US20200208314A1 - Semi-continuous filaments including a crystalline polyolefin and a hydrocarbon tackifier resin, and process for making same - Google Patents

Semi-continuous filaments including a crystalline polyolefin and a hydrocarbon tackifier resin, and process for making same Download PDF

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Publication number
US20200208314A1
US20200208314A1 US16/631,443 US201816631443A US2020208314A1 US 20200208314 A1 US20200208314 A1 US 20200208314A1 US 201816631443 A US201816631443 A US 201816631443A US 2020208314 A1 US2020208314 A1 US 2020208314A1
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Prior art keywords
nonwoven web
filaments
semi
filament
particulates
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US16/631,443
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English (en)
Inventor
Eugene G. Joseph
Saurabh Batra
Michael R. Berrigan
John D. Stelter
Jacob J. Thelen
Zackary J. Becker
Liyun Ren
Sachin Talwar
Michael D. Romano
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3M Innovative Properties Co
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3M Innovative Properties Co
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Priority to US16/631,443 priority Critical patent/US20200208314A1/en
Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BERRIGAN, MICHAEL R., BECKER, Zackary J., TALWAR, Sachin, THELEN, Jacob J., JOSEPH, EUGENE G., STELTER, JOHN D., BATRA, Saurabh, REN, Liyun, ROMANO, MICHAEL D.
Publication of US20200208314A1 publication Critical patent/US20200208314A1/en
Abandoned legal-status Critical Current

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Classifications

    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282Addition polymers
    • D04H1/4291Olefin series
    • 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
    • D01D5/08Melt spinning methods
    • 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
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/08Melt spinning methods
    • D01D5/098Melt spinning methods with simultaneous stretching
    • D01D5/0985Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
    • 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
    • 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
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005Synthetic yarns or filaments
    • D04H3/007Addition polymers

Definitions

  • the present disclosure relates to semi-continuous filaments including a crystalline polyolefin (co)polymer and a hydrocarbon tackifier resin, and more particularly, to nonwoven webs including such filaments, and methods for preparing such nonwoven webs.
  • Melt-spinning is a process for forming nonwoven webs of thermoplastic (co)polymeric filaments.
  • one or more thermoplastic (co)polymer streams are extruded through a die containing one or more orifices and attenuated form micro-filaments, which are collected to form a melt-spun nonwoven web.
  • melt-spun nonwoven webs include polyethylene (PE) and polypropylene (PP).
  • PE polyethylene
  • PP polypropylene
  • Melt-spun nonwoven webs are used in a variety of applications, including acoustic and thermal insulation, filtration media, surgical drapes, and wipes, among others.
  • the present disclosure describes a nonwoven web including at least one semi-continuous filament including from about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w of at least one hydrocarbon tackifier resin.
  • the at least one semi-continuous filament exhibits molecular orientation, and the nonwoven web exhibits a Heat of Fusion measured using Differential Scanning Calorimetry of greater than 50 Joules/g.
  • the at least one semi-continuous filament comprises a plurality of melt-spun filaments.
  • the at least one semi-continuous filament is subjected to a filament bonding step before, during, or after collection, thereby forming a spun-bond web.
  • the at least one crystalline polyolefin (co)polymer is selected from polyethylene, isotactic polypropylene, syndiotactic polypropylene, isotactic polybutylene, syndiotactic polybutylene, poly-4-methyl pentene), and mixtures thereof.
  • the at least one crystalline polyolefin (co)polymer exhibits a Heat of Fusion measured using Differential Scanning Calorimetry of greater than 50 Joules/g.
  • the at least one crystalline polyolefin (co)polymer is selected to be isotactic polypropylene, syndiotactic polypropylene, and mixtures thereof.
  • the at least one hydrocarbon tackifier resin is a saturated hydrocarbon.
  • the at least one hydrocarbon tackifier resin is selected from C 5 piperylene derivatives, C 9 resin oil derivatives, and mixtures thereof.
  • the at least one hydrocarbon tackifier resin makes up from 2% to 40% by weight of the (co)polymeric filaments, more preferably from 5% to 30% by weight of the (co)polymeric filaments, even more preferably from 7% to 20% by weight of the (co)polymeric filaments.
  • the filaments further include between about 0 to 30% w/w of at least one plasticizer.
  • the at least one plasticizer is selected from oligomers of C 5 to C 14 olefins, and mixtures thereof.
  • the multiplicity of filaments exhibits a mean Actual Filament Diameter of less than 5 micrometers as determined using the Optical Microscopy Test as described herein. In other exemplary embodiments, the multiplicity of melt-spun filaments exhibits a mean Actual Filament Diameter of from about 1 micrometer to about 50 micrometers, inclusive; more preferably from 3 micrometers to 20 micrometers, inclusive; from 4 micrometers to 10 micrometers, inclusive; as determined using the Optical Microscopy Test described herein. 15.
  • the nonwoven web exhibits a Stiffness of at least 800 mg as measured using the Stiffness Test as described herein.
  • the present disclosure describes a process for making a nonwoven web made up of at least one semi-continuous filament, the process including heating a mixture of about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w of at least one hydrocarbon tackifier resin to at least a Melting Temperature of the mixture to form a molten mixture, extruding the molten mixture through at least one orifice to form at least one semi-continuous filament, attenuating the at least one semi-continuous filament to draw and molecularly orient the at least one semi-continuous filament, and then cooling the at least one semi-continuous filament to a temperature below the Melting Temperature of the molten mixture to form a nonwoven web,
  • the at least one semi-continuous filament exhibits molecular orientation, and at least one of the crystalline polyolefin (co)polymer or the nonwoven web exhibits
  • the at least one semi-continuous filament comprises a plurality of semi-continuous filaments
  • the process further includes collecting the plurality of semi-continuous filaments as the nonwoven web on a collector.
  • the plurality of semi-continuous filaments is comprised of melt-spun filaments.
  • the melt-spun filaments are subjected to a filament bonding step before, during, or after collection, thereby producing a spun-bond nonwoven web.
  • the process further includes at least one of addition of a plurality of staple filaments to the plurality of semi-continuous filaments, or addition of a plurality of particulates to the plurality of semi-continuous filaments.
  • the process further includes processing the collected nonwoven web using a process selected from autogenous bonding, through-air bonding, electret charging, embossing, needle-punching, needle tacking, hydroentangling, or a combination thereof.
  • Exemplary embodiments according to the present disclosure may have certain surprising and unexpected advantages over the art.
  • One such advantage of exemplary embodiments of the present disclosure relates to increased tensile strength exhibited by the webs, even when prepared at low Basis Weight (i.e., less than or equal to 50 g/m 2 , “gsm”).
  • Increased tensile strength for low Basis Weight webs is important for many insulation applications, for example, thermal or acoustic insulation, more particularly acoustic or thermal insulation mats used in motor vehicles (e.g., aircraft, trains, automobiles, trucks, ships, and submersibles).
  • exemplary nonwoven webs as described herein may advantageously exhibit a Maximum Load in the Machine Direction Maximum Tensile Load in the Machine Direction as measured with the Tensile Strength Test as defined herein, of at least 40 Newtons (N), at least 50 N, at least 75 N, at least 100 N, at least 125 N, or even at least 150 N; and generally no greater than 1,000 N, 750 N, 500 N, or 250 N.
  • N Maximum Load in the Machine Direction Maximum Tensile Load in the Machine Direction as measured with the Tensile Strength Test as defined herein, of at least 40 Newtons (N), at least 50 N, at least 75 N, at least 100 N, at least 125 N, or even at least 150 N; and generally no greater than 1,000 N, 750 N, 500 N, or 250 N.
  • the nonwoven webs as described herein may advantageously exhibit improved Stiffness, as evidenced by a Stiffness measured with the
  • Stiffness Test as defined herein, of at least 800 mg, 900 mg, 1,000 mg, 1500 mg, or even 2,000 mg; and generally no greater than 5,000 mg, 4,000 mg, 3,000 mg, or 2,500 mg.
  • the nonwoven webs exhibit a Basis Weight of from 1 g/m 2 (gsm) to 400 gsm, more preferably from 1 gsm to 200 gsm, even more preferably from 1 gsm to 100 gsm, or even 1 gsm to about 50 gsm.
  • Another advantage of exemplary embodiments relates to an increased ability to stretch the filaments by increasing the attenuation pressure without filament breakage, thus leading to higher filament spinning speeds and smaller diameter filaments.
  • this may also advantageously limit or eliminate the possibility of newly formed filaments breaking and forming filament fragments ((i.e., “fly”) which can fall onto the collected nonwoven web and degrade the appearance of the web where they land.
  • An additional advantage of exemplary embodiments relates to an ability to use a higher melt temperature for the melt-spun process, which leads to a lower mean Actual Filament Diameter (AFD) of about 5 micrometers or less, and may even permit the production of sub-micrometer filaments (i.e., nanofilaments) having a mean Actual Filament Diameter (AFD) of less than one micrometer.
  • AFD Average Actual Filament Diameter
  • Such nonwoven webs including sub-micrometer filaments achieve better acoustic and/or thermal insulation performance at equal or lower Basis Weight than comparable microfilament webs, thus leading to improved insulation performance at a lower production cost.
  • Embodiments of the present disclosure may also exhibit higher production rates due to the lower melt viscosities achieved during melt-spinning of the filaments.
  • a nonwoven web comprising:
  • At least one semi-continuous filament comprising from about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer
  • Embodiment B The nonwoven web of Embodiment A or any following Embodiment, wherein the at least one crystalline polyolefin (co)polymer is selected from the group consisting of polyethylene, isotactic polypropylene, syndiotactic polypropylene, isotactic polybutylene, syndiotactic polybutylene, poly-4-methyl pentene, and mixtures thereof.
  • C The nonwoven web Embodiment B, wherein the at least one crystalline polyolefin (co)polymer exhibits a Heat of Fusion measured using Differential Scanning Calorimetry of greater than 50 Joules/g, D.
  • the nonwoven web of Embodiment G wherein the at least one hydrocarbon tackifier resin makes up from 7% to 20% by weight of the (co)polymeric filaments.
  • I The nonwoven web of any preceding or following Embodiment, further comprising between about 0 to 30% of at least one plasticizer.
  • J The nonwoven web of Embodiment H, wherein the at least one plasticizer is selected from the group consisting of oligomers of C 5 to C 14 olefins, and mixtures thereof.
  • K. The nonwoven web of any preceding or following Embodiment, wherein the nonwoven web exhibits a Maximum Load in the Machine Direction of at least 40 Newtons as measured using the Tensile Strength Test described herein.
  • L The nonwoven web of any preceding or following Embodiment, wherein the nonwoven web exhibits a Maximum Load in the Machine Direction of at least 40 Newtons as measured using the Tensile Strength Test described herein.
  • N The melt-spun nonwoven web of any preceding Embodiment, wherein the plurality of (co)polymeric filaments exhibits a mean Actual Filament Diameter of less than five micrometers as determined using the Optical Microscopy Test described herein.
  • a process for making a melt-spun nonwoven web comprising:
  • Embodiment S further comprising processing the collected nonwoven web using a process selected from the group consisting of autogenous bonding, through-air bonding, electret charging, calendering, embossing, needle-punching, needle tacking, hydroentangling, or a combination thereof.
  • (co)polymer or “(co)polymers” includes homopolymers and copolymers, as well as homopolymers or copolymers that may be formed in a miscible blend, e.g., by coextrusion or by reaction, including, e.g., transesterification.
  • copolymer includes random, block and star (e.g. dendritic) copolymers.
  • molecularly same (co)polymer means one or more (co)polymers that have essentially the same repeating molecular unit, but which may differ in molecular weight, method of manufacture, commercial form, and the like.
  • homogeneous means exhibiting only a single phase of matter when observed at a macroscopic scale.
  • Actual Filament Diameter or “AFD” means the mean number diameter determined by measuring 20 individual filaments using the Optical Microscopy Test described herein.
  • Effective Filament Diameter means the apparent diameter of the filaments in a nonwoven web based on an air permeation test in which air at 1 atmosphere and room temperature is passed at a face velocity of 5.3 cm/sec through a web sample of known thickness, and the corresponding pressure drop is measured. Based on the measured pressure drop, the Effective Filament Diameter is calculated as set forth in Davies, C. N., The Separation of Airborne Dust and Particles , Institution of Mechanical Engineers, London Proceedings, 1B (1952).
  • microfilaments means a population of filaments having a mean AFD of at least one micrometer ( ⁇ m) and preferably less than 1,000 ⁇ m.
  • microfilaments means a population of microfilaments having a mean AFD of at least 10 ⁇ m and preferably less than or equal to 100 ⁇ m.
  • fine microfilaments means a population of microfilaments having a mean AFD of from one ⁇ m to 20 ⁇ m, inclusive.
  • ultrafilaments means a population of microfilaments having a mean AFD of from one ⁇ m to 10 ⁇ m, inclusive.
  • sub-micrometer filaments means a population of filaments having a mean AFD of less than 1 ⁇ m.
  • filaments means a population of filaments having a mean AFD of less than 1 ⁇ m.
  • filament is of finite but indeterminate length, the length of the filament being on the order of at least a factor of 1,000; 5,000; 10,000; 50,000; 100,000; or more times the Actual Fiber Diameter.
  • molecularly orient and “molecular orientation” with reference to a single filament means that at least a substantial portion of the (co)polymer molecules making up the filament are aligned along the longitudinal axis of the filament.
  • a particle or particulate means a small distinct piece or individual part of a material in finely divided form.
  • a particulate may also include a collection of individual particles associated or clustered together in finely divided form.
  • individual particles used in certain exemplary embodiments of the present disclosure may clump, physically intermesh, electro-statically associate, or otherwise associate to form particulates.
  • particulates in the form of agglomerates of individual particles may be intentionally formed such as those described in U.S. Pat. No. 5,332,426 (Tang et al.).
  • nonwoven web means a web characterized by entanglement or point bonding of at least one semi-continuous filament and preferably a plurality of semi-continuous filaments.
  • particle-loaded nonwoven web means a composite nonwoven web containing particles bonded to the filaments or enmeshed among the filaments, the particles optionally being absorbent and/or adsorbent.
  • melt-spinning and “spun-bonding” mean processes for forming a nonwoven web by extruding a filament-forming material through one or more orifices to form at least one semi-continuous filament, attenuating the at least one semi-continuous filament by drawing the filament, and thereafter collecting a layer of the attenuated at least one semi-continuous filament, and, for spun-bonding, bonding the attenuated at least one semi-continuous filament before, during and/or after collection on a collector.
  • die means a processing assembly including one or more orifices for use in a process for extruding a molten (co)polymer mixture to form one or more semi-continuous filament(s), such process including but not limited to melt-spinning and/or spun-bonding processes.
  • melt-spun filament(s) means one or more semi-continuous filament(s) prepared using a melt-spinning process.
  • spun-bond filaments(s) means one or more semi-continuous filament(s) prepared using a melt-spinning process, wherein the one or more semi-continuous filament(s) are bonded together at one or more contact points along the surface(s) of the filament(s).
  • rollers means a process of passing a nonwoven web through rollers to obtain a compressed material.
  • the rollers may optionally be heated, in which case bonding together of the components of the nonwoven web may be achieved.
  • autogenous bonding means bonding between filaments at an elevated temperature as obtained in an oven or with a through-air bonder without application of solid contact pressure such as in point-bonding or calendering.
  • Densification means a process whereby filaments which have been deposited either directly or indirectly onto a filter winding arbor or mandrel are compressed, either before or after the deposition, and made to form an area, generally or locally, of lower porosity, whether by design or as an artifact of some process of handling the forming or formed filter. Densification also includes the process of calendering webs.
  • machine direction means the longitudinal direction in which a nonwoven web of indeterminate length is moved or wound onto a collector, and is distinguished from the “cross-web” direction, which is the lateral direction extending between the two lateral edges of the nonwoven web.
  • cross-web direction is orthogonal to the machine direction for a rectangular nonwoven web.
  • Web Basis Weight is calculated from the weight of a 10 cm ⁇ 10 cm web sample.
  • Web Thickness is measured on a 10 cm ⁇ 10 cm web sample using a thickness testing gauge having a tester foot with dimensions of 5 cm ⁇ 12.5 cm at an applied pressure of 150 Pa.
  • Polymer Density is the mass per unit volume of the (co)polymer or (co)polymer blend that is used to form the nonwoven filaments of a nonwoven web.
  • the Polymer Density for a (co)polymer may generally be found in the literature, and the Polymer Density of a (co)polymer blend may be calculated from the weighted average of the component (co)polymer Polymer Densities, based upon the weight percentages of the individual (co)polymers used to make up the (co)polymer blend.
  • the Polymer Density of polypropylene resin is 0.91 g/cm 3 and the Polymer Density of the hydrocarbon tackifier resins used herein is about 1.00 g/cm 3 .
  • Solidity provided herein using the following formula, a Polymer Density of 0.91 g/cm 3 was used.
  • Melting Temperature is the highest magnitude peak among principal and any secondary endothermic melting peaks in a cooling after first heating heat flow curve plotted as a function of temperature, as obtained using Differential Scanning Calorimetry (DSC).
  • joining with reference to a particular layer in a multi-layer nonwoven web means joined with or attached to another layer, in a position wherein the two layers are either next to (i.e., adjacent to) and directly contacting each other, or contiguous with each other but not in direct contact (i.e., there are one or more additional layers intervening between the layers).
  • a viscosity of “about” 1 Pa-sec refers to a viscosity from 0.95 to 1.05 Pa-sec, but also expressly includes a viscosity of exactly 1 Pa-sec.
  • a perimeter that is “substantially square” is intended to describe a geometric shape having four lateral edges in which each lateral edge has a length which is from 95% to 105% of the length of any other lateral edge, but which also includes a geometric shape in which each lateral edge has exactly the same length.
  • orientation such as “atop”, “on”, “over,” “covering”, “uppermost”, “underlying” and the like for the location of various elements in the disclosed coated articles, we refer to the relative position of an element with respect to a horizontally-disposed, upwardly-facing substrate. However, unless otherwise indicated, it is not intended that the substrate or articles should have any particular orientation in space during or after manufacture.
  • the disclosure describes a nonwoven web comprising at least one semi-continuous filament including from about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w of at least one hydrocarbon tackifier resin, wherein the at least one semi-continuous filament exhibits molecular orientation, and further wherein the nonwoven web exhibits a Heat of Fusion measured using Differential Scanning Calorimetry of greater than 50 Joules/g.
  • the nonwoven webs as described herein may advantageously exhibit improved tensile strength, as evidenced by a Maximum Tensile Load in the Machine Direction as measured with the Tensile Strength Test as defined herein, of at least 40 Newtons (N), at least 50 N, at least 75 N, at least 100 N, at least 125 N, or even at least 150 N; and generally no greater than 1,000 N, 750 N, 500 N, or 250 N.
  • the semi-continuous filaments in the non-woven fibrous webs or composite webs may advantageously exhibit a mean Actual Filament Diameter (determined using the test method described below) of from about 1 micrometer to about 50 micrometers ( ⁇ m), inclusive; more preferably from 3 ⁇ m to 20 ⁇ m, inclusive; even more preferably from about 4 ⁇ m to about 10 ⁇ m or even to about 9 ⁇ m, 8 ⁇ m, 7 ⁇ m, 6 ⁇ m, or even 5 ⁇ m, inclusive.
  • the nonwoven web may take a variety of forms, including mats, webs, sheets, scrims, fabrics, and a combination thereof.
  • Nonwoven webs of the present disclosure comprise semi-continuous filaments comprising from about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w at least one hydrocarbon tackifier resin.
  • a single crystalline polyolefin (co)polymer) may be mixed with a single hydrocarbon tackifier resin.
  • a single crystalline polyolefin (co)polymer may be advantageously mixed with two or more hydrocarbon tackifier resins.
  • two or more crystalline polyolefin (co)polymers may be mixed with a single hydrocarbon tackifier resin.
  • two or more crystalline polyolefin (co)polymers may be advantageously mixed with two or more hydrocarbon tackifier resins.
  • the crystalline polyolefin (co)polymers useful in practicing embodiments of the present disclosure are generally crystalline polyolefin (co)polymers with a moderate level of crystallinity.
  • (co)polymer crystallinity arises from stereoregular sequences in the (co)polymer, for example stereoregular ethylene, propylene, or butylene sequences.
  • the (co)polymer can be: (A) a propylene homopolymer in which the stereoregularity is disrupted in some manner such as by regio-inversions; (B) a random propylene copolymer in which the propylene stereoregularity is disrupted at least in part by co-monomers; or (C) a combination of (A) and (B).
  • the crystalline polyolefin (co)polymer is a (co)polymer that includes a non-conjugated diene monomer to aid in vulcanization and other chemical modification of the blend composition.
  • the amount of diene present in the (co)polymer is preferably less than 10% by weight, and more preferably less than 5% by weight.
  • the diene may be any non-conjugated diene which is commonly used for the vulcanization of ethylene propylene rubbers including, but not limited to, ethylidene norbornene, vinyl norbornene, and dicyclopentadiene.
  • the crystalline polyolefin (co)polymer is a random copolymer of propylene and at least one co-monomer selected from ethylene, C 4 -C 12 alpha-olefins, and combinations thereof.
  • the copolymer includes ethylene-derived units in an amount ranging from a lower limit of 2%, 5%, 6%, 8%, or 10% by weight to an upper limit of 20%, 25%, or 28% by weight.
  • This embodiment also includes propylene-derived units present in the copolymer in an amount ranging from a lower limit of 72%, 75%, or 80% by weight to an upper limit of 98%, 95%, 94%, 92%, or 90% by weight. These percentages by weight are based on the total weight of the propylene and ethylene-derived units; i.e., based on the sum of weight percent propylene-derived units and weight percent ethylene-derived units being 100%.
  • the crystalline polyolefin (co)polymer is a random propylene copolymer having a narrow compositional distribution.
  • the crystalline polyolefin (co)polymer is a random propylene copolymer exhibiting a Heat of Fusion determined using DSC of greater than 50 J/g.
  • the copolymer is described as random because for a copolymer comprising propylene, co-monomer, and optionally diene, the number and distribution of co-monomer residues is consistent with the random statistical polymerization of the monomers.
  • the number of block monomer residues of any one kind adjacent to one another is greater than predicted from a statistical distribution in random copolymers with a similar composition.
  • Historical ethylene-propylene copolymers with stereoblock structure have a distribution of ethylene residues consistent with these blocky structures rather than a random statistical distribution of the monomer residues in the (co)polymer.
  • the intramolecular composition distribution (i.e., randomness) of the copolymer may be determined by 13 C NMR, which locates the co-monomer residues in relation to the neighboring propylene residues.
  • the crystallinity of the crystalline polyolefin (co)polymers may be expressed in terms of heat of fusion.
  • Embodiments of the present disclosure include crystalline polyolefin (co)polymers exhibiting a heat of fusion as determined using differential scanning Calorimetry (DSC) greater than 50 J/g, greater than 51 J/g, greater than 55 J/g, greater than 60 J/g, greater than 70 J/g, greater than 80 J/g, greater than 90 J/g, greater than 100 J/g, or even about 110 J/g.
  • DSC differential scanning Calorimetry
  • the crystalline polyolefin (co)polymers exhibit a heat of fusion as determined using DSC less than 210 J/g, less than 200 J/g, less than 190 J/g, less than 180 J/g. less than 170 J/g. less than 160 J/g, less than 150 J/g, less than 140 J/g, less than 130 J/g, less than 120 J/g, less than 110 J/g, or even less than 100 J/g.
  • the (co)polymer has a single Melting Point.
  • a sample of propylene (co)polymer will show secondary melting peaks adjacent to the principal peak, which are considered together as a single Melting Point. The highest of these peaks is considered to be the Melting Point.
  • the crystalline polyolefin (co)polymer preferably has a melting point determined using DSC ranging from an upper limit of 300° C., 275° C., 250° C., 200° C., 175° C., 150° C., 125° C., 110° C., or even about 105° C., to a lower limit of about 105° C., 110° C., 120° C., 125° C., 130° C., 140° C., 150° C., 160° C., 175, 180° C., 190° C., 200° C., 225° C., or even about 250° C.
  • the crystalline polyolefin (co)polymers used in the disclosure generally have a weight average molecular weight (Mw) within the range having an upper limit of 5,000,000 Daltons (Da or g/mol), 1,000,000 Da, or 500,000 Da, and a lower limit of 10,000 Da, 20,000 Da, or 80,000 Da, and a molecular weight distribution W w /W n (MWD), sometimes referred to as a “polydispersity index” (PDI), ranging from a lower limit of 1.5, 1.8, or 2.0 to an upper limit of 40, 20, 10, 5, or 4.5.
  • Mw and MWD as used herein, can be determined by a variety of methods, including those in U.S. Pat. No.
  • At least one crystalline polyolefin (co)polymer is generally present in an amount from about 50% w/w (50.0% w/w, 55% w/w, 60% w/w, 65% w/w, 70% w/w, 75% w/w, 80% w/w, 85% w/w, or even about 90% w/w) to about 99% w/w (99.0% w/w, 98% w/w 97% w/w, 96% w/w, 95% w/w, 90% w/w, 85% w/w, 80% w/w, 75% w/w, 70% w/w, 65% w/w, or even about 60% w/w) based on the total weight of the composition.
  • the hydrocarbon tackifier resin is selected to be miscible (i.e., forms a homogenous melt) with the crystalline polyolefin (co)polymer(s) when the mixture is in a molten state, that is, when the mixture of the at least one crystalline polyolefin (co)polymer and the at least one hydrocarbon tackifier resin is heated to a temperature at or above the Melting Temperature (as determined using DSC) of the mixture.
  • suitable petroleum resins include, but are not limited to aliphatic hydrocarbon tackifier resins, hydrogenated aliphatic hydrocarbon tackifier resins, mixed aliphatic and aromatic hydrocarbon tackifier resins, hydrogenated mixed aliphatic and aromatic hydrocarbon tackifier resins, cycloaliphatic hydrocarbon tackifier resins, hydrogenated cycloaliphatic resins, mixed cycloaliphatic and aromatic hydrocarbon tackifier resins, hydrogenated mixed cycloaliphatic and aromatic hydrocarbon tackifier resins, aromatic hydrocarbon tackifier resins, substituted aromatic hydrocarbons, and hydrogenated aromatic hydrocarbon tackifier resins.
  • the hydrocarbon tackifier resin has a number average molecular weight (M n ) within the range having an upper limit of 5,000 Da, or 2,000 Da, or 1,000 Da, and a lower limit of 200 Da, or 400 Da, or 500 Da; a weight average molecular weight (M w ) ranging from 500 Da to 10,000 Da or 600 to 5,000 Da or 700 to 4,000 Da; a Z average molecular weight (M z ) ranging from 500 Da to 10,000 Da, and a polydispersity index (PDI) as measured by M w /M n , of from 1.5 to 3.5, where M n , M w , and M z are determined using size exclusion chromatography (SEC), or as provided by the supplier.
  • M n number average molecular weight
  • M w weight average molecular weight
  • M z Z average molecular weight
  • PDI polydispersity index
  • the hydrocarbon tackifier resin has a lower molecular weight than the crystalline polyolefin (co)polymer.
  • hydrocarbon tackifier resins of the present disclosure are generally selected to be miscible with the crystalline polyolefin (co)polymer in a molten state.
  • Hydrocarbon tackifier resins useful in embodiments of the present disclosure may have a softening point within the range having an upper limit of 180° C., 150° C., or 140° C., and a lower limit of 80° C., 120° C., or 125° C. Softening point (° C.) is measured using a ring and ball softening point device according to AS 198 E-28 (Revision 1996).
  • the hydrocarbon tackifier resin is a saturated hydrocarbon.
  • the hydrocarbon tackifier resin is selected from C 5 piperylene derivatives, C 9 resin oil derivatives, and mixtures thereof.
  • the hydrocarbon tackifier resin makes up from about 2% w/w (2.0% w/w, 3% w/w, 4% w/w, 5% w/w, 10% w/w, 15% w/w, 20% w/w) to about 40% (40.0% w/w, 35% w/w, 30% w/w, or even 25% w/w) based on the weight of the (co)polymeric filaments in the nonwoven web, more preferably from 5% to 30% by weight of the (co)polymeric filaments, even more preferably from 7% to 20% by weight of the (co)polymeric filaments.
  • the nonwoven webs of the present disclosure may further comprise one or more optional components.
  • the optional components may be used alone or in any combination suitable for the end-use application of the nonwoven webs.
  • Three non-limiting, currently preferred optional components include optional electret filament components, optional non-melt-spun filament components, and optional particulate components as described further below.
  • the (co)polymeric filaments further include a plasticizer in an amount between about 0% to about 30% w/w of the filament composition, more preferably from 1% to 20% w/w, 1% to 10% w/w, 1% to 5%, or even 1% to 2.5%.
  • the plasticizer is selected from oligomers of C 5 to C 14 olefins, and mixtures thereof.
  • suitable commercially available plasticizers includes SHF and SUPEERSYNTM available from Exxon-Mobil Chemical Company (Houston, Tex.); STNFLUIDTM available from Chevron-Phillips Chemical Co.
  • the nonwoven webs of the present disclosure may optionally comprise electret filaments.
  • Suitable electret filaments are described in U.S. Pat. Nos. 4,215,682; 5,641,555; 5,643,507; 5,658,640; 5,658,641; 6,420,024; 6,645,618, 6,849,329; and 7,691,168, the entire disclosures of which are incorporated herein by reference.
  • Suitable electret filaments may be produced by meltblowing filaments in an electric field, e.g. by melting a suitable dielectric material such as a (co)polymer or wax that contains polar molecules, passing the molten material through a melt-spinning die to form discrete filaments, and then allowing the molten (co)polymer to re-solidify while the discrete filaments are exposed to a powerful electrostatic field.
  • Electret filaments may also be made by embedding excess charges into a highly insulating dielectric material such as a (co)polymer or wax, e.g. by means of an electron beam, a corona discharge, injection from an electron, electric breakdown across a gap or a dielectric barrier, and the like.
  • Particularly suitable electret filaments are hydro-charged filaments.
  • the nonwoven web optionally further comprises a plurality of non-melt-spun filaments.
  • the nonwoven web may additionally comprise discrete non-melt-spun filaments.
  • the discrete non-melt-spun filaments are staple filaments.
  • the discrete non-melt-spun filaments act as filling filaments, e.g. to reduce the cost or improve the properties of the melt-spun nonwoven web.
  • Non-limiting examples of suitable non-melt-spun filling filaments include single component synthetic filaments, semi-synthetic filaments, polymeric filaments, metal filaments, carbon filaments, ceramic filaments, and natural filaments.
  • Synthetic and/or semi-synthetic polymeric filaments include those made of polyester (e.g., polyethylene terephthalate), nylon (e.g., hexamethylene adipamide, polycaprolactam), polypropylene, acrylic (formed from a (co)polymer of acrylonitrile), rayon, cellulose acetate, polyvinylidene chloride-vinyl chloride copolymers, vinyl chloride-acrylonitrile copolymers, and the like.
  • Non-limiting examples of suitable metal filaments include filaments made from any metal or metal alloy, for example, iron, titanium, tungsten, platinum, copper, nickel, cobalt, and the like.
  • Non-limiting examples of suitable carbon filaments include graphite filaments, activated carbon filaments, poly(acrylonitrile)-derived carbon filaments, and the like.
  • Non-limiting examples of suitable ceramic filaments include any metal oxide, metal carbide, or metal nitride, including but not limited to silicon oxide, aluminum oxide, zirconium oxide, silicon carbide, tungsten carbide, silicon nitride, and the like.
  • Non-limiting examples of suitable natural filaments include those of bamboo, cotton, wool, jute, agave, sisal, coconut, soybean, hemp, and the like.
  • the filament component used may be virgin filaments or recycled waste filaments, for example, recycled filaments reclaimed from garment cuttings, carpet manufacturing, filament manufacturing, textile processing, or the like.
  • the size and amount of discrete non-melt-spun filling filaments, if included, used to form the nonwoven web, will generally depend on the desired properties (i.e., loftiness, openness, softness, drapability) of the nonwoven web 100 and the desired loading of the chemically active particulate. Generally, the larger the filament diameter, the larger the filament length, and the presence of a crimp in the filaments will result in a more open and lofty nonwoven article. Generally, small and shorter filaments will result in a more compact nonwoven article.
  • the nonwoven web further comprises a plurality of particulates.
  • Exemplary nonwoven webs according to the present disclosure may advantageously include a plurality of chemically active particulates.
  • the chemically active particulates can be any discrete particulate, which is a solid at room temperature, and which is capable of undergoing a chemical interaction with an external fluid phase. Exemplary chemical interactions include adsorption, absorption, chemical reaction, catalysis of a chemical reaction, dissolution, and the like.
  • the chemically active particulates may advantageously be selected from sorbent particulates (e.g. adsorbent particulates, absorbent particulates, and the like), desiccant particulates (e.g. particulates comprising a hygroscopic substance such as, for example, calcium chloride, calcium sulfate, and the like, that induces or sustains a state of dryness in its local vicinity), biocide particulates, microcapsules, and combinations thereof.
  • sorbent particulates e.g. adsorbent particulates, absorbent particulates, and the like
  • desiccant particulates e.g. particulates comprising a hygroscopic substance such as, for example, calcium chloride, calcium sulfate, and the like, that induces or sustains a state of dryness in its local vicinity
  • biocide particulates e.g. adsorbent particulates, absorbent particulates, and the like
  • the chemically active particulates may be selected from activated carbon particulates, activated alumina particulates, silica gel particulates anion exchange resin particulates, cation exchange resin particulates, molecular sieve particulates, diatomaceous earth particulates, anti-microbial compound particulates, metal particulates, and combinations thereof.
  • the chemically active particulates are sorbent particulates.
  • sorbent particulates include mineral particulates, synthetic particulates, natural sorbent particulates or a combination thereof. Desirably the sorbent particulates will be capable of absorbing or adsorbing gases, aerosols, or liquids expected to be present under the intended use conditions.
  • the sorbent particulates can be in any usable form including beads, flakes, granules or agglomerates.
  • Preferred sorbent particulates include activated carbon; silica gel; activated alumina and other metal oxides; metal particulates (e.g., silver particulates) that can remove a component from a fluid by adsorption or chemical reaction; particulate catalytic agents such as hopcalite (which can catalyze the oxidation of carbon monoxide); clay and other minerals treated with acidic solutions such as acetic acid or alkaline solutions such as aqueous sodium hydroxide; ion exchange resins; molecular sieves and other zeolites; biocides; fungicides and virucides.
  • Activated carbon and activated alumina are presently particularly preferred sorbent particulates.
  • Mixtures of sorbent particulates can also be employed, e.g., to absorb mixtures of gases, although in practice to deal with mixtures of gases it may be better to fabricate a multilayer sheet article employing separate sorbent particulates in the individual layers.
  • the chemically active sorbent particulates are selected to be gas adsorbent or absorbent particulates.
  • gas adsorbent particulates may include activated carbon, charcoal, zeolites, molecular sieves, an acid gas adsorbent, an arsenic reduction material, an iodinated resin, and the like.
  • absorbent particulates may also include naturally porous particulate materials such as diatomaceous earth, clays, or synthetic particulate foams such as melamine, rubber, urethane, polyester, polyethylene, silicones, and cellulose.
  • the absorbent particulates may also include superabsorbent particulates such as sodium polyacrylates, carboxymethyl cellulose, or granular polyvinyl alcohol.
  • the sorbent particulates comprise liquid an activated carbon, diatomaceous earth, an ion exchange resin (e.g. an anion exchange resin, a cation exchange resin, or combinations thereof), a molecular sieve, a metal ion exchange sorbent, an activated alumina, an antimicrobial compound, or combinations thereof.
  • an ion exchange resin e.g. an anion exchange resin, a cation exchange resin, or combinations thereof
  • a molecular sieve e.g. an anion exchange resin, a cation exchange resin, or combinations thereof
  • a metal ion exchange sorbent e.g. an anion exchange resin, a cation exchange resin, or combinations thereof
  • the web has a sorbent particulate density in the range of about 0.20 to about 0.5 g/cc.
  • sorbent chemically active particulates may be used to create a nonwoven web.
  • the sorbent particulates have a mean size greater than 1 mm in diameter.
  • the sorbent particulates have a mean size less than 1 cm in diameter.
  • a combination of particulate sizes can be used.
  • the sorbent particulates include a mixture of large particulates and small particulates.
  • the desired sorbent particulate size can vary a great deal and usually will be chosen based in part on the intended service conditions.
  • sorbent particulates particularly useful for fluid filtration applications may vary in size from about 0.001 to about 3000 ⁇ m mean diameter.
  • the sorbent particulates are from about 0.01 to about 1500 ⁇ m mean diameter, more generally from about 0.02 to about 750 ⁇ m mean diameter, and most generally from about 0.05 to about 300 ⁇ m mean diameter.
  • the sorbent particulates may comprise nano-particulates having a population mean diameter less than 1 ⁇ m.
  • Porous nano-particulates may have the advantage of providing high surface area for sorption of contaminants from a fluid medium (e.g., absorption and/or adsorption).
  • the particulates are adhesively bonded to the filaments using an adhesive, for example a hot melt adhesive, and/or the application of heat to the melt-spun nonwoven web (i.e., thermal bonding).
  • sorbent particulates having different size ranges can also be employed, although in practice it may be better to fabricate a multilayer sheet article employing larger sorbent particulates in an upstream layer and smaller sorbent particulates in a downstream layer.
  • At least 80 weight percent sorbent particulates, more generally at least 84 weight percent and most generally at least 90 weight percent sorbent particulates are enmeshed in the web.
  • the sorbent particulate loading level may for example be at least about 500 gsm for relatively fine (e.g. sub-micrometer-sized) sorbent particulates, and at least about 2,000 gsm for relatively coarse (e.g., micron-sized) sorbent particulates.
  • the chemically active particulates are metal particulates.
  • the metal particulates may be used to create a polishing nonwoven web.
  • the metal particulates may be in the form of short filament or ribbon-like sections or may be in the form of grain-like particulates.
  • the metal particulates can include any type of metal such as but not limited to silver (which has antibacterial/antimicrobial properties), copper (which has properties of an algaecide), or blends of one or more of chemically active metals.
  • the chemically active particulates are solid biocides or antimicrobial agents.
  • solid biocide and antimicrobial agents include halogen containing compounds such as sodium dichloroisocyanurate dihydrate, benzalkonium chloride, halogenated dialkylhydantoins, and triclosan.
  • the chemically active particulates are microcapsules.
  • Microcapsules are described in U.S. Pat. No. 3,516,941 (Matson), and include examples of the microcapsules that can be used as the chemically active particulates.
  • the microcapsules may be loaded with solid or liquid biocides or antimicrobial agents.
  • One of the main qualities of a microcapsule is that by means of mechanical stress the particulates can be broken in order to release the material contained within them. Therefore, during use of the nonwoven web, the microcapsules will be broken due to the pressure exerted on the nonwoven web, which will release the material contained within the microcapsule.
  • useful particulates may comprise a (co)polymer, for example, a thermoplastic (co)polymer, which may be in the form of semi-continuous filaments.
  • Suitable polymers include polyolefins, particularly thermoplastic elastomers (TPE's) (e.g., VISTAMAXXTM, available from Exxon-Mobil Chemical Company, Houston, Tex.).
  • particulates comprising a TPE may be preferred, as TPE's are generally somewhat tacky, which may assist bonding together of the particulates to form a three-dimensional network before addition of the filaments to form the nonwoven web.
  • particulates comprising a VISTAMAXXTM TPE may offer improved resistance to harsh chemical environments, particularly at low pH (e.g., pH no greater than about 3) and high pH (e.g., pH of at least about 9) and in organic solvents.
  • Suitable particulates may have a variety of physical forms (e.g., solid particulates, porous particulates, hollow bubbles, agglomerates, semi-continuous filaments, staple filaments, flakes, and the like); shapes (e.g., spherical, elliptical, polygonal, needle-like, and the like); shape uniformities (e.g., monodisperse, substantially uniform, non-uniform or irregular, and the like); composition (e.g. inorganic particulates, organic particulates, or combination thereof); and size (e.g., sub-micrometer-sized, micro-sized, and the like).
  • physical forms e.g., solid particulates, porous particulates, hollow bubbles, agglomerates, semi-continuous filaments, staple filaments, flakes, and the like
  • shapes e.g., spherical, elliptical, polygonal, needle-like, and the like
  • shape uniformities e.g.,
  • particulate size in some exemplary embodiments, it may be desirable to control the size of a population of the particulates.
  • particulates are physically entrained or trapped in the filament nonwoven web.
  • the population of particulates is generally selected to have a mean diameter of at least 50 ⁇ m, more generally at least 75 ⁇ m, still more generally at least 100 ⁇ m.
  • the particulates may be preferred to use finer particulates that are adhesively bonded to the filaments using an adhesive, for example a hot melt adhesive, and/or the application of heat to one or both of thermoplastic particulates or thermoplastic filaments (i.e., thermal bonding).
  • an adhesive for example a hot melt adhesive
  • the particulates have a mean diameter of at least 25 ⁇ m, more generally at least 30 ⁇ m, most generally at least 40 ⁇ m.
  • the chemically active particulates have a mean size less than 1 cm in diameter. In other embodiments, the chemically active particulates have a mean size of less than 1 mm, more generally less than 25 micrometers, even more generally less than 10 micrometers.
  • the particulates may comprise a population of sub-micrometer-sized particulates having a population mean diameter of less than one micrometer ( ⁇ m), more generally less than about 0.9 ⁇ m, even more generally less than about 0.5 ⁇ m, most generally less than about 0.25 ⁇ m.
  • ⁇ m micrometer
  • Such sub-micrometer-sized particulates may be particularly useful in applications where high surface area and/or high absorbency and/or adsorbent capacity is desired.
  • the population of sub-micrometer-sized particulates has a population mean diameter of at least 0.001 ⁇ m, more generally at least about 0.01 ⁇ m, most generally at least about 0.1 ⁇ m, most generally at least about 0.2 ⁇ m.
  • the particulates comprise a population of micro-sized particulates having a population mean diameter of at most about 2,000 ⁇ m, more generally at most about 1,000 ⁇ m, most generally at most about 500 ⁇ m. In other exemplary embodiments, the particulates comprise a population of micro-sized particulates having a population mean diameter of at most about 10 ⁇ m, more generally at most about 5 ⁇ m, even more generally at most about 2 ⁇ m (e.g., ultrafine micro-filaments).
  • particulates may also be used within a single finished web. Using multiple types of particulates, it may be possible to generate continuous particulate webs even if one of the particulate types does not bond with other particulates of the same type.
  • An example of this type of system would be one where two types are particulates are used, one that bonds the particulates together (e.g., a semi-continuous polymeric filament particulate) and another that acts as an active particulate for the desired purpose of the web (e.g., a sorbent particulate such as activated carbon).
  • a sorbent particulate such as activated carbon
  • the chemically active particulates may be used relative to the total weight of the fibrous web.
  • the chemically active particulates comprise less than 90% wt. of the total nonwoven article weight. In one embodiment, the chemically active particulates comprise at least 10% wt. of the total nonwoven article weight.
  • the chemically active particulates may be advantageously distributed throughout the entire thickness of the nonwoven web. However, in some of the foregoing embodiments, the chemically active particulates are preferentially distributed substantially on a major surface of the nonwoven web.
  • the present disclosure describes a process for making a nonwoven web, comprising heating a mixture of about 50% w/w to about 99% w/w of a crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w of a hydrocarbon tackifier resin to at least a Melting Temperature of the mixture to form a molten mixture, extruding the molten mixture through at least one orifice to form at least one semi-continuous filament, attenuating the at least one semi-continuous filament to draw and molecularly orient the at least one semi-continuous filament, and cooling the at least one semi-continuous filament to a temperature below the Melting Temperature of the molten mixture to form a melt-spun nonwoven web, wherein the at least one semi-continuous (co)polymeric filament exhibits molecular orientation, and further wherein at least one of the crystalline polyolefin (co)polymer or the nonwoven web exhibits
  • the at least one semi-continuous filament comprises a plurality of semi-continuous filaments
  • the process further includes collecting the plurality of semi-continuous filaments as the nonwoven web on a collector.
  • the plurality of semi-continuous filaments is comprised of melt-spun filaments.
  • the crystalline polyolefin (co)polymer/hydrocarbon resin tackifier mixture is melted to form a molten mixture, which is then extruded through one or more orifices of a melt-spinning die.
  • melt-spun filaments are subjected to a filament bonding step before, during, or after collection, thereby producing a spun-bond nonwoven web.
  • bonding comprises one or more of autogenous thermal bonding, non-autogenous thermal bonding, through air bonding, and ultrasonic bonding.
  • the process further includes at least one of addition of a plurality of staple filaments to the plurality of semi-continuous filaments, or addition of a plurality of particulates to the plurality of semi-continuous filaments.
  • the process further includes processing the collected nonwoven web using a process selected from bonding, electret charging, embossing, needle-punching, needle tacking, hydroentangling, or a combination thereof.
  • the melt-spinning should be performed within a range of temperatures hot enough to enable the crystalline polyolefin (co)polymer/hydrocarbon resin tackifier mixture to be melt-spun but not so hot as to cause unacceptable deterioration of the crystalline polyolefin (co)polymer/hydrocarbon resin tackifier mixture.
  • the melt-spinning can be performed at a temperature that causes the molten mixture of the crystalline polyolefin (co)polymer and hydrocarbon resin tackifier to reach a processing temperature at least 40-50° C. above the melting temperature.
  • the processing temperature of the molten mixture is selected to be 200° C., 225° C., 250° C., 260° C., 270° C., 280° C., or even at least 290° C.; to less than or equal to about 360° C., 350° C., 340° C., 330° C., 320° C., 310° C., or even 300° C.
  • the process further includes at least one of addition of a plurality of staple filaments to the plurality of discrete, semi-continuous filaments, or addition of a plurality of particulates to the plurality of discrete, semi-continuous filaments, to form a composite nonwoven web.
  • the method of making a composite nonwoven web comprises combining the microfilament or coarse microfilament population with the fine microfilament population, the ultrafine microfilament population, or the sub-micrometer filament population by mixing filament streams, hydroentangling, wet forming, plexifilament formation, or a combination thereof.
  • nonwoven composite fibrous webs may be formed exhibiting various desired concentration gradients and/or layered structures.
  • the population of fine, ultrafine or sub-micrometer filaments may be combined with the population of microfilaments or coarse microfilaments to form an inhomogenous mixture of filaments.
  • at least a portion of the population of fine, ultrafine or sub-micrometer filaments is intermixed with at least a portion of the population of microfilaments.
  • the population of fine, ultrafine or sub-micrometer filaments may be formed as an overlayer on an underlayer comprising the population of microfilaments.
  • the population of microfilaments may be formed as an overlayer on an underlayer comprising the population of fine, ultrafine or sub-micrometer filaments.
  • substantially uniform distribution of particles throughout the web is desired.
  • non-uniform distributions may be advantageous.
  • a particulate density gradient may advantageously be created within the composite nonwoven web. For example, gradients through the depth of the web may create changes to the pore size distribution that could be used for depth filtration. Webs with a surface loading of particles could be formed into a filter where the fluid is exposed to the particles early in the flow path and the balance of the web provides a support structure and means to prevent sloughing of the particles. The flow path could also be reversed so the web can act as a pre-filter to remove some contaminants prior to the fluid reaching the active surface of the particles.
  • the optional particulates could be added to a nonwoven filament stream by air laying a filament web, adding particulates to the filament web (e.g., by passing the web through a fluidized bed of particulates), optionally with post heating of the particulate-loaded web to bond the particulates to the filaments.
  • a pre-formed web could be sprayed with a pre-formed dispersion of particulates in a volatile fluid (e.g. an organic solvent, or even water), optionally with post heating of the particulate-loaded web to remove the volatile fluid and bond the particulates to the filaments.
  • a volatile fluid e.g. an organic solvent, or even water
  • the process further includes collecting the plurality of discrete, semi-continuous filaments as the nonwoven web on a collector.
  • the composite nonwoven web may be formed by depositing the population of fine, ultrafine or sub-micrometer filaments directly onto a collector surface, or onto an optional support layer on the collector surface, the support layer optionally comprising microfilaments, so as to form a population of fine, ultrafine or sub-micrometer filaments on the porous support layer.
  • the process may include a step wherein the optional support layer, which optionally may comprise polymeric microfilaments, is passed through a filament stream of fine, ultrafine or sub-micrometer filaments. While passing through the filament stream, fine, ultrafine or sub-micrometer filaments may be deposited onto the support layer so as to be temporarily or permanently bonded to the support layer. When the filaments are deposited onto the support layer, the filaments may optionally bond to one another, and may further harden while on the support layer.
  • the fine, ultrafine or sub-micrometer filament population is combined with an optional porous support layer that comprises at least a portion of the coarse microfilament population.
  • the microfilaments forming the porous support layer are compositionally the same as the population of microfilaments that forms the first layer.
  • the fine, ultrafine or sub-micrometer filament population is combined with an optional porous support layer and subsequently combined with at least a portion of the coarse microfilament population.
  • the porous support layer adjoins the second layer opposite the first layer.
  • the porous support layer comprises a nonwoven fabric, a woven fabric, a knitted fabric, a foam layer, a screen, a porous film, a perforated film, an array of filaments, or a combination thereof.
  • the porous support layer comprises a thermoplastic mesh.
  • the process further includes processing the collected nonwoven web using a process selected from bonding (e.g., autogenous bonding, through-air bonding, calendering, and the like), electret charging, embossing, needle-punching, needle tacking, hydroentangling, or a combination thereof.
  • bonding e.g., autogenous bonding, through-air bonding, calendering, and the like
  • electret charging e.g., embossing, needle-punching, needle tacking, hydroentangling, or a combination thereof.
  • some bonding may occur between the filaments themselves (e.g., autogenous bonding) and between the filaments and any optional particulates, before or during collection. “Bonding the filaments together” means adhering the filaments together firmly without an additional adhesive material, so that the filaments generally do not separate when the web is subjected to normal handling).
  • Bonding may be achieved, for example, using thermal bonding, adhesive bonding, powdered binder, hydroentangling, needle-punching, calendering, or a combination thereof.
  • Conventional bonding techniques using heat and pressure applied in a point-bonding process or by smooth calender rolls can be used, though such processes may cause undesired deformation of filaments or excessive compaction of the web.
  • a presently-preferred technique for bonding the filaments is through-air bonding as disclosed in U.S. Pat. Pub. No. 2008/0038976 (Berrigan et al.).
  • any bonding technique may be used to achieve supplemental bonding, for example, application of one or more adhesives to one or more surfaces to be bonded, ultrasonic welding, or other thermal bonding methods able to form localized bond patterns, as known to those skilled in the art.
  • supplemental bonding may make the web more easily handled and better able to hold its shape.
  • the melt-spun filaments may be advantageously electrostatically charged.
  • the melt-spun filaments may be subjected to an electret charging process.
  • An exemplary electret charging process is hydro-charging. Hydro-charging of filaments may be carried out using a variety of techniques including impinging, soaking or condensing a polar fluid onto the filament, followed by drying, so that the filament becomes charged. Representative patents describing hydro-charging include U.S. Pat. Nos. 5,496,507; 5,908,598; 6,375,886 B1; 6,406,657 B1; 6,454,986 and 6,743,464 B1.
  • water is employed as the polar hydro-charging liquid, and the media preferably is exposed to the polar hydro-charging liquid using jets of the liquid or a stream of liquid droplets provided by any suitable spray means.
  • Devices useful for hydraulically entangling filaments are generally useful for carrying out hydro-charging, although the operation is carried out at lower pressures in hydro-charging than generally used in hydro-entangling.
  • U.S. Pat. No. 5,496,507 describes an exemplary apparatus in which jets of water or a stream of water droplets are impinged upon the filaments in web form at a pressure sufficient to provide the subsequently-dried media with a filtration-enhancing electret charge.
  • the pressure necessary to achieve optimum results may vary depending on the type of sprayer used, the type of (co)polymer from which the filament is formed, the thickness and density of the web, and whether pretreatment such as corona charging was carried out before hydro-charging. Generally, pressures in the range of about 69 kPa to about 3450 kPa are suitable.
  • the water used to provide the water droplets is relatively pure. Distilled or deionized water is preferable to tap water.
  • the electret filaments may be subjected to other charging techniques in addition to or alternatively to hydro-charging, including electrostatic charging (e.g., as described in U.S. Pat. Nos. 4,215,682, 5,401,446 and 6,119,691), tribo-charging (e.g., as described in U.S. Pat. No. 4,798,850) or plasma fluorination (e.g., as described in U.S. Pat. No. 6,397,458 B1).
  • electrostatic charging e.g., as described in U.S. Pat. Nos. 4,215,682, 5,401,446 and 6,119,691
  • tribo-charging e.g., as described in U.S. Pat. No. 4,798,850
  • plasma fluorination e.g., as described in U.S. Pat. No. 6,397,458 B1
  • Corona charging followed by hydro-charging and plasma fluorination followed by hydro-charging are particularly suitable
  • Various processes conventionally used as adjuncts to filament-forming processes may be used in connection with filaments as they exit from one or more orifices of the belt blowing die. Such processes include spraying of finishes, adhesives or other materials onto the filaments, application of an electrostatic charge to the filaments, application of water mists to the filaments, and the like.
  • various materials may be added to a collected web, including bonding agents, adhesives, finishes, and other webs or films.
  • extruded filaments or filaments may be subjected to a number of additional processing steps, e.g., further drawing, spraying, and the like.
  • Various fluids may also be advantageously applied to the filaments before or during collection, including water sprayed onto the filaments, e.g., heated water or steam to heat the filaments, or cold water to quench the filaments.
  • the collected mass may additionally or alternatively be wound into a storage roll for later processing if desired.
  • the collected melt-spun nonwoven web may be conveyed to other apparatus such as calenders, embossing stations, laminators, cutters and the like; or it may be passed through drive rolls and wound into a storage roll.
  • one or more of the following process steps may optionally be carried out on the web once formed:
  • a surface treatment or other composition e.g., a fire-retardant composition, an adhesive composition, or a print layer
  • Nonwoven fibrous webs can be made using the foregoing processes.
  • the nonwoven web or composite web takes the form of a mat, web, sheet, a scrim, or a combination thereof.
  • the nonwoven web or composite web may advantageously include charged melt-spun filaments, e.g., electret filaments.
  • the melt-spun nonwoven web or web is porous.
  • the nonwoven web or composite web may advantageously be self-supporting.
  • the melt-spun nonwoven web or composite nonwoven web advantageously may be pleated, e.g., to form a filtration medium, such as a liquid (e.g., water) or gas (e.g., air) filter, a heating, ventilation or air conditioning (HVAC) filter, or a respirator for personal protection.
  • a filtration medium such as a liquid (e.g., water) or gas (e.g., air) filter, a heating, ventilation or air conditioning (HVAC) filter, or a respirator for personal protection.
  • HVAC heating, ventilation or air conditioning
  • Webs of the present disclosure may be used by themselves, e.g., for filtration media, decorative fabric, or a protective or cover stock. Or they may be used in combination with other webs or structures, e.g., as a support for other fibrous layers deposited or laminated onto the web, as in a multilayer filtration media, or a substrate onto which a membrane may be cast. They may be processed after preparation as by passing them through smooth calendering rolls to form a smooth-surfaced web, or through shaping apparatus to form them into three-dimensional shapes.
  • a nonwoven web or composite web of the present disclosure can further comprise at least one or a plurality of other types of filaments (not shown) such as, for example, staple or otherwise semi-continuous filaments, melt spun continuous filaments or a combination thereof.
  • the present exemplary fibrous webs can be formed, for example, into a non-woven web that can be wound about a tube or other core to form a roll, and either stored for subsequent processing or transferred directly to a further processing step. The web may also be cut into individual sheets or mats directly after the web is manufactured or sometime thereafter.
  • the melt-spun nonwoven webs or composite webs can be used to make any suitable article such as, for example, a thermal insulation article, an acoustic insulation article, a fluid filtration article, a wipe, a surgical drape, a wound dressing, a garment, a respirator, or a combination thereof.
  • the thermal or acoustic insulation articles may be used as an insulation component for vehicles (e.g., trains, airplanes, automobiles and boats).
  • Other articles such as, for example, bedding, shelters, tents, insulation, insulating articles, liquid and gas filters, wipes, garments, garment components, personal protective equipment, respirators, and the like, can also be made using melt-spun nonwoven webs of the present disclosure.
  • Nonwoven webs may be preferred for certain applications, for examples as furnace filters or gas filtration respirators.
  • Such nonwoven webs typically have a density greater than 75 kg/m 3 and typically greater than 100 kg/m 3 or even 120 kg/m 3 .
  • open, lofty nonwoven webs suitable for use in certain fluid filtration applications generally have a maximum density of 60 kg/m 3 .
  • the nonwoven webs exhibit a Basis Weight of from 1 gsm to 400 gsm, more preferably from 1 gsm to 200 gsm, even more preferably from 1 gsm to 100 gsm, or even 1 gsm to about 50 gsm.
  • Certain presently-preferred nonwoven webs according to the present disclosure may have a Solidity less than 50%, 340%, 30%, 20%, or more preferably less than 15%, even more preferably less than 10%.
  • Mono-component polypropylene and blends of Polypropylene and OPPERATM resins were used to prepare semi-continuous filaments comprising from about 50% w/w to about 99% w/w of at least one crystalline polyolefin (co)polymer, and from about 1% w/w to about 40% w/w of at least one hydrocarbon tackifier resin, as well as nonwoven webs including such semi-continuous filaments.
  • the crystalline polyolefin (co)polymer was selected as Total 3860 polypropylene (available from Total Petrochemicals and Refining U.S.A., Houston, Tex.).
  • the hydrocarbon tackifier resin was selected as OPPERATM PR100A (available from Exxon-Mobil Chemical Co., Spring, Tex.)
  • Solvents and other reagents used may be obtained from Sigma-Aldrich Chemical Company (Milwaukee, Wis.).
  • the Actual Filament Diameter was determined using an optical microscope equipped with a calibrated reticle.
  • the AFD is the average (mean) number diameter determined from measurements taken on 20 individual filaments observed in the nonwoven web sample when positioned under the microscope objective at a focal point of the objective lens.
  • the Effective Filament Diameter was determined using an air flow rate of 32 L/min (corresponding to a face velocity of 5.3 cm/sec), using the method set forth in Davies, C. N., “The Separation of Airborne Dust and Particles,” Institution of Mechanical Engineers, London, Proceedings IB, 1952.
  • DSC Differential Scanning Calorimetry
  • the DSC analysis was carried out using a Model DSC Q2000 available from Ta Instruments Co. (New Castle, Del.). Approximately 1.5 mg to 10 mg of the crystalline polyolefin, the mixture of the crystalline polyolefin with the hydrocarbon tackifier resin, or the nonwoven web produced from the mixture, was loaded and sealed in an aluminum pan and placed in the DSC Q2000 apparatus.
  • Heating-Cooling-Heating cycle Each sample was initially heated from ⁇ 20° C. to 250° C. (or at least 30° C. above the Melting Temperature of the sample) at a rate of 10° C./minute. Each sample was then held for 1 minute at 250° C., and then subsequently cooled down to ⁇ 20° C. (or at least 50° C. below the crystallization temperature of the sample) at a rate of 20° C./min. Each sample was then held for 1 minute at ⁇ 20° C. and then subsequently heated from ⁇ 20° C. to 200° C. at 10° C./min.
  • the temperature corresponding to the highest-temperature endothermic peak was reported as the Melting Temperature (° C.), and the area under the same highest-temperature endothermic peak was reported as the Heat of Fusion.
  • the tensile properties of webs in the Examples were measured by pulling to failure a 1 inch by 6-inch sample (2.5 cm by 15.2 cm). The thickness of the nonwoven web samples was about 0.15 cm.
  • the Tensile Strength Test was carried out using a commercially available tensile test apparatus designated as Instron Model 5544 (available from Instron Company, Canton, Mass.). The gauge length was 4 inches (10.2 cm), and the cross-head speed was 308 millimeters/per minute. The Maximum Tensile Load (in Newtons) was determined in the machine direction of the nonwoven web.
  • Stiffness of the nonwoven webs in the machine direction was measured with a Gurley Bending Resistance Tester Model 4171E (available from Gurley Precision Instruments, Inc., Troy, N.Y.). Five 1.5 inch (about 3.9 cm) ⁇ 2 inch (about 5.1 cm) coupons were cut from the center lane of each nonwoven web with the 1.5 inch (about 3.9 cm) length corresponding to the machine direction of the web. Each coupon was then clamped in the Gurley Bending Resistance Tester, and the Tester motor was operated in each of two directions such that the Tester pendulum swung across the coupon until full deflection of the pendulum was achieved.
  • Pendulum weights and positions were selected such that deflection of the pendulum was kept between 1 inch (2.54 cm) and 6 inches (about 15.2 cm) for any given sample.
  • Results of nonwoven web Stiffness are reported for each nonwoven web as the average of the force (in mg) measured for each coupon from both directions.
  • melt-spun (spun-bond) nonwoven webs prepared according to the processes described in the present disclosure.
  • melt-spun (spun-bond) filaments and nonwoven webs including such filaments were prepared using an apparatus as depicted in FIG. 1 of U.S. Pat. Nos. 6,607,624 (Berrigan et al.), and using the process as described generally by Berrigan et al.
  • reference numeral 12 instead of two single-screw extruders (reference numeral 12 as shown in FIG.
  • Mono-component semi-continuous filaments and melt-spun (spun-bond) nonwoven webs including such filaments were prepared using Total 3860 polypropylene.
  • the semi-continuous filaments were formed from a multi-orifice die that was 18′′ (about 45.7 cm) wide and had approximately 1800 orifices.
  • the semi-continuous filaments were extruded at 0.04 grams/orifice/minute (ghm) at a temperature of 245° C.
  • the air attenuator was kept at 3 psig (about 20,684 Pa), which led to the calculated filament spinning speed of 837 m/min.
  • the melt-spun (spun-bond) nonwoven web was made at a target basis weight of ⁇ 120 gsm.
  • the melt-spun (spun-bond) web was made using the conditions which described in Comparative Example C-1, except the air pressure of the attenuator was increased to 7 psig (about 48,263 Pa). This was the point where considerable filament breakage was observed.
  • the filament size of the melt-spun (spun-bond) media obtained was 6.2 ⁇ m at a calculated filament spinning speed of 1464 m/min.
  • the melt-spun (spun-bond) media was made as described in Comparative Example C-2 except the 25 mm Berstorff twin-screw extruder was used with two loss in weight feeders to control the feeding of the Total PP 3860 and OPPERA PR100A resins to the extruder barrel and a melt pump to control the polymer melt flow to a die.
  • the web was made using the blend ratio of (90/10) in between PP 3860 and OPPERATM PR 100A.
  • the extruder temperature was at about 245° C. and it delivered the blend melt stream to the melt-spun (spun-bond) die maintained at 245° C.
  • the gear pump was adjusted so that a 0.04 grams/orifice/minute (ghm) polymer throughput rate was maintained at the melt-spun (spun-bond) die.
  • the resulting web was collected at the collector and had a basis weight of approximately 121 g/m 2 .
  • the air attenuator was kept at 3 psig (about 20,684 Pa) which led to a filament size of 8.3 microns at a calculated filament spinning speed of 817 m/min.
  • melt-spun (spun-bond) web was made using the conditions which described in Example 1, except the air pressure of the attenuator was increased to 18 psig (124,106 Pa). At this point no significant filament breakage occurred.
  • the filament size of the melt-spun (spun-bond) media obtained was 4.6 ⁇ m at a calculated filament spinning speed of 2660 m/min.
  • melt-spun (spun-bond) web was made using the conditions which described in Example 1, except the ratio of PP 3860 and OPPERATM PR 100A was increased to 80/20 w/w.
  • the filament size of the melt-spun (spun-bond) media obtained was 7.3 ⁇ m at a calculated filament spinning speed of 1056 m/min.
  • melt-spun (spun-bond) web was made using the conditions which described in Example 5, except the air pressure of the attenuator was increased to 16 psig (110,316 Pa).
  • the filament size of the melt-spun (spun-bond) media obtained was 5.2 ⁇ m at a calculated filament spinning speed of 2081 m/min.
  • melt-spun (spun-bond) web was made using the conditions which described in Example 6, except the flow rate of the blend was increased from 0.04 to 0.11 grams/orifice/minute and the air pressure of the attenuator was increased to 18 psig (124,106 Pa).
  • the filament size of the melt-spun (spun-bond) media obtained was 7.5 ⁇ m at a calculated filament spinning speed of 2751 m/min.
  • melt-spun (spun-bond) web was made using the conditions which described in Example 7, except the air pressure of the attenuator was increased to 40 psig (275,790 Pa).
  • the filament size of the melt-spun (spun-bond) media obtained was 6.1 ⁇ m at a calculated filament spinning speed of 4159 m/min.
  • OPPERATM PR 100A allows the filaments to be stretched and oriented more, as is evident from the filament spinning speed increase and decrease in filament size for Example 2 relative to Comparative Example C-2.
  • This high orientation of the filament also leads to a considerable increase in the ratio of stiffness/thickness, which increases from 2.55 g/m to 8.36 g/m, as well as the tensile properties of the nonwoven web.
  • MD machine direction
  • the addition of OPPERATM PR 100A at 10 weight % helps to increase the throughput from 10 lbs/hr (about 4.55 kg/hr) to 25 lbs/hr (about 11.36 kg/hr), without a considerable change in the Actual Filament Diameter. Therefore, the OPPERATM additive can be used to increase the throughput of the melt-spinning process without significantly altering the desired Actual Filament Diameter.
  • Comparative Example C-1 and Examples 1 and 4 were all carried out at the same throughput and same attenuation pressure which leads to a similar filament spinning speed.
  • the stiffness of the webs increases with increasing OPPERATM PR 100A weight percentage.
  • the ratio of stiffness to thickness increases from 3.59 g/m (0% OPPERATM PR 100A) to 4.59 g/m (10% OPPERATM PR 100A) to 7.93 g/m (20% OPPERATM PR 100A).

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  • Manufacturing & Machinery (AREA)
  • Nonwoven Fabrics (AREA)
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