WO2016179384A1 - Synthetic fibers with enhanced soil resistance and methods for production and use thereof - Google Patents

Synthetic fibers with enhanced soil resistance and methods for production and use thereof Download PDF

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Publication number
WO2016179384A1
WO2016179384A1 PCT/US2016/030967 US2016030967W WO2016179384A1 WO 2016179384 A1 WO2016179384 A1 WO 2016179384A1 US 2016030967 W US2016030967 W US 2016030967W WO 2016179384 A1 WO2016179384 A1 WO 2016179384A1
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WO
WIPO (PCT)
Prior art keywords
fiber
synthetic fiber
polymer
soil resistance
affecting additive
Prior art date
Application number
PCT/US2016/030967
Other languages
French (fr)
Inventor
Mansour K ABDULBAKI
Wae-Hai Tung
Original Assignee
Invista Technologies S.Ar.L.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Invista Technologies S.Ar.L. filed Critical Invista Technologies S.Ar.L.
Priority to JP2018510320A priority Critical patent/JP2018515701A/en
Priority to CA2985101A priority patent/CA2985101A1/en
Priority to AU2016258018A priority patent/AU2016258018B2/en
Priority to EP16727002.4A priority patent/EP3292234A1/en
Priority to US15/570,784 priority patent/US20180119310A1/en
Priority to CN201680026259.0A priority patent/CN108138369A/en
Publication of WO2016179384A1 publication Critical patent/WO2016179384A1/en

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Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/253Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds

Definitions

  • the present disclosure relates to a soil resistance-affecting additive and synthetic fibers made therefrom having enhanced soil resistance.
  • the present disclosure also relates to articles of manufacture prepared from these fibers and methods for their production and use.
  • U.S. Patent 5,882,762 to Goeman discloses carpet yarn comprising a plurality of filaments of thermoplastic polymers with a fluorochemical or non-fiuorochemical hydrophilicity imparting compound dispersed within the filaments. It was found that the presence of the hydrophilicity imparting compound in the filaments allowed production of carpet yarn with a reduced amount of spin finish or even without the spin finish normally required. Carpets produced using such yarn were less susceptible to soiling.
  • U.S. Patent 8,247,519 discloses articles fabricated from polyamides and comprising fluoroether functionalized aromatic moieties with soil and oil resistance.
  • U.S. Patent 8,304,513 discloses soil resistant polyester polymers, particularly
  • poly(trimethylene terephthalate) comprising fluorovinylether functionalized aromatic repeat units.
  • U.S. Patent 8,697,831 discloses soil resistant polyamides, particularly nylon 6,6 and nylon 6 comprising fluoroether functionalized aromatic repeat units.
  • An aspect of the present invention relates to a synthetic fiber comprising a first fiber forming polymer, and a soil resistance-affecting additive.
  • the soil resistance-affecting additive is present in the fiber at a range from about 0.1 to 10 percent by weight.
  • At least a portion of the soil resistance-affecting additive is present on the surface of the fiber. Preferred is that this portion present on the surface is sufficient to impart soil resistant properties to the fiber.
  • At least a portion of the soil resistance-affecting additive is not polymerized with first fiber forming polymer.
  • At least a portion of the soil resistance-affecting additive has bloomed to the surface of the fiber.
  • the first fiber forming polymer of the synthetic fiber is a polyamide, a polyester, or a polyolefm, or any combination thereof.
  • the soil resistance-affecting additive of the synthetic fiber is an aromatic sulfonate or an alkali metal salt thereof.
  • the soil resistance-affecting additive is a polymer.
  • Another aspect of the present invention relates to a synthetic fiber comprising a first fiber forming polymer, a second polymer and a soil resistance-affecting additive.
  • the first fiber forming polymer is present in a range from about 80 to 99 percent by weight; the second polymer is present in a range from about 0.2 to 10 percent by weight; and the soil resistance-affecting additive is present in the fiber at a range from about 0.1 to 10 percent by weight.
  • the second polymer of the synthetic fiber has a melting point which is less than the melting point of the first fiber forming polymer and/or does not cause the synthetic fiber to fibrillate.
  • the second polymer is a polyolefm, a polylactic acid or a polystyrene or any combination thereof.
  • the soil resistance-affecting additive of the synthetic fiber is an aromatic sulfonate or an alkaH metal salt thereof.
  • Another aspect of the present invention relates to articles of manufacture, at least a portion of which comprises one or more of these synthetic fibers.
  • Nonlimiting examples of these articles of manufacture include yarns and fabrics formed from the synthetic fibers and carpets formed from the yams.
  • Yet another aspect of the present invention relates to method for producing a synthetic fiber with enhanced soil resistance.
  • the method comprises forming a polymer melt of a first fiber forming polymer and a soil resistance-affecting additive.
  • the soil resistance-affecting additive is present in a range from about 0.1 to 10 percent by weight.
  • a synthetic fiber is then formed from the polymer melt.
  • the method comprises forming a polymer melt comprising a first fiber forming polymer and a masterbatch compound.
  • the masterbatch compound comprises a second polymer and a soil resistance- affecting additive.
  • the first fiber forming polymer is present in a range from about 80 to 99 percent by weight, and the masterbatch compound is present in a range from about 0.2 to 20 percent by weight.
  • a synthetic fiber is then formed from the polymer melt.
  • FIG. 1 is a plot which shows soiling performance after the carpet samples were hot water extracted before they were soiled. This plot indicates the durability of the soiling performance of the carpet samples. As indicated in FIG. 1, the examples with the inventive embodiments performed the best after HWE treatment.
  • FIG. 2 is a plot of colorimetric L* progression upon the soiling and vacuum cleaning (S&V). and hot water extraction (HWE) cycles of a single set of carpets. H denotes that this carpet was pre-HWE 3X before the testing to mimic scouring.
  • FIG. 3 is a SEM micrograph of a triloba! filament from an embodiment of the current invention. Depicted is pigmented 1.0wt% dimethyl-5-sulfoisophthalate, sodium salt (NaSIM) in a polyester fiber where the masterbatch carrier of the NaSIM is polypropylene.
  • FIG. 4 is a set of SEM micrographs and XDS spectra of longitudinal sections of an embodiment of the current invention. Depicted is a trilobal filament of NaSIM in pigmented PET where the masterbatch carrier of the NaSIM is polypropylene.
  • FIG. 5 is a SEM micrograph of an example of an embodiment of the current invention. Depicted is a trilobal filament of pigmented 0.5wt% 5-sulfoisophthalic acid, sodium salt (SSIPA) in a polyester fiber that was added with a polypropylene masterbatch carrier.
  • SSIPA 5-sulfoisophthalic acid, sodium salt
  • fibers with enhanced soil resistance are provided by this disclosure.
  • the synthetic fiber comprises a first fiber forming polymer and a soil resistance-affecting additive.
  • first fiber forming polymers which can be used in this embodiment include, but are not limited to, polyamides, polyesters, and polyolefins and any blends or combinations thereof.
  • Suitable polyamides include fiber forming polyamides known in the art to be suitable for the formation of bulked continuous filament fibers, having sufficient viscosity, tenacity, chemical stability and crystallinity to be at least moderately durable in such application.
  • the polyamide may be selected from the group consisting of nylon 5,6; nylon 6,6; nylon 6; nylon 7; nylon 11; nylon 12; nylon 6/10;, nylon 6/12; nylon DT; nylon 6T; nylon 61; and blends or copolymers thereof.
  • the polyamide is nylon 6,6 polymer.
  • Suitable polyolefins include polypropylene.
  • Suitable polyesters include fiber forming polyesters known in the art.
  • the polyester resin may be selected from the group consisting of polyethylene terephthalate (PET), polybutylene terephthalate, polytrimethylene terephthalate, polyethylene naphthalate, polylactic acid (PLA) and blends or copolymers thereof.
  • the first fiber forming polymer is present in the synthetic fiber in a range from about 90 to 99 percent by weight.
  • Patent 6,680,018 disclose a similar composition and method wherein the stain resistance of polyamide fibers is improved by melt compounding a combination of sulfonated polyester concentrate and thermoplastic carrier resin with fiber-forming polyamide compositions subsequent to polymerization of the polyamide and prior to the formation of the fibers.
  • the synthetic fiber of this embodiment further comprises a soil resistance-affecting additive.
  • the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt (SSIPA) and dimethyl-5-suIfoisophthalate, sodium salt (NaSIM).
  • the soil resistance-affecting additive is a polymer.
  • a nonlimiting example of a polymer useful as a soil resistance-affecting additive in this embodiment is polypropylene.
  • the soil resistant additive is present in the synthetic fiber in a range from about 0.1 to about 10 percent by weight.
  • the synthetic fiber of the present disclosure comprises a first fiber forming polymer, a second polymer and a soil resistance-affecting additive.
  • first fiber forming polymers which can be used in this embodiment include, but are not limited to, polyamides, polyesters, and polyolefins and any blends or combinations thereof.
  • Suitable polyamides include fiber forming polyamides known in the art to be suitable for the formation of bulked continuous filament fibers, having sufficient viscosity, tenacity, chemical stability and crystallinity to be at least moderately durable in such application.
  • the polyamide may be selected from the group consisting of nylon 5,6; nylon 6,6; nylon 6; nylon 7; nylon 11; nylon 12; nylon 6/10;, nylon 6/12; nylon DT; nylon 6T; nylon 61; and blends or copolymers thereof.
  • the polyamide is nylon 6,6 polymer.
  • Suitable polyolefins include polypropylene.
  • Suitable polyesters include fiber forming polyesters known in the art.
  • the polyester resin may be selected from the group consisting of polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polyethylene naphthalate, polylactic acid (PLA) and blends or copolymers thereof.
  • the first fiber forming polymer is present in the synthetic fiber in a range from about 80 to 99 percent by weight.
  • the synthetic fiber of this embodiment further comprises a soil resistance-affecting additive.
  • the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof.
  • Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt and dimethyl-5-sulfoisophthalate, sodium salt.
  • the soil resistant additive is present in the synthetic fiber in a range from about 0.1 to about 10 percent by weight.
  • the synthetic fiber of this embodiment further comprises a second polymer.
  • the second polymer having a melting point that is less than the melting point of the first fiber forming polymer.
  • the presence of the second polymer does not cause the synthetic fiber to fibrillate.
  • second polymers useful in the present disclosure include, but are not limited to, polyolefins, polylactic acid and polystyrene, or any blend or combination thereof.
  • the polyolefin is an unmodified polyolefin.
  • the second polymer is polypropylene.
  • the second polymer is present in the synthetic fiber in a range from about 0.5 to about 10 percent by weight.
  • at least a portion of the soil resistance- affecting additive is present on the surface of the fiber. Preferred is that this portion present on the surface of the fiber is sufficient to impart soil resistant properties to the fiber.
  • At least a portion of the soil resistance- affecting additive is not polymerized with the first fiber forming polymer. Instead, preferred in the synthetic fibers of this disclosure is that at least a portion of the soil resistance-affecting additive has bloomed to the surface of the fiber.
  • the synthetic fiber of this disclosure has a multilobal cross section.
  • a majority meaning greater than 50%
  • at least 75% or substantially all of the soil resistant additive present on the surface of the fibers is located in the area between the lobes.
  • the present disclosure also relates to articles of manufacture comprising at least a poition of a synthetic fiber or fibers of this disclosure.
  • articles of manufacture include, but are not limited to, yarns prepared from the synthetic fibers, as well as fabrics and carpets prepared from the synthetic fibers and/or yarns.
  • Also provided by this disclosure are processes for forming these synthetic fibers with enhanced soil resistance.
  • the process comprises forming a polymer melt comprising a first fiber forming polymer and a soil resistance-affecting additive.
  • the soil resistance-affecting additive is present in a range from about 0.1 to 10 percent by weight.
  • a synthetic fiber is then formed from the polymer melt.
  • the soil resistance-affecting additive used in the process can be an aromatic sulfonate or an alkali metal salt thereof, or a polymer.
  • Nonlimiting examples include 5- sulfoisophthalic acid, sodium salt; dimethyl-5-sulfoisophthalate, sodium salt; and polypropylene.
  • the soil resistance-affecting additive is added to the polymer melt by powder addition. In another nonlimiting embodiment, the soil resistance- affecting additive is added as a powder capsule.
  • the process comprises forming a polymer melt comprising a first fiber forming polymer and a masterbatch compound.
  • the masterbatch compound comprises a second polymer and a soil resistance- affecting additive.
  • the first fiber forming polymer is present in a range from about 80 to 99 percent by weight, and the masterbatch compound is present in a range from about 1 to 20 percent by weight.
  • no additional steps are required to remove volatiles while forming the polymer melt.
  • a synthetic fiber is then formed from this polymer melt.
  • the soil resistant additive used in the process can be an aromatic sulfonate or an alkali metal salt thereof. Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt and dimethyl-5-sulfoisophthalate, sodium salt.
  • the masterbatch compound comprises a thermoplastic carrier, also referred to herein as second polymer.
  • thermoplastic carriers useful in the masterbatch include, but are not limited to polyolefins, polylactic acid, polystyrene, or a blend or copolymer thereof.
  • the thermoplastic carrier is a polyolefin.
  • the thermoplastic carrier is an unmodified polyolefin.
  • the thermoplastic carrier is polypropylene.
  • thermoplastic carrier is present in the masterbatch compound in a range from about 40 to about 90 percent by weight. In one nonlimiting embodiment, the masterbatch compound comprises about 50% of the thermoplastic carrier.
  • the masterbatch compound further comprises a soil resistance-affecting additive.
  • Suitable soil resistance-affecting additives include, but are not limited to aromatic sulfonates and alkali metal salts thereof, such as 5-sulfoisophthalic acid, sodium salt and dimethyl-5- sulfoisophthalate, sodium salt.
  • the soil resistance-affecting additive is present in the masterbatch compound in a range from about 10 to about 60 percent by weight.
  • the masterbatch compound has a moisture content less than about 200 ppm, more preferably less than about 50 ppm. In another nonlimiting embodiment,
  • the masterbatch compound is not dried or conditioned prior to forming the polymer melt.
  • the masterbatch compound may further comprise other additives, to be used to confer additional benefits to articles upon polymer melt extrusion and melt spinning.
  • additives are inorganic pigments, and ultraviolet (UV) light absorbers or optical brightening agents.
  • UV light absorbers or optical brightening agents examples include titanium dioxide, barium sulfate, carbon black, manganese dioxide, and zinc oxide.
  • UV light absorbers or optical brightening agents examples include 2,2'-(l ,2-ethenediyldi-4,l phenylene)bisbenzoxazole, available commercially by Eastman Chemical Company under the tradename Eastobrite® OB-1, and 2,2'-(2 ,5- thiophenediyl)bis(5-tert-butylbenzoxazole, available commercially by Mayzo, Inc. under the tradename Benetex® OB.
  • the masterbatch compound is present in fiber in a range from about 1 to about 20 percent by weight.
  • the present disclosure also relates to articles of manufacture, at least a portion of which comprises a synthetic fiber produced in accordance with this process.
  • Nonlimiting examples include yams prepared from synthetic fibers produced by this process, as well as fabrics and carpets prepared from these synthetic fibers and/or yarns.
  • masterbatches were prepared with the following soil resistance-affecting additives:
  • the masterbatches were added at the extruder hopper to a standard bottle-grade PET resin, at 0.5 wt% and 2 wt% actives.
  • the resultant pigmented trilobal PET fibers were processed and tufted into a 30 oz./sq. yd residential cut pile carpet. It was found that the characteristic stain resistance of PET was not negatively impacted by blending with the soil resistant additive.
  • a filament in accordance with the present disclosure has an exterior modification ratio (R2/R1) that can be about 1.50 to 3.00, and more particularly can be about 2.15 to 2.85.
  • the modification ratio (MR) for the control items was nominally the same, at 2.5.
  • Modification ratio determinations, in particular for triloba! bulked continuous filaments, are described as disclosed in European Patent 1,518,948, and U.S. Patent Publication 2015 0275400.
  • the synthetic fibers of this disclosure were found to have markedly improved soiling performance in carpet form.
  • Carpets produced from these synthetic fibers have a "built- in,” or fiber bound, anti-soil performance that exceeds current fluorochemical-based topical anti- soil treatment in efficacy.
  • this built-in resistance is more durable than topical treatments for anti-soil which are known to "walk off with wear and foot traffic so that the topical chemistry is no longer effective.
  • using the synthetic fibers of this disclosure ehminates the need for topical application of chemicals by downstream carpet mills. Use of a non-fluoiinated compound to enhance soil resistance also diminishes possible environmental concerns.
  • Accelerated drum soiling is recorded as Delta E, and measured according to ASTM D6540. Within the reproducibility limitations of this test, the relative soiling performance of variously-treated samples may be determined.
  • the test simulates the soiling of carpet in residential or commercial environments to a traffic count level of about 100,000 to 300,000. According to ASTM D6540, soiling tests can be conducted on up to six carpet samples simultaneously using a drum.
  • the base color of the sample (using the L, a, b color space) is measured using the hand held color measurement instrument sold by Minolta Corporation as "Chromameter" model CR-310 (at Camden). This measurement output is in the form L*, a* and b* values and describes a color value in color space. This is the original color value.
  • the carpet sample is mounted on a thin plastic sheet and placed in the drum. Two hundred fifty grams (250 g) of dirty Zytel 101 nylon beads (by DuPont Canada, Mississauga, Ontario) are placed on the sample.
  • the dirty beads are prepared by mixing ten grams (10 g) of AATCC TM-122 synthetic carpet soil (by Manufacturer Textile Innovators Corp., Windsor, N.C.) with one thousand grams (1000 g) of new Nylon Zytel 101 beads.
  • One thousand grams (1000 g) of 3 ⁇ 4-inch diameter steel ball bearings are added into the drum. The drum is run for 30 minutes with direction reversal and the sample removed. After removal the carpet is cleaned with a vacuum cleaner and the chromameter is used again to measure the color of the carpet after cleaning.
  • the difference between the color measurements of each carpet is the total color difference, ⁇ *, and is based on L*, a*, and b* color differences in color space, known to those skilled in the field where
  • AATCC TM175 - Stain Resistance Pile Floor Coverings
  • Comparative Examples 1 , 2, and 5 and Examples 3, 4, 6, and 7 were produced using pilot scale machinery.
  • the pilot equipment included a 12" twin screw extruder having five heating zones, a filter screen pack, any of a selection of desired spinnerets, a fiber quenching zone, godet rolls, and winders.
  • a standard spinning method was used to produce fiber from the pilot scale machinery, as follows: the polymer was extruded through the spinnerets and divided into two 184 filament segments. The molten fibers were then rapidly quenched in a chimney, where cooling air at about 10— 15 °C was blown past the filaments at four hundred and fifty cubic feet per minute [300-600 cfm] through the quench zone.
  • the filaments were then coated with a lubricant for drawing and crimping.
  • the coated yarns were drawn at about 2422 yards per minute (2.9x draw ratio) using a pair of heated draw rolls.
  • the draw roll temperature was 160° C.
  • the filaments were then forwarded into a dual-impingement hot air bulking jet, similar to that described in Coon, U.S. Patent 3,525,134, teachings of which are herein incorporated by reference, to form two BCF yarns (1000 denier, 5.4 dpi).
  • the temperature of the air in the bulking jet was 180 °C.
  • Comparative Example 1 PET BCF, no melt additive, no topical anti-soil treatment
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge ftifting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and the FIGs 1-2.
  • Comparative Example 2 PET BCF, no melt additive, treated with topical soil resist
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color.
  • Example 3 PET BCF, masterbatch additive, 1.0 wt% masterbatch
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery.
  • the masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks.
  • This BCF yarn had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
  • Example 4 PET BCF, masterbatch additive, 4 wt% masterbatch
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery.
  • the masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks.
  • This BCF yarn had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
  • Comparative Example 5 PET BCF, no melt additive, treated with topical soil resist, 50 oz/yd 2 carpet
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yam had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine and an anti-soil treatment was applied by spraying the tufted carpet with an anti-soil chemistry comprising clay nanoparticles (Laponite ®) and fluorochemicals (Capstone® RCP) at 1.2% owf. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
  • Example 6 PET BCF, masterbatch additive, 1.0 wt% masterbatch
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery.
  • the masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks.
  • This BCF yarn had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling , stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
  • Example 7 PET BCF, masterbatch additive, 4 wt% masterbatch
  • PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery.
  • the masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks.
  • This BCF yarn had a wool beige color. It was tufted into carpet having 1 ⁇ 2" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine.
  • the caipet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

Synthetic fibers with enhanced soil resistance, yarns and carpets prepared from these fibers and compounds and methods for their production are provided.

Description

Synthetic Fibers with Enhanced Soil Resistance and Methods for Production and Use
Thereof
Field of Invention
[0001] The present disclosure relates to a soil resistance-affecting additive and synthetic fibers made therefrom having enhanced soil resistance. The present disclosure also relates to articles of manufacture prepared from these fibers and methods for their production and use.
Background
[0002] In the production of textiles, such as carpet and apparel, it is common to treat substrates with a composition to impart desirable properties, such as resistance to soiling by particulates and dry soil.
[0003] Various fluorochemical compositions, and methods for their application, have been described for commercial use to impart soil resistance to carpets.
[0004] For example, U.S. Patent 5,882,762 to Goeman discloses carpet yarn comprising a plurality of filaments of thermoplastic polymers with a fluorochemical or non-fiuorochemical hydrophilicity imparting compound dispersed within the filaments. It was found that the presence of the hydrophilicity imparting compound in the filaments allowed production of carpet yarn with a reduced amount of spin finish or even without the spin finish normally required. Carpets produced using such yarn were less susceptible to soiling.
[0005] U.S. Patent 8,247,519 discloses articles fabricated from polyamides and comprising fluoroether functionalized aromatic moieties with soil and oil resistance.
[0006] U.S. Patent 8,304,513 discloses soil resistant polyester polymers, particularly
poly(trimethylene terephthalate) comprising fluorovinylether functionalized aromatic repeat units.
[0007] U.S. Patent 8,697,831 discloses soil resistant polyamides, particularly nylon 6,6 and nylon 6 comprising fluoroether functionalized aromatic repeat units.
[0008] Therefore, there is a need to provide polymeric fibers that have improved built-in soil resistance. Summary of the Invention
[0009] An aspect of the present invention relates to a synthetic fiber comprising a first fiber forming polymer, and a soil resistance-affecting additive.
[0010] In one nonHmiting embodiment, the soil resistance-affecting additive is present in the fiber at a range from about 0.1 to 10 percent by weight.
[0011] In one nonHmiting embodiment, at least a portion of the soil resistance-affecting additive is present on the surface of the fiber. Preferred is that this portion present on the surface is sufficient to impart soil resistant properties to the fiber.
[0012] In one nonHmiting embodiment, at least a portion of the soil resistance-affecting additive is not polymerized with first fiber forming polymer.
[0013] In one nonHmiting embodiment, at least a portion of the soil resistance-affecting additive has bloomed to the surface of the fiber.
[0014] In one nonHmiting embodiment, the first fiber forming polymer of the synthetic fiber is a polyamide, a polyester, or a polyolefm, or any combination thereof.
[0015] In one nonHmiting embodiment, the soil resistance-affecting additive of the synthetic fiber is an aromatic sulfonate or an alkali metal salt thereof. In another nonHmiting embodiment, the soil resistance-affecting additive is a polymer.
[0016] Another aspect of the present invention relates to a synthetic fiber comprising a first fiber forming polymer, a second polymer and a soil resistance-affecting additive. In one nonlirniting embodiment, the first fiber forming polymer is present in a range from about 80 to 99 percent by weight; the second polymer is present in a range from about 0.2 to 10 percent by weight; and the soil resistance-affecting additive is present in the fiber at a range from about 0.1 to 10 percent by weight.
[0017] In one nonHmiting embodiment, the second polymer of the synthetic fiber has a melting point which is less than the melting point of the first fiber forming polymer and/or does not cause the synthetic fiber to fibrillate.
[001 S[ In one nonlirniting embodiment, the second polymer is a polyolefm, a polylactic acid or a polystyrene or any combination thereof.
[0019] In one nonlirniting embodiment, the soil resistance-affecting additive of the synthetic fiber is an aromatic sulfonate or an alkaH metal salt thereof. [0020] Another aspect of the present invention relates to articles of manufacture, at least a portion of which comprises one or more of these synthetic fibers. Nonlimiting examples of these articles of manufacture include yarns and fabrics formed from the synthetic fibers and carpets formed from the yams.
[0021] Yet another aspect of the present invention relates to method for producing a synthetic fiber with enhanced soil resistance.
[0022] In one nonlimiting embodiment, the method comprises forming a polymer melt of a first fiber forming polymer and a soil resistance-affecting additive. In this nonlimiting embodiment, the soil resistance-affecting additive is present in a range from about 0.1 to 10 percent by weight. A synthetic fiber is then formed from the polymer melt.
[0023] In another nonlimiting embodiment, the method comprises forming a polymer melt comprising a first fiber forming polymer and a masterbatch compound. In this nonlimiting embodiment, the masterbatch compound comprises a second polymer and a soil resistance- affecting additive. In this nonlimiting embodiment, the first fiber forming polymer is present in a range from about 80 to 99 percent by weight, and the masterbatch compound is present in a range from about 0.2 to 20 percent by weight. A synthetic fiber is then formed from the polymer melt.
Brief Description of the Drawings
[0024] FIG. 1 is a plot which shows soiling performance after the carpet samples were hot water extracted before they were soiled. This plot indicates the durability of the soiling performance of the carpet samples. As indicated in FIG. 1, the examples with the inventive embodiments performed the best after HWE treatment.
[0025] FIG. 2 is a plot of colorimetric L* progression upon the soiling and vacuum cleaning (S&V). and hot water extraction (HWE) cycles of a single set of carpets. H denotes that this carpet was pre-HWE 3X before the testing to mimic scouring.
[0026] FIG. 3 is a SEM micrograph of a triloba! filament from an embodiment of the current invention. Depicted is pigmented 1.0wt% dimethyl-5-sulfoisophthalate, sodium salt (NaSIM) in a polyester fiber where the masterbatch carrier of the NaSIM is polypropylene. [0027] FIG. 4 is a set of SEM micrographs and XDS spectra of longitudinal sections of an embodiment of the current invention. Depicted is a trilobal filament of NaSIM in pigmented PET where the masterbatch carrier of the NaSIM is polypropylene.
[0028] FIG. 5 is a SEM micrograph of an example of an embodiment of the current invention. Depicted is a trilobal filament of pigmented 0.5wt% 5-sulfoisophthalic acid, sodium salt (SSIPA) in a polyester fiber that was added with a polypropylene masterbatch carrier.
Detailed Description of the Invention
[0029] Provided by this disclosure are fibers with enhanced soil resistance, yarns, fabrics and carpets prepared from these fibers, and methods and masterbatch compositions for their production.
[0030] In one nordhniting embodiment, the synthetic fiber comprises a first fiber forming polymer and a soil resistance-affecting additive.
[0031] Examples of first fiber forming polymers which can be used in this embodiment include, but are not limited to, polyamides, polyesters, and polyolefins and any blends or combinations thereof.
[0032] Suitable polyamides include fiber forming polyamides known in the art to be suitable for the formation of bulked continuous filament fibers, having sufficient viscosity, tenacity, chemical stability and crystallinity to be at least moderately durable in such application. The polyamide may be selected from the group consisting of nylon 5,6; nylon 6,6; nylon 6; nylon 7; nylon 11; nylon 12; nylon 6/10;, nylon 6/12; nylon DT; nylon 6T; nylon 61; and blends or copolymers thereof. In one embodiment the polyamide is nylon 6,6 polymer.
[0033] Suitable polyolefins include polypropylene.
[0034] Suitable polyesters include fiber forming polyesters known in the art. The polyester resin may be selected from the group consisting of polyethylene terephthalate (PET), polybutylene terephthalate, polytrimethylene terephthalate, polyethylene naphthalate, polylactic acid (PLA) and blends or copolymers thereof.
[0035] In this embodiment, the first fiber forming polymer is present in the synthetic fiber in a range from about 90 to 99 percent by weight.
[0036] It had previously been known to enhance stain resistance of polyamide fibers by forming the fibers from polyamides prepared by copolymerizing monomers, some of which contain sulfonate moieties. U.S. Patent 6,133,382, U.S. Patent 6,334,877 and U.S. Patent 6,589,466 disclose a fiber-forming polyarnide and a method to improve stain resistance of polyamide fibers by melt compounding a sulfonated polyester concentrate with fiber-forming polyamide compositions subsequent to polymerization of the polyamide and the concentrate and prior to the formation of the fibers. U.S. Patent 6,433,107 and U.S. Patent 6,680,018 disclose a similar composition and method wherein the stain resistance of polyamide fibers is improved by melt compounding a combination of sulfonated polyester concentrate and thermoplastic carrier resin with fiber-forming polyamide compositions subsequent to polymerization of the polyamide and prior to the formation of the fibers.
[0037] In addition, none of the disclosures referred to above contemplate the improvement of soil resistance for polyester-based fiber compositions, where the preponderance of the fiber composition is polyester. Furthermore, polyester compositions having up to 2% content by mass of sulfonic acid moieties are not deemed to be effectively soil resistant. As a result, there has been a long felt need to provide polymeric materials, especially polyester based materials, with improved soil resistance.
[0038] Through undue experimentation, the inventors surprisingly found that soil resistance of synthetic fibers could be improved by the addition of the soil resistance-affecting additive disclosed herein.
[0039] The synthetic fiber of this embodiment further comprises a soil resistance-affecting additive. In one nonlimiting embodiment, the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt (SSIPA) and dimethyl-5-suIfoisophthalate, sodium salt (NaSIM). In another nonlimiting embodiment, the soil resistance-affecting additive is a polymer. A nonlimiting example of a polymer useful as a soil resistance-affecting additive in this embodiment is polypropylene.
[0040] In this embodiment, the soil resistant additive is present in the synthetic fiber in a range from about 0.1 to about 10 percent by weight.
[0041] In another nonlimiting embodiment, the synthetic fiber of the present disclosure comprises a first fiber forming polymer, a second polymer and a soil resistance-affecting additive. [0042] Examples of first fiber forming polymers which can be used in this embodiment include, but are not limited to, polyamides, polyesters, and polyolefins and any blends or combinations thereof.
[0043] Suitable polyamides include fiber forming polyamides known in the art to be suitable for the formation of bulked continuous filament fibers, having sufficient viscosity, tenacity, chemical stability and crystallinity to be at least moderately durable in such application. The polyamide may be selected from the group consisting of nylon 5,6; nylon 6,6; nylon 6; nylon 7; nylon 11; nylon 12; nylon 6/10;, nylon 6/12; nylon DT; nylon 6T; nylon 61; and blends or copolymers thereof. In one embodiment the polyamide is nylon 6,6 polymer.
[0044] Suitable polyolefins include polypropylene.
[0045] Suitable polyesters include fiber forming polyesters known in the art. The polyester resin may be selected from the group consisting of polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polyethylene naphthalate, polylactic acid (PLA) and blends or copolymers thereof.
[0046] In this embodiment, the first fiber forming polymer is present in the synthetic fiber in a range from about 80 to 99 percent by weight.
[0047] The synthetic fiber of this embodiment further comprises a soil resistance-affecting additive. In one nonhmiting embodiment, the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof. Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt and dimethyl-5-sulfoisophthalate, sodium salt.
[0048] In this embodiment, the soil resistant additive is present in the synthetic fiber in a range from about 0.1 to about 10 percent by weight.
[0049] The synthetic fiber of this embodiment further comprises a second polymer. Preferred is that the second polymer having a melting point that is less than the melting point of the first fiber forming polymer. Also preferred is that the presence of the second polymer does not cause the synthetic fiber to fibrillate. Examples of second polymers useful in the present disclosure include, but are not limited to, polyolefins, polylactic acid and polystyrene, or any blend or combination thereof. In one nonlimiting embodiment, the polyolefin is an unmodified polyolefin. In another nonlimiting embodiment, the second polymer is polypropylene.
[0050] In one nonlimiting embodiment, the second polymer is present in the synthetic fiber in a range from about 0.5 to about 10 percent by weight. [0051] In the synthetic fibers of the present invention, at least a portion of the soil resistance- affecting additive is present on the surface of the fiber. Preferred is that this portion present on the surface of the fiber is sufficient to impart soil resistant properties to the fiber.
[0052] Further, in the synthetic fibers of this disclosure at least a portion of the soil resistance- affecting additive is not polymerized with the first fiber forming polymer. Instead, preferred in the synthetic fibers of this disclosure is that at least a portion of the soil resistance-affecting additive has bloomed to the surface of the fiber.
[0053] In one nonlimiting embodiment, the synthetic fiber of this disclosure has a multilobal cross section. In another nonlimiting embodiment, a majority (meaning greater than 50%), at least 75% or substantially all of the soil resistant additive present on the surface of the fibers is located in the area between the lobes.
[0054] The present disclosure also relates to articles of manufacture comprising at least a poition of a synthetic fiber or fibers of this disclosure. Examples of such articles include, but are not limited to, yarns prepared from the synthetic fibers, as well as fabrics and carpets prepared from the synthetic fibers and/or yarns.
[0055] Also provided by this disclosure are processes for forming these synthetic fibers with enhanced soil resistance.
[0056] In one nonlimiting embodiment, the process comprises forming a polymer melt comprising a first fiber forming polymer and a soil resistance-affecting additive. In this nonlimiting embodiment, the soil resistance-affecting additive is present in a range from about 0.1 to 10 percent by weight. A synthetic fiber is then formed from the polymer melt. In this embodiment, the soil resistance-affecting additive used in the process can be an aromatic sulfonate or an alkali metal salt thereof, or a polymer. Nonlimiting examples include 5- sulfoisophthalic acid, sodium salt; dimethyl-5-sulfoisophthalate, sodium salt; and polypropylene.
[0057] In one nonlimiting embodiment, the soil resistance-affecting additive is added to the polymer melt by powder addition. In another nonlimiting embodiment, the soil resistance- affecting additive is added as a powder capsule.
[0058] In another nonlimiting embodiment, the process comprises forming a polymer melt comprising a first fiber forming polymer and a masterbatch compound. In this nonlimiting embodiment, the masterbatch compound comprises a second polymer and a soil resistance- affecting additive. The first fiber forming polymer is present in a range from about 80 to 99 percent by weight, and the masterbatch compound is present in a range from about 1 to 20 percent by weight. In one nonlimiting embodiment, no additional steps are required to remove volatiles while forming the polymer melt. A synthetic fiber is then formed from this polymer melt. In this embodiment, the soil resistant additive used in the process can be an aromatic sulfonate or an alkali metal salt thereof. Nonlimiting examples include 5-sulfoisophthalic acid, sodium salt and dimethyl-5-sulfoisophthalate, sodium salt.
[0059] Also provided by the present disclosure is a masterbatch compound. The masterbatch compound comprises a thermoplastic carrier, also referred to herein as second polymer.
Examples of thermoplastic carriers useful in the masterbatch include, but are not limited to polyolefins, polylactic acid, polystyrene, or a blend or copolymer thereof. In one nonlimiting embodiment, the thermoplastic carrier is a polyolefin. In one nonlimiting embodiment the thermoplastic carrier is an unmodified polyolefin. In another nonlimiting embodiment, the thermoplastic carrier is polypropylene.
[0060] In one nonlimiting embodiment, the thermoplastic carrier is present in the masterbatch compound in a range from about 40 to about 90 percent by weight. In one nonlimiting embodiment, the masterbatch compound comprises about 50% of the thermoplastic carrier.
[0061] The masterbatch compound further comprises a soil resistance-affecting additive.
Suitable soil resistance-affecting additives include, but are not limited to aromatic sulfonates and alkali metal salts thereof, such as 5-sulfoisophthalic acid, sodium salt and dimethyl-5- sulfoisophthalate, sodium salt. In one nonlimiting embodiment, the soil resistance-affecting additive is present in the masterbatch compound in a range from about 10 to about 60 percent by weight.
[0062] In one nonlimiting embodiment, the masterbatch compound has a moisture content less than about 200 ppm, more preferably less than about 50 ppm. In another nonlimiting
embodiment, the masterbatch compound is not dried or conditioned prior to forming the polymer melt.
[0063] The masterbatch compound may further comprise other additives, to be used to confer additional benefits to articles upon polymer melt extrusion and melt spinning. Examples of such additives are inorganic pigments, and ultraviolet (UV) light absorbers or optical brightening agents. Examples of inorganic pigments are titanium dioxide, barium sulfate, carbon black, manganese dioxide, and zinc oxide. Examples of UV light absorbers or optical brightening agents are 2,2'-(l ,2-ethenediyldi-4,l phenylene)bisbenzoxazole, available commercially by Eastman Chemical Company under the tradename Eastobrite® OB-1, and 2,2'-(2 ,5- thiophenediyl)bis(5-tert-butylbenzoxazole, available commercially by Mayzo, Inc. under the tradename Benetex® OB.
[0064] In one nonlimiting embodiment, the masterbatch compound is present in fiber in a range from about 1 to about 20 percent by weight.
[0065] The present disclosure also relates to articles of manufacture, at least a portion of which comprises a synthetic fiber produced in accordance with this process. Nonlimiting examples include yams prepared from synthetic fibers produced by this process, as well as fabrics and carpets prepared from these synthetic fibers and/or yarns.
[0066] In nonlimiting embodiments, masterbatches were prepared with the following soil resistance-affecting additives:
5-sulfoisophthalic acid, sodium salt Dmiethyl5-sulfoisophthalate, sodium salt
[0067] The masterbatches were added at the extruder hopper to a standard bottle-grade PET resin, at 0.5 wt% and 2 wt% actives. The resultant pigmented trilobal PET fibers were processed and tufted into a 30 oz./sq. yd residential cut pile carpet. It was found that the characteristic stain resistance of PET was not negatively impacted by blending with the soil resistant additive.
Further, Vetterman drum performance was similar to the equivalent control. In Accelerated Drum Soil tests (ASTM D6540-12), however, carpet prepared from fibers of this disclosure containing 4wt% of the masterbatch showed an advantage of 4 - 5.5 ΔΕ units as compared to untreated PET, were equivalent to PET carpet treated with anti-soil chemistry comprising synthetic clay nanoparticles (Laponite ® S482) at 2% owf, and performed better than PET carpet treated with anti-soil chemistry comprising synthetic clay nanoparticles (Laponite ® S482) and fluorochemical (Capstone® RCP) at 1.2% owf. In general a filament in accordance with the present disclosure has an exterior modification ratio (R2/R1) that can be about 1.50 to 3.00, and more particularly can be about 2.15 to 2.85. The modification ratio (MR) for the control items was nominally the same, at 2.5. Modification ratio determinations, in particular for triloba! bulked continuous filaments, are described as disclosed in European Patent 1,518,948, and U.S. Patent Publication 2015 0275400.
[0068] Further testing was performed to confirm that the soil resistant additive of this disclosure does not migrate out of the synthetic fibers on its own, during dyeing processes, or with wet cleaning. Clean carpets were aggressively hot water extracted, and then soiled, to monitor any changes in performance. The sustained anti-soiling performance data indicated that the additive was not leached from the polymer fibers.
[0069] Thus, the synthetic fibers of this disclosure were found to have markedly improved soiling performance in carpet form. Carpets produced from these synthetic fibers have a "built- in," or fiber bound, anti-soil performance that exceeds current fluorochemical-based topical anti- soil treatment in efficacy. Further, this built-in resistance is more durable than topical treatments for anti-soil which are known to "walk off with wear and foot traffic so that the topical chemistry is no longer effective. In addition, using the synthetic fibers of this disclosure ehminates the need for topical application of chemicals by downstream carpet mills. Use of a non-fluoiinated compound to enhance soil resistance also diminishes possible environmental concerns.
[0070] The following sections provide further illustration of the synthetic fiber and fabrics knitted of this invention as well as comparative fibers and fabrics knitted therefrom. These working examples are illustrative only and are not intended to limit the scope of the invention in any way.
TEST METHOD
[0071] Accelerated drum soiling is recorded as Delta E, and measured according to ASTM D6540. Within the reproducibility limitations of this test, the relative soiling performance of variously-treated samples may be determined. The test simulates the soiling of carpet in residential or commercial environments to a traffic count level of about 100,000 to 300,000. According to ASTM D6540, soiling tests can be conducted on up to six carpet samples simultaneously using a drum. The base color of the sample (using the L, a, b color space) is measured using the hand held color measurement instrument sold by Minolta Corporation as "Chromameter" model CR-310 (at Camden). This measurement output is in the form L*, a* and b* values and describes a color value in color space. This is the original color value. The carpet sample is mounted on a thin plastic sheet and placed in the drum. Two hundred fifty grams (250 g) of dirty Zytel 101 nylon beads (by DuPont Canada, Mississauga, Ontario) are placed on the sample. The dirty beads are prepared by mixing ten grams (10 g) of AATCC TM-122 synthetic carpet soil (by Manufacturer Textile Innovators Corp., Windsor, N.C.) with one thousand grams (1000 g) of new Nylon Zytel 101 beads. One thousand grams (1000 g) of ¾-inch diameter steel ball bearings are added into the drum. The drum is run for 30 minutes with direction reversal and the sample removed. After removal the carpet is cleaned with a vacuum cleaner and the chromameter is used again to measure the color of the carpet after cleaning. The difference between the color measurements of each carpet (before and after soiling and cleaning) is the total color difference, ΔΕ*, and is based on L*, a*, and b* color differences in color space, known to those skilled in the field where
[0072]
Figure imgf000012_0001
Figure imgf000012_0002
AATCC TM175 - Stain Resistance: Pile Floor Coverings, and
ASTM D5417 - Vetterman Drum
EXAMPLES
[0073] Comparative Examples 1 , 2, and 5 and Examples 3, 4, 6, and 7 were produced using pilot scale machinery. The pilot equipment included a 12" twin screw extruder having five heating zones, a filter screen pack, any of a selection of desired spinnerets, a fiber quenching zone, godet rolls, and winders. A standard spinning method was used to produce fiber from the pilot scale machinery, as follows: the polymer was extruded through the spinnerets and divided into two 184 filament segments. The molten fibers were then rapidly quenched in a chimney, where cooling air at about 10— 15 °C was blown past the filaments at four hundred and fifty cubic feet per minute [300-600 cfm] through the quench zone. The filaments were then coated with a lubricant for drawing and crimping. The coated yarns were drawn at about 2422 yards per minute (2.9x draw ratio) using a pair of heated draw rolls. The draw roll temperature was 160° C. The filaments were then forwarded into a dual-impingement hot air bulking jet, similar to that described in Coon, U.S. Patent 3,525,134, teachings of which are herein incorporated by reference, to form two BCF yarns (1000 denier, 5.4 dpi). The temperature of the air in the bulking jet was 180 °C.
[0074] The spun, drawn, and crimped BCF yarns were tufted into carpets and heat-set on a Superba heat-setting machine at setting temperature of 290°C. The holdup time in the setting zone was about 60 seconds. The heatset carpets were tested according to standard test methods ASTM D6540 - Accelerated Soiling of Pile Yarn Floor Covering, AATCC TM193 - Aqueous Liquid Repellency, AATCC TM175 - Stain Resistance: Pile Floor Coverings, and ASTM D5417 — Vetterman Drum.
[0075] Comparative Example 1: PET BCF, no melt additive, no topical anti-soil treatment
[0076] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge ftifting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and the FIGs 1-2.
[0077] Comparative Example 2: PET BCF, no melt additive, treated with topical soil resist
[0078] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge tufting machine and an anti-soil treatment was applied by spraying the tufted carpet with an anti-soil chemistry comprising clay nanoparticles (Laponite ® S482, B YK-Chemie GmbH, Wesel, Germany) and fiuorochemical (Capstone® RCP, Chemours Co., Wilmington, DE USA) at 1.2% owf. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
[0079] Example 3: PET BCF, masterbatch additive, 1.0 wt% masterbatch
[0080] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. A masterbatch of polypropylene and sodiosulfonated isophthalic acid, dimethyl ester (1:1 weight ratio) was added in the melt at 1 wt% to a PET polymer product made by Indorama, Spartanburg, SC, USA. The masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
[0081] Example 4: PET BCF, masterbatch additive, 4 wt% masterbatch
[0082] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. A masterbatch of polypropylene and sodiosulfonated isophthalic acid, dimethyl ester (1 : 1 weight ratio) was added in the melt at 4 wt% to a PET polymer product made by Indorama, Spartanburg, SC, USA. The masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 16 stitches per inch, 30 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
[0083] Comparative Example 5: PET BCF, no melt additive, treated with topical soil resist, 50 oz/yd2 carpet
[0084] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. Pigments of various colors were mixed with a PET polymer product made by Indorama, Spartanburg, SC, USA. The pigments and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yam had a wool beige color. It was tufted into carpet having ½" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine and an anti-soil treatment was applied by spraying the tufted carpet with an anti-soil chemistry comprising clay nanoparticles (Laponite ®) and fluorochemicals (Capstone® RCP) at 1.2% owf. The carpet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
[0085] Example 6: PET BCF, masterbatch additive, 1.0 wt% masterbatch
[0086] PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. A masterbatch of polypropylene and sodiosulfonated isophthalic acid, dimethyl ester (1 : 1 weight ratio) was added in the melt at 1 wt% to a PET polymer product made by Indorama, Spartanburg, SC, USA. The masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The carpet was tested for accelerated soiling , stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
[0087] Example 7: PET BCF, masterbatch additive, 4 wt% masterbatch
PET bulked continuous filament (BCF, 1000 denier, 184 filaments) was made on pilot scale machinery. A masterbatch of polypropylene and sodiosulfonated isophthalic acid, dimethyl ester (1:1 weight ratio) was added in the melt at 4 wt% to a PET polymer product made by Indorama, Spartanburg, SC, USA. The masterbatch and PET were mixed at the screw feeder. Fibers were spun with no process breaks. This BCF yarn had a wool beige color. It was tufted into carpet having ½" pile height, 50 oz per square yard cut pile carpet on a 1/8 gauge tufting machine. The caipet was tested for accelerated soiling, stain repellency, and wear resistance as shown in Table 1 and FIGs 1-2.
Table 1. Data summary for Examples 1-7. Values shown are averages on multiple (3-5) measurements.
Figure imgf000015_0001
Figure imgf000016_0001
Table 2. Mechanical properties measured by ASTM D2256 - Yarns - Tensile by Single Strand method (10in).
Figure imgf000016_0002
Figure imgf000017_0001

Claims

What is claimed is:
1. A synthetic fiber comprising:
a) a first fiber forming polymer; and
b) a soil resistance-affecting additive present in the fiber at a range from about 0.1 to 10 percent by weight.
2. The synthetic fiber of claim 1 wherein at least a portion of the soil resistance- affecting additive is present on the surface of the fiber.
3. The synthetic fiber of claim 2 wherein the portion of the soil resistance-affecting additive present on the surface of the fiber is sufficient to impart soil resistant properties to the fiber.
4. The synthetic fiber of claim 1 wherein at least a portion of the soil resistance- affecting additive is not polymerized with first fiber forming polymer.
5. The synthetic fiber of claim 1 wherein at least a portion of the soil resistance- affecting additive has bloomed to the surface of the fiber.
6. The synthetic fiber of any of claims 1 to 5 wherein the fiber has a multilobal cross section and a majority of the soil resistance-affecting additive present on the surface of the fiber is located in the area between the lobes.
7. The synthetic fiber of any of claims 1 to 5, wherein the fiber has a multilobal cross section and at least 75 percent by weight of the soil resistance-affecting additive present on the surface of the fiber is located in the area between the lobes.
8. The synthetic fiber of any of claims 1 to 5 wherein the fiber has a multilobal cross section and substantially all of the soil resistance-affecting additive present on the surface of the fiber is located in the area between the lobes.
9. The synthetic fiber of claim 1 wherein the first fiber fonriing polymer is selected from the group consisting of apolyamide, a polyester, and a polyolefin, and combinations thereof.
10. The synthetic fiber of claim 1 wherein the first fiber forming polymer is a polyester.
11. The synthetic fiber of claim 10 wherein the polyester is selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate and polybutylene terephthalate, and combinations thereof.
12. The synthetic fiber of claim 1 wherein the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof.
13. The synthetic fiber of claim 12 wherein the soil resistance-affecting additive is 5- sulfoisophthalic acid, sodium salt.
14. The synthetic fiber of claim 12 wherein soil resistance-affecting additive is dimethyl 5-sulfoisophthalate, sodium salt.
15. A yarn formed from the synthetic fiber of any of claims 1-14.
16. A carpet formed from the yarn of claim 15.
17. A fabric formed from the synthetic fiber of any of claims 1-14.
18. A synthetic fiber comprising:
(a) a first fiber forming polymer present in a range from about 80 to 99 percent by weight;
(b) a second polymer present in a range from about 0.2 to 10 percent by weight; and
(c) a soil resistance-affecting additive present in the fiber at a range from about 0.1 to 10 percent by weight.
19. The synthetic fiber of claim 18 wherein at least a portion of the soil resistance- affecting additive is present on the surface of the fiber.
20. The synthetic fiber of claim 19 wherein the portion of the soil resistance-affecting additive present on the surface of the fiber is sufficient to impart soil resistant properties to the fiber.
21. The synthetic fiber of claim 19 wherein at least a portion of the soil resistance- affecting additive is not polymerized with first fiber forming polymer.
22. The synthetic fiber of claim 19 wherein at least a portion of the soil resistance- affecting additive has bloomed to the surface of the fiber.
23. The synthetic fiber of any of claims 18 to 22 wherein the fiber has a multilobal cross section and a majority of the soil resistance-affecting additive present on the surface of the fiber is located in the area between the lobes.
24. The synthetic fiber of any of claims 18 to 22 wherein the fiber has a multilobal cross section and at least 75 percent by weight of the soil resistance-affecting additive present on the surface of the fiber is located in the area between the lobes.
25. The synthetic fiber of claim 18 wherein the second polymer has a melting point which is less than the melting point of the first fiber forming polymer.
26. The synthetic fiber of claim 18 wherein the presence of the second polymer does not cause the synthetic fiber to fibrillate.
27. The synthetic fiber of claim 18 wherein the first fiber forming polymer is selected from the group consisting of a polyamide. a polyester, and a polyolefin, and combinations thereof.
28. The synthetic fiber of claim 18 wherein the first fiber forming polymer is selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate, and polybutylene terephthalate, and combinations thereof.
29. The synthetic fiber of claim 18 wherein the second polymer is selected from the group consisting of a polyolefin, a polylactic acid and a polystyrene, and combinations thereof.
30. The synthetic fiber of claim 18 wherein the second polymer is an unmodified polyolefin.
31. The synthetic fiber of claim 18 wherein the second polymer is polypropylene.
32. The synthetic fiber of claim 18 wherein the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof.
33. The synthetic fiber of claim 32 wherein the soil resistance-affecting additive is 5- sulfoisophthalic acid, sodium salt.
34. The synthetic fiber of claim 32 wherein soil resistance-affecting additive is dimethyl 5-sulfoisophthalate, sodium salt.
35. A yarn formed from the synthetic fiber of any of claims 18-34.
36. A carpet formed from the yarn of claim 34.
37. A fabric formed from the synthetic fiber of any of claims 18-34.
38. A process for forming a synthetic fiber, said process comprising the steps of: a) foitnitig a polymer melt comprising a first fiber foiming polymer and a masterbatch compound, wherein the masterbatch compound comprises a second polymer and a soil resistance-affecting additive, and wherein the first fiber fonriitig polymer is present in a range from about 80 to 99 percent by weight, and the masterbatch compound is present in a range from about 0.2 to 20 percent by weight; and b) forming a synthetic fiber from the polymer melt.
39. The process of claim 38 wherein at least a portion of the soil resistance-affecting additive is present on the surface of the fiber.
40. The process of claim 39 wherein the portion of the soil resistance-affecting additive present on the surface of the fiber is sufficient to impart soil resistant properties to the fiber.
41. The process of claim 38 wherein the masterbatch compound has a moisture content less than about 200 ppm.
42. The process of claim 38 wherein the masterbatch compound has a moisture content less than about 50 ppm.
43. The process of claim 38 wherein the masterbatch compound is not dried or conditioned prior to forming the polymer melt.
44. The process of claim 38 wherein no additional step is required to remove volatiles while forming the polymer melt.
45. The process of claim 38 wherein the second polymer has a melting point which is less than the melting point of the first fiber forming polymer.
46. The process of claim 38 wherein the presence of the second polymer does not cause the synthetic fiber to fibrillate.
47. The process of claim 38 wherein the second polymer is present in the masterbatch compound in a range from about 20 to 80 percent by weight.
48. The process of claim 38 wherein the second polymer is selected from the group consisting of a polyolefm, a polylactic acid and a polystyrene, and combinations thereof.
49. The process of claim 38 wherein the second polymer is an unmodified polyolefin.
50. The process of claim 38 wherein the second polymer is polypropylene.
51. The process of claim 38 wherein the first fiber forairng polymer is selected from the group consisting of a polyamide, a polyester, and a polyolefin, and combinations thereof.
52. The process of claim 38 wherein the first fiber forming polymer is polyethylene terephthalate.
53. The process of claim 38 wherein the soil resistance-affecting additive is present in the masterbatch compound in a range from about 20 to 80 percent by weight.
54. The process of claim 38 wherein the soil resistance-affecting additive is an aromatic sulfonate or an alkali metal salt thereof.
55. The process of claim 38 wherein the soil resistance-affecting additive is 5- sulfoisophthalic acid, sodium salt.
56. The process of claim 38 wherein soil resistance-affecting additive is dimethyl 5- sulfoisophthalate, sodium salt.
57. A synthetic fiber formed from the process of any of claims 38-56.
58. A fabric formed from the synthetic fiber of claim 57.
59. A yarn formed from the synthetic fiber of claim 57.
60. A carpet formed from the yarn of claim 59.
PCT/US2016/030967 2015-05-05 2016-05-05 Synthetic fibers with enhanced soil resistance and methods for production and use thereof WO2016179384A1 (en)

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AU2016258018A AU2016258018B2 (en) 2015-05-05 2016-05-05 Synthetic fibers with enhanced soil resistance and methods for production and use thereof
EP16727002.4A EP3292234A1 (en) 2015-05-05 2016-05-05 Synthetic fibers with enhanced soil resistance and methods for production and use thereof
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