surface of the treated fabric inward to the second chemical layer. This decrease is believed to be due to the existence of ethylene oxide segments in the stain release agent.
  • the F/O ratio begins to increase again at the interface between the second chemical layer and the first chemical layer, which is comprised of the repellent agent.
  • the F/O ratio continues to increase as the profile analysis moves through the second chemical layer. This increase is believed to be due to the lack of ethylene oxide segments in the repellent agent.
  • the F/O ratio diminishes as the polyester fiber is reached.
  • An 18 inch by 18 inch piece of white broadloom carpet comprised of nylon 6,6 fiber and having a cut pile construction and a weight of 32 ounces per square yard was obtained from Milliken & Company.
  • the carpet was treated according to the multi-layer floorcovering application procedure described above using the chemical agents listed below.
  • FC661 a stain-blocking agent commercially available as "3M Brand Stain Release Concentrate" which contains a 29.5% aqueous solution comprising a blend of sulfonated novalak and acrylic resins;
  • Ludox SM a colloidal silica available from Grace Davison
  • Milliguard DXG a hydrophilic fluorinated stain release agent available from Milliken & Company comprised of approximately 30% fluoroakyl acrylate copolymer solids.
  • the carpet was dried at a temperature of 350F in zone 1 and 320F in zone 2 of the range for a total of approximately 5 minutes.
  • the face fiber portion of the carpet was then sheared using a shearing machine.
  • the Dry Soil Resistance Rating ⁇ Ecmc of the treated carpet is 24.16.
  • the ⁇ Ecmc for the untreated white control is 40.14.
  • the carpet cleanability of the treated carpet is 5.0.
  • the water repellency and oil repellency ratings of the treated carpet are 4.0 and 4.0, respectively. Comparative Example 7
  • Example 7 The same carpet as described in Example 7 was treated according to the multi-layer floorcovering application procedure described above, except that no BK96 repellent agent was added in the first chemical mix described in step #2 of the application procedure and 2.0% of BK96 was added in the second chemical mix.
  • the Dry Soil Resistance Rating ⁇ Ecmc of the treated carpet is 25.37.
  • the ⁇ Ecmc for the untreated white control is 40.14.
  • the Carpet Cleanability of the treated carpet is 5.0.
  • the Water Repellency and Oil Repellency ratings of the treated carpet are 2.0 and 3.0, respectively.
  • Example 7 and Comparative Example 7 illustrate the improved repellency, stain release, and soil resistance achieved using the multi-layer floorcovering application procedure wherein a repellent agent is applied in the first chemical layer.
  • step of steaming significantly improves the fluorochemical penetration into the center of the yarn bundle and to the bottom of the carpet yarn bundle.
  • the combination of layering the chemicals in a specific arrangement and the step of steaming the floorcovering article significantly improves the water and oil repellency, stain release, and soil resistance of the treated floorcovering articles. This combination also significantly improves the wear durability and cleaning durability of the fluorochemical finish which results in extended lifetime performance of the floorcovering article.
  • the treated textile substrate of the present invention has many applicable end- uses.
  • the treated textile substrate may be ideally suited for use in upholstery applications such as for automotive upholstery, commercial upholstery, and residential upholstery.
  • Other desirable end-uses include treated floorcovering articles (such as carpets and rugs) and outdoor fabrics (such as automobile convertible top fabrics, outdoor furniture fabrics and coverings, awnings, boat covers, and grill covers).
  • the treated textile substrate may be incorporated into articles of apparel such as outerwear (e.g., rainwear), workwear (e.g., uniforms), sportswear, activewear, and fashion apparel (e.g., shirts, pants, and other garments).

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  • Engineering & Computer Science (AREA)
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  • Chemical & Material Sciences (AREA)
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Abstract

L'invention concerne des substrate textiles auxquels on a appliqué un traitement d'apprêt pendant le processus de fabrication. Ce traitement d'apprêt confère des propriétés hydrofuges et/ou oléofuges et une résistance aux taches et à la salissure. Améliorées. Ledit traitement d'apprêt met généralement en oeuvre un agent répulsif, un agent de détachage et un composant particulaire. D'autres composés, tels que des agents antitaches, des agents de réticulation, des agents de couplage, des agents antimicrobiens et des agents de réglage du pH, peuvent être ajoutés au traitement. Les composants du traitement d'apprêt sont généralement appliqués au substrat textile au moyen d'un procédé d'application qui permet d'obtenir des structures en couche sur la surface du substrat traité, ce qui permet d'améliorer grandement la durabilité de ce traitement. De ce fait, les substrats textiles traités possèdent des propriétés de résistance aux tâches et à la salissure et des propriétés hydrofuges et/ou oléofuges excellentes.
EP06760528A 2005-06-03 2006-05-30 Substrats textiles a structure d'appret en couche Withdrawn EP1907621A1 (fr)

Applications Claiming Priority (3)

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US11/145,337 US7485588B2 (en) 2003-01-10 2005-06-03 Method for making textile substrates having layered finish structure for improving liquid repellency and stain release
US11/145,389 US7407899B2 (en) 2003-01-10 2005-06-03 Textile substrates having layered finish structure for improving liquid repellency and stain release
PCT/US2006/020802 WO2006132852A1 (fr) 2005-06-03 2006-05-30 Substrats textiles a structure d'appret en couche

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