US3671292A - Zirconium anti-soil treatment of synthetic fibers and resultant article - Google Patents

Zirconium anti-soil treatment of synthetic fibers and resultant article Download PDF

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US3671292A
US3671292A US84197769A US3671292A US 3671292 A US3671292 A US 3671292A US 84197769 A US84197769 A US 84197769A US 3671292 A US3671292 A US 3671292A
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zirconium
test
soiling
fiber
samples
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Julian J Hirshfeld
Bertie J Reuben
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Monsanto Co
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Monsanto Co
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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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71—Salts of phosphoric acids
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/20—Halides of elements of Groups 4 or 14 of the Periodic Table, e.g. zirconyl chloride
    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
    • D06M11/60—Ammonia as a gas or in solution
    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/63—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with hydroxylamine or hydrazine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D06M11/65—Salts of oxyacids of nitrogen
    • D—TEXTILES; PAPER
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/335—Amines having an amino group bound to a carbon atom of a six-membered aromatic ring
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/342—Amino-carboxylic acids; Betaines; Aminosulfonic acids; Sulfo-betaines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35—Heterocyclic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46—Compounds containing quaternary nitrogen atoms
    • D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/503—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
    • Y10T428/2958—Metal or metal compound in coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/2279—Coating or impregnation improves soil repellency, soil release, or anti- soil redeposition qualities of fabric
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/2861—Coated or impregnated synthetic organic fiber fabric
    • Y10T442/2885—Coated or impregnated acrylic fiber fabric
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/2861—Coated or impregnated synthetic organic fiber fabric
    • Y10T442/2893—Coated or impregnated polyamide fiber fabric

Definitions

  • This invention relates to a process of treating textile articles to impart anti-soiling characteristics thereto and to textile articles treated by such a process. More specifically, the invention concerns a process of treating textile articles comprised of synthetic fibers with zirconium salts to impart anti-soiling characteristics thereto and to such articles treated by the process.
  • Soiling of textile articles is generally effected by three methods, i.e., directly contacting the article with soiling particles, contacting the article with air-borne soiling particles, and contacting the article with liquid-borne substances containing soiling particles. Retention of these soiling particles on the textile article can be explained by three mechanisms, i.e., purely mechanical forces of entrapment or occlusion, interfacial adhesional forces such as Van der Walls forces and electrostatic forces. Removal of the soiling particles from the textile article is dependent on 3,671,292 Patented June 20, 1972 Ice numerous factors. Generaly speaking, large soiling particles can be readily removed whereas soiling particles within the range of less than 20 microns, and especially around 1 micron, are extremely difficult to remove from the textile article.
  • the textile industry has tried to prevent the soiling of textile articles by treating the articles with numerous organic and inorganic compositions. Most of these compositions are merely deposited on the article without any chemical bonding, and, as a result, are not efiective over a prolonged period of time and are easily removed by washing, dry-cleaning or even vacuuming.
  • articles having interstices on the surface of the fiber are made soil-resistant by depositing small particles, usually less than 20 microns in diameter, of silicas on the fiber to fill the interstices and thus prevent the entrapment of soiling particles therein.
  • most of these silicas do not chemically bond to the fiber and are easily removed by washing and vacuuming and, in some cases, cause dusting problems.
  • the textile industry has tried to prevent the build-up of static charges on hydrophobic fibers by treating these fibers with cationic softeners; however, limited success has been experienced since most of these softeners are usually water soluble and are readily removed by washing.
  • Another object of this invention is to provide textile articles comprised of a synthetic fiber selected from the group consisting of polyamide fiber, polyester fiber, acrylic fiber, olefin fiber, modacrylic fiber, and spandex fiber with a process which imparts good anti-soiling characteristics thereto.
  • the term textile article is meant to include fiber, yarn, all types of fabric, all types of carpets, and any textile article comprised of synthetic fiber.
  • synthetic fiber is meant to include spandex fiber (a manufactured fiber in which the fiber-forming substance is any longchain synthetic polymer composed of at least by weight of a segmented polyurethane) polyester fiber (a manufactured fiber in which the fiber-forming substance is any long-chain synthetic polymer composed of at least 85 by weight of an ester of a dihydric alcohol and a dibasic acid or derivative thereof, such as terephthalic acid, or dimethylterephthalate), olefin fiber (a manufactured fiber in which the fiber-forming substance is any long-chain synthetic polymer composed of at least 85% by weight of ethylene, propylene, or other olefin units), modacrylic (a manufactured fiber in which the fiber-forming substance is any long-chain synthetic polymer composed of less than 85 but at least 35% by weight of acrylonitrile units), nylon fiber .(a manufactured fiber in which the fiber-forming substance
  • zirconium salts useful in the invention include any zirconium salt that is water soluble in the sense that they can be made soluble in water at certain pHs.
  • Zirconium salts usually contain small amounts of hafnium, generally from about 0.5% to about 4.5% by weight.
  • Hafnium is extremely similar to zirconium and, for purposes of this invention, it is to be assumed that where zirconium salts are mentioned herein it is meant to include zirconium salts with small concentrations, i.e., less than about 5.4% of hafnium.
  • zirconium salts examples include zirconium acetate, zirconium oxychloride, zirconium sulfate, zirconium acetylacetonate, potassium zirconyl carbonate, zirconium chloride, zirconium fluoride, zirconium nitrite, ammonium zirconyl carbonate, sodium zirconium oxychloride, sodium zirconium glycolate, and zirconium tetrachloride. From an economical standpoint, zirconium acetate is a particularly useful zironium salt.
  • a nitrogen containing base is present in the acidic aqueous solution containing the zirconium salt.
  • the nitrogen containing base can be either an organic or an inorganic derivative of ammonia.
  • the organic nitrogen containing base can be a primary amine, a secondary amine, a tertiary amine, or a quaternary ammonium salt and can contain one or more groupings selected from the class consisting of alkyl, aryl, alkaryl and aralkyl. The groupings can contain substituents such as hydroxyl, carboxyl, sulfonic, nitro and halogens (chloro, bromo, fluoro, and iodo).
  • Examples of useful inorganic nitrogen containing bases include hydroxylamine sulfate, hydroxylamine chloride, sulfamic acid, ammonium sulfamate, hydrazine, hydroxylamine, ammonia, and ammonium carbonate.
  • Examples of useful organic nitrogen containing bases include ammonium carbamate, ethylene diamine, 1,6-hexamethylenediamine, guanidine, pyridine, monoethanolamine, glycine, aminoacetic acid, p-aminobenzoic acid, aniline, aniline hydrochloride, furfurylamine, o-toluidine, morpholine, N-methylfurfurylamine, N-methyltetrahydrofurfurylamine, and piperazine.
  • the nitrogen containing base does help the deposition of the zirconium residue onto the fiber.
  • the nitrogen containing base forms a loose complex with the zirconium salt and this complex, due to its changed electrical bharacteristic, enables the zirconium salt to more readily attach itself to the nitrogenous sites in the fiber.
  • the nitrogen containing base acts as a transfer agent or carrier for the zirconium compound. Its use results in a more durable deposition of the zirconium residue on the synthetic fibers than would otherwine be accomplished.
  • the acidity of the aqueous solution should be within a pH range of from about 1.5 to less than about 7. Acids such as sulfuric acid, hydrochloride acid, acetic acid, phosphoric acid and formic acid are examples of acids useful to adjust the pH of the solution. Preferably, it is desired that the pH of the solution be within the range of from about 2 to about 5.
  • the acidity of the aqueous solution helps to solubilize the zirconium salt and the nitrogen containing base, and to maintain the zirconium in solution until, when the article is dried, a zirconium residue is thereby uniformly-de posited in the form of a microscopic cohesive and adhesive substantially continuous film of particles imbedded within the surface of the fibers.
  • the zirconium salt should be present in the acidic aqueous solution in amounts ranging from about 0.2% to about 20.0%, and preferably within the range of from about 1% to about 5%, the percents "based on' the weight of the textile article.
  • Useful weight ratios of the zirconium salt to the nitrogen containing base within the acidic aqueous solution are from about 5:0.2 to about 1:1, and preferably about 5:3, respectively.
  • the temperature of the acidic aqueous solution should be within the range of from about room temperature to about 212 F. Higher temperatures, for example within the range of from about 175 F. to about the boiling point temperature of the solution are preferred in facilitating the contacting of the textile article with the acidic aqueous solution.
  • Contacting the textile article with the acidic aqueous solution can be accomplished by immersion, padding, spraying, exhaust bath, roll application and any other like means known in. the textile art.
  • the method of contacting should be adequate to completely wet the textile article with the solution-Contact time can vary from a few seconds to minutes or even hours.
  • the contact time can vary from about a half of a second to about 3 seconds; where an exhaust procedure is used, the contact time can vary from about 15 minutes to about 30 or more minutes; and where the article is immersed in the solution, the contact time can vary from about 5 minutes to about minutes.
  • Contact time should be measured from the time of contact of the solution described. If, for example, it should be desirable to introduce the nitrogen-containing base while the textile article is in contact with the acidic aqueous solution of the zirconium salt, contact time would be measured from the time of introduction of the nitrogen-containing base.
  • the article is dried. Drying can be effected at temperatures within the range of from about room temperature up to about 350 F. Preferably, the textile articles are dried at temperatures within the range of 200 F. to 350 F.
  • Textile articles treated by the process of this invention exhibit good anti-soiling properties. Such properties are sufiiciently afiixed thereto to withstand dry-cleaning, washing, vacuuming, etc. Also, the textile article can be sub jected to a dyeing process either before or after it is treated with the acidic aqueous solution of this invention.
  • the sample is blank dyed by immersing it for 60 minutes in a boiling aqueous solution (liquor to goods ratio being about 35: 1) containing about 0.5 (based on weight of goods) of a nonionic surfactant followed by rinsing and drying.
  • a boiling aqueous solution containing about 0.5 (based on weight of goods) of a nonionic surfactant followed by rinsing and drying.
  • Other blank dyeing procedures for particular fibers are of common knowledge in the art.
  • photo reflectance measurements or readings are made of two samples (dimensions being 2" x 4") of the textile article used in each example. Initial reflectance readings are made after the textile article is first treated in accordance with the invention and then reflectance readings are made after the sample is soiled. The difference in the reflectance readings indicate the antisoiling properties or characteristics of the samples, i.e. a large number indicates poor anti-soiling properties whereas a small number indicated good anti-soiling properties.
  • the photo reflectance readings are measured by using a Photovolt Reflectance Meter (Model No. 610, Photovolt Corp., New York City, N. Y.).
  • the samples of the textile articles are soiled by either of two methods, i.e. by an artificial soiling test or by a floor soiling test.
  • the artificial soiling test is accomplished by placing the samples in a one gallon wide mouth jar having therein two glass rods long by diameter) glued on opposite sides of the jar and containing (based on Weight of the sample) of artificial soil and 10 number two rubber stoppers.
  • the artificial soil has the following composition (the soil is sifted through a 30 mesh screen):
  • the jar is then sealed, placed on a ball mill and rotated at 95-100 r.p.m. for 30 minutes in a clockwise direction and 30 minutes in a counter-clockwise direction at the same r.p.m. Thereafter, the samples are removed from the jar, vacuumized, and the photo reflectance readings of the two samples measured.
  • the difference between the average initial reflectance readings and the average of the final reflectance readings indicate the degree of soil resistance. As mentioned earlier, a small photo reflectance difference number indicates a good anti-soiling property whereas a large number indicates a poor anti-soiling property of the textile article.
  • the procedure in the floor soiling test is the same as the above artificial soiling test except the samples are soiled by placing them in the pathway of a well-traveled walkway and soiled by natural means, such as by shoes, air-borne soiling particles, etc.
  • Control samples that is samples that are not treated with the acidic aqueous solution containing the zirconium salt and the nitrogen containing base, are soiled under the same conditions as the test samples.
  • the test results of the control samples as compared to the test results of the test samples indicate the significances of the invention.
  • the percent increase in anti-soiling characteristic imparted to the samples is indicated in the examples as Percent Improvement of Test Sample Over Control Sample.
  • the initial reflectance readingsof the control samples are taken after the control samples are scoured. Percents where used are based on weight unless otherwise specified.
  • Example 1 The following scoured samples are immersed in separate aqueous solutions (liquor to goods ratio 40:1) at room temperature, each solution has a pH of 2.4 and contains 1.1% zirconium acetate, 3% sulfuric acid and 3% hydroxylamine sulfate, the percents based on weight of ,the samples.
  • the solutions are heated to and maintained at the boiling point for 30 minutes. Thereafter, the samples are removed from the solutions, rinsed in water, blank dyed, rinsed again in water, dried, and then subjected to the artificial soiling test.
  • the results of the soiling test are indicated in Table 1.
  • Control samples i.e. samples identical to their respective test samples except that they are. not treated in the aqueous solutions, are .presentedftoshow. the significance of the invention.
  • Control 66 30 36 Test 66 40 26 28 (h) Spandex knit (Blue C,
  • Example 2 I Samples are treated as described in Example 1 except the solutions are at a pH of 3.7 and contain 3% acetic acid instead of the sulfuric acid. The results of the artificial soiling test are indicated in Table II.
  • Example 3 25 The following samples are treated as described in Example 1 except the aqueous solution is at a pH of l 5 2.6 and contains 5% zirconium oxychloride, 3% hydro- EXamP e chloric acid and 3% hydroxylamme hydrochloride.
  • the A li k i Samples composed of 765% of a l results of the soiling test are indicated in Table III.
  • mer being 93% acrylonitrile and 7% vinyl acetate 10.5% of a copolymer being 50% acrylonitrile and 50% methylvinylpyridine and 13% polyvinylchloride are treated as described in Example 1 except the aqueous solution is at a pH of 3.9 and contains 3% ammonium TABLE 111 sulfamate instead of the hydroxylamine sulfate.
  • the re- Pment sults of the artificial soiling test are indicated in Table V.
  • Example 8 At a temperature of from about room temperature
  • Example 8 to about the boiling point thereof, containing es- 40 sentially as solutes from about 0.2% to about 20%
  • Scoured samples of nylon knit are treated as described of a water-soluble zirconium salt and from about in Example 1 except the aqueous solutions (liquor to 0.2% to about 20% of a material selected from the goods ratio being 30:1) contain composit1ons as outlined group consisting of organic and inorganic derivain Table VIII.
  • the pH of the solutions and the results tives of ammonia, the percents based on the weight of the artificial soiling tests are indlcated 1n the followof the textile article; and
  • acetic acid to adjust the pH of the bath to the numbers polyester fibers, and acrylic fibers.
  • zirconium salt is selected from the group consisting of zirconium acetate, zirconium oxychloride, zirconium sulfate, zirconium acetylacetonate, potassium zirconyl carbonate, zirconium chloride, zirconium fluoride, zirconium nitrite, ammonium zirconyl carbonate, sodium zirconyl oxychloride, sodium zirconium glycerinate, and zirconium tetrachloride; and said derivative of ammonia is selected from the group consisting of primary amines, secondary amines, tertiary amines, and quarternary ammonium salts.
  • synthetic fibers are selected from the group consisting of polyamide fibers, polyester fibers, and acrylic fibers.
  • the acidic aqueous solution contains from 0.4% to about 8.0% of the zirconium-containing material and from about 0.2% to about 5.0% of the ammonium derivative, the percents being based on the weight of the fibers.
  • a textile article comprised of synthetic fibers having bonded and embedded within the surface of said fibers, a microscopic uniform film of particles consisting essentially of the reaction product of a zirconium salt and a derivative of ammonia, said textile article having been produced by the process of (1) immersing the article in an acidic aqueous solution at a pH of from about 1.5 to less than about 7, at a temperature of from about room temperature to about the boiling point thereof, containing essentially as a solute about 02-20 percent of zirconium acetate and about 02-20 percent of a material selected from the group consisting of organic and inorganic derivatives of ammonia, the percents being based on the weight of the textile article; (2) then drying the article.
  • a textile article comprised of synthetic fibers having bonded and embedded within the surface of said fibers a uniform microscopic uniform film of particles consisting essentially of a zirconium reaction product which is the residue of an evaporated acidic aqueous solution of from about 0.2% to about 20% of a water-soluble zirconium salt and from about 0.2% of a material selected from the group consisting of organic and inorganic derivatives of ammonia, the percents being based on the weight of the textile article.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
US84197769 1964-12-18 1969-07-15 Zirconium anti-soil treatment of synthetic fibers and resultant article Expired - Lifetime US3671292A (en)

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CH (1) CH449574A (enrdf_load_stackoverflow)
DE (1) DE1469437A1 (enrdf_load_stackoverflow)
FR (1) FR1461026A (enrdf_load_stackoverflow)
GB (1) GB1112167A (enrdf_load_stackoverflow)
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3887740A (en) * 1972-05-01 1975-06-03 Corning Glass Works Process for depositing oxide coatings
US3993830A (en) * 1972-04-28 1976-11-23 Colgate-Palmolive Company Soil-release finish
US4201805A (en) * 1971-03-18 1980-05-06 International Wool Secretariat Zirconium flame-resist, low smoke emission treatment
US4317859A (en) * 1979-03-27 1982-03-02 Monsanto Company Soil-resistant yarns
US4423113A (en) * 1982-03-22 1983-12-27 Monsanto Company Zirconium oxide coated nylon fibers
US4808191A (en) * 1987-06-04 1989-02-28 Milliken Research Corporation Process for pattern dyeing of textile materials
US5908663A (en) * 1996-02-01 1999-06-01 Minnesota Mining And Manufacturing Company Topical carpet treatment
US20050095933A1 (en) * 2003-11-03 2005-05-05 Kimbrell William C. Textile substrates, compositions useful for treating textile substrates, and related methods
US20070178038A1 (en) * 1999-06-03 2007-08-02 Pope Edward J Method for forming hafnium carbide and hafnium nitride ceramics and preceramic polymers

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1379752A (en) * 1971-03-18 1975-01-08 Iws Nominee Co Ltd Zirconium flame-resist treatment
DE3247351A1 (de) * 1982-12-22 1984-06-28 Bayer Ag, 5090 Leverkusen Formkoerper und ihre herstellung
RU2145653C1 (ru) * 1998-12-30 2000-02-20 Санкт-Петербургский государственный университет технологии и дизайна Способ получения текстильного объемного волокнистого катализатора
RU2258716C2 (ru) * 2002-08-12 2005-08-20 Казанский государственный медицинский университет Способ получения хемосорбционного материала
RU2262557C1 (ru) * 2004-04-08 2005-10-20 Общество с ограниченной ответственностью ООО "Аквафор" (ООО "Аквафор") Способ получения ионообменного полиакрилонитрильного волокна (варианты)
RU2265032C1 (ru) * 2004-05-20 2005-11-27 Государственное образовательное учреждение высшего профессионального образования "Санкт-Петербургский государственный университет технологии и дизайна" Способ получения трикотажного материала с каталитическими свойствами
RU2266304C1 (ru) * 2004-05-20 2005-12-20 Государственное образовательное учреждение высшего профессионального образования "Санкт-Петербургский государственный университет технологии и дизайна" Способ получения текстильного полимерного катализатора

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4201805A (en) * 1971-03-18 1980-05-06 International Wool Secretariat Zirconium flame-resist, low smoke emission treatment
US3993830A (en) * 1972-04-28 1976-11-23 Colgate-Palmolive Company Soil-release finish
US3887740A (en) * 1972-05-01 1975-06-03 Corning Glass Works Process for depositing oxide coatings
US4317859A (en) * 1979-03-27 1982-03-02 Monsanto Company Soil-resistant yarns
US4423113A (en) * 1982-03-22 1983-12-27 Monsanto Company Zirconium oxide coated nylon fibers
US4808191A (en) * 1987-06-04 1989-02-28 Milliken Research Corporation Process for pattern dyeing of textile materials
US5908663A (en) * 1996-02-01 1999-06-01 Minnesota Mining And Manufacturing Company Topical carpet treatment
US20070178038A1 (en) * 1999-06-03 2007-08-02 Pope Edward J Method for forming hafnium carbide and hafnium nitride ceramics and preceramic polymers
US7572881B2 (en) * 1999-06-03 2009-08-11 Pope Edward J A Method for forming hafnium carbide and hafnium nitride ceramics and preceramic polymers
US20050095933A1 (en) * 2003-11-03 2005-05-05 Kimbrell William C. Textile substrates, compositions useful for treating textile substrates, and related methods

Also Published As

Publication number Publication date
IL24800A (en) 1969-02-27
CH1751265A4 (enrdf_load_stackoverflow) 1967-08-15
NL129268C (enrdf_load_stackoverflow) 1900-01-01
LU50071A1 (enrdf_load_stackoverflow) 1966-06-15
BE673933A (enrdf_load_stackoverflow) 1966-06-17
DE1469437A1 (de) 1970-07-16
NL6516463A (enrdf_load_stackoverflow) 1966-06-20
GB1112167A (en) 1968-05-01
CH449574A (de) 1968-04-11
FR1461026A (fr) 1966-12-02

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