(19) United States
`(12) Patent Application Publication (10) Pub. No.: US 2006/0237130 A1
`Thompson
`(43) Pub. Date:
`Oct. 26, 2006
`
`US 20060237 130A1
`
`(54) ACOUSTIC WEB
`(75) Inventor: Delton R. Thompson, Woodbury, MN
`(US)
`Correspondence Address:
`3M INNOVATIVE PROPERTIES COMPANY
`PO BOX 33427
`ST. PAUL, MN 55133-3427 (US)
`(73) Assignee: 3M Innovative Properties Company
`
`(21) Appl. No.:
`
`11/423,985
`
`(22) Filed:
`
`Jun. 14, 2006
`Related U.S. Application Data
`
`(62) Division of application No. 10/335,752, filed on Jan.
`2, 2003.
`
`
`
`Publication Classification
`
`(51) Int. Cl.
`(2006.01)
`B32B 37/00
`(52) U.S. Cl. .......................................................... 156/273.3
`
`(57)
`
`ABSTRACT
`
`Pore plugging is reduced when laminating an airflow resis
`tive membrane to a thermoplastic hot melt adhesive, by
`treating the membrane to reduce its Surface energy. This
`enables fabrication of acoustical laminates incorporating
`Substantial amounts of recycled fibrous insulating mat
`manufacturing waste, and permits design of the laminate
`based primarily on one-quarter wavelength sound absorp
`tion considerations and control of the porosity and interfa
`cial adhesion of the airflow resistant membrane.
`
`MacNeil Exhibit 2163
`Yita v. MacNeil IP, IPR2020-01139, Page 1
`
`

`

`Patent Application Publication Oct. 26
`
`2006 Sheet 1 of 2
`
`US 2006/02371.30 A1
`
`
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`MacNeil Exhibit 2163
`Yita v. MacNeil IP, IPR2020-01139, Page 2
`
`

`

`Patent Application Publication Oct. 26, 2006 Sheet 2 of 2
`
`US 2006/02371.30 A1
`
`
`
`MacNeil Exhibit 2163
`Yita v. MacNeil IP, IPR2020-01139, Page 3
`
`

`

`US 2006/0237 130 A1
`
`Oct. 26, 2006
`
`ACOUSTC WEB
`
`CROSS-REFERENCE TO RELATED
`APPLICATION
`0001. This is a divisional of U.S. patent application Ser.
`No. 10/335,752, filed Jan. 2, 2003, the entire disclosure of
`which is incorporated herein by reference.
`
`FIELD
`0002 This invention relates to sound absorptive articles
`and methods for their preparation.
`
`BACKGROUND
`0003 Typical insulating mat substrates may employ air
`laid nonwoven polyester fibers bound with adhesive bicom
`ponent fibers, open- or closed-cell foam sheets, or resinated
`shoddy mats. If made in a porous structure and with a
`Suitable thickness, these Substrates can absorb sound and
`thereby reduce noise levels in nearby spaces. For example,
`porous insulating mat Substrates can be laminated to carpet
`ing, headliners, trunk liners, hood liners, interior panels, and
`other porous decorative or functional facings such as those
`employed in vehicles, in order to provide enhanced noise
`reduction compared to use of the facing by itself.
`0004 Typical vehicular carpet laminates have a fibrous
`face of nylon or other synthetic tufted into a high basis
`weight supporting layer made of nylon or other compatible
`synthetic. The Supporting layer backside is typically extru
`sion coated with a molten hot melt adhesive or calcium
`carbonate-loaded latex to fix the fiber tufts. Optionally, a hot
`melt adhesive may be applied as a thin primary backcoat
`followed by a heavy latex secondary backcoat. The resulting
`backed carpet can be applied over an insulating mat. To form
`a vehicular carpet laminate, the backed carpet and the
`insulating mat typically are preheated followed by compres
`sion molding. The backcoat adhesively bonds the carpet to
`the mat. The resulting laminate is Subsequently air quenched
`and water jet cut to yield the final vehicular part.
`0005 For applications involving noise reduction, latex
`carpet backings typically are omitted in favor of hot melt
`adhesive primary backings. Calcium carbonate-loaded lat
`tices typically are sufficiently thick and impermeable to
`prevent the passage of sound waves through the backing and
`into the insulating mat, thus limiting the available noise
`reduction. Hot melt adhesive backings typically may be
`continuous and impervious when applied, but become
`porous during lamination of the backing to the insulating
`mat due to capillary flow of the adhesive into the carpet or
`into the mat. Polyolefins such as low density polyethylene
`(“LDPE) are often used as the hot melt adhesive.
`0006 When an airflow resistive membrane is positioned
`between a carpet and an insulating mat, improved sound
`insulating performance can be obtained, see e.g., M.
`Schwartz and E. J. Gohmann, Jr., “Influence of Surface
`Coatings on Impedance and Absorption of Urethane Foams,
`J. Acoust. Soc. Am., 34 (4): 502-513 (April, 1962), M.
`Schwartz and W. L. Buehner, “Effects of Light Coatings on
`Impedance and Absorption of Open-Celled Foams, J.
`Acoust. Soc. Am., 35 (10): 1507-1510 (October, 1963), U.S.
`Pat. Nos. 5,459,291, 5,824,973, 6,145,617, 6,217,691,
`6,270,608 and 6,296,075, U.S. Published Patent Application
`
`No. US 2001/0036788 A1 and PCT Published Application
`Nos. WO99/44817 A1, WO 00/27671 A1, WO 01/64991A2
`and WO 02/20307 A1.
`
`SUMMARY OF THE INVENTION
`0007 Airflow resistive membranes can experience partial
`or even Substantially complete pore plugging when molded
`or laminated against a carpet or other decorative or func
`tional object backed with a hot melt adhesive. Pore plugging
`can be exacerbated when the hot melt adhesive has a lower
`Surface energy than the Surface energy of the membrane.
`Meltblown webs made of polyamide (e.g., Nylon 6) or
`polyester (e.g., polybutylene terephthalate) are especially
`useful airflow resistive membrane materials, but are suscep
`tible to plugging by molten polyolefin. The low surface
`energy molten polyolefin readily wets the higher Surface
`energy polyamide or polyester membrane material, can flow
`into pores or other interstices in the membrane, and may fill
`the pores and Saturate the membrane when cooled. This can
`undesirably reduce porosity and Sound absorption perfor
`mance, although it may also increase interfacial adhesion.
`0008. The above-mentioned PCT Published Application
`No. WO 00/2767 A1 describes a vehicle roof lining that
`includes a porous barrier layer said to be made of a material
`that prevents the migration of adhesive components. This
`Application states that the barrier layer's Surface areas can
`be treated to promote wettability of adhesives coming into
`contact with the surface, while the barrier layer's core could
`repel adhesives. Such a treatment presumably would involve
`increasing the Surface energy at the barrier's Surface to
`promote such wettability.
`0009. The present invention provides, in one aspect, a
`method for laminating an adhesive layer to a semipermeable
`airflow resistive membrane, comprising treating the airflow
`resistive membrane to reduce its Surface energy before
`laminating the adhesive layer to the membrane.
`0010. The invention also provides a method for making a
`Sound-modifying structure comprising:
`0011 a) providing a stack of layers comprising a
`decorative facing layer, a thermoplastic adhesive layer,
`a porous membrane that has been treated to render the
`membrane substantially impenetrable by molten poly
`ethylene, and a layer of fibrous material, and
`0012 b) laminating the stack of layers together under
`Sufficient heat and pressure to form a unitary porous
`Sound-modifying, structure.
`0013 The invention also provides a method for attenu
`ating Sound waves passing from a source area to a receiving
`area of a vehicle, comprising:
`0014) a) providing an acoustical laminate comprising a
`fibrous or open cell foam underlayment, a hot melt
`adhesive layer, a porous membrane that has been
`treated to render the membrane substantially impen
`etrable by molten polyethylene a hot melt adhesive
`layer, and a decorative layer, and
`0015 b) positioning the laminate between the source
`area and the receiving area such that a major face of the
`laminate intercepts and thereby attenuates Sound waves
`passing from the Source area to the receiving area.
`
`MacNeil Exhibit 2163
`Yita v. MacNeil IP, IPR2020-01139, Page 4
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`US 2006/0237 130 A1
`
`Oct. 26, 2006
`
`0016. The invention also provides a porous laminate
`comprising a discontinuous hot melt adhesive layer adhered
`to a semipermeable low Surface energy airflow resistive
`porous layer whose pores are substantially impenetrable by
`the adhesive.
`0017. The invention also provides a porous laminate
`comprising a thermoplastic adhesive layer adjacent to a
`semipermeable fluorochemically-treated airflow resistive
`membrane.
`0018. The invention further provides a sound-absorbing
`laminate having a porous Sound-absorbing spacing layer
`adjacent to a semipermeable airflow resistive membrane that
`is substantially impenetrable by molten polyethylene.
`0019. In a further embodiment, the invention provides a
`Sound-modifying structure comprising a sound-reflecting
`Surface spaced from a semipermeable Sound modifying
`laminate comprising a facing layer and a porous membrane
`that is substantially impenetrable by molten polyethylene.
`0020. In another embodiment, the invention provides a
`vehicular Sound-absorbing, structure comprising a decora
`tive layer backcoated with a discontinuous hot melt adhesive
`layer adhered to a fluorochemically-treated nonwoven air
`flow resistive membrane having an airflow resistance
`between 50 and 5000 mks Rayls.
`0021. In yet another embodiment, the invention provides
`a carpet comprising fibers tufted into a backing backcoated
`with a discontinuous hot melt adhesive layer adhered to a
`fluorochemically-treated nonwoven airflow resistive mem
`brane having an airflow resistance between 50 and 5000 mks
`Rayls.
`0022. In another embodiment, the invention provides an
`acoustical laminate comprising:
`0023 a) a fibrous or open cell foam underlayment,
`0024 b) a hot melt adhesive layer,
`0025 c) a fluorochemically-treated nonwoven airflow
`resistive membrane having an airflow resistance
`between 50 and 5000 mks Rayls,
`0026.
`d) a hot melt adhesive layer, and
`0027 e) a decorative layer.
`BRIEF DESCRIPTION OF THE DRAWING
`0028 FIG. 1 is a perspective view of a carpet bonded to
`an airflow resistive membrane and insulating mat, with the
`carpet and membrane being partly peeled away to better
`illustrate individual layers.
`0029 FIG. 2 is an enlarged top view of the airflow
`resistive membrane of FIG. 1.
`0030 FIG. 3 is a schematic side view of a carpet bonded
`to an airflow resistive membrane and insulating mat.
`0031
`FIG. 4 is a photograph comparing fluorochemi
`cally-treated and nonfluorochemically-treated membranes in
`automotive carpet laminates that have been pulled apart to
`expose the membrane-carpet interface.
`
`DETAILED DESCRIPTION
`0032. In the practice of the present invention, the word
`'semipermeable' refers to a membrane having an acoustical
`
`airflow resistance between about 50 and about 5000 mks
`Rayls when evaluated using ASTM C522. The phrase “low
`Surface energy” refers to a surface whose Surface energy is
`less than about 34 dynes/cm. The phrase “hot melt adhe
`sive refers to a thermoplastic material having a melting
`point and adhesive strength over a range of temperatures
`Suitable for use in assembling acoustic laminates for vehicu
`lar applications.
`0033 FIG. 1 is a perspective view of an acoustical
`laminate 10. Laminate 10 includes carpet 12 made from
`nylon fibers 14 tufted into nylon spunbond fabric 16 and
`backcoated with LDPE hot melt adhesive layer 18. Layer 18
`bonds carpet 12 to airflow resistive nylon meltblown fiber
`membrane 20. Membrane 20 is shown in an enlarged top
`view in FIG. 2, and includes a porous nonwoven portion 22
`interspersed with generally nonporous embossed regions 24.
`Embossed regions 24 can improve the tensile strength of
`membrane 24. Referring again to FIG. 1, membrane 20 is
`bonded by discontinuous LDPE hot melt adhesive layer 26
`to a nonwoven insulating mat 28 whose thickness provides
`a space S between carpet 12 and sound-reflecting surface 30.
`Mat 28 is bonded to surface 30 via a suitable adhesive layer
`29. Mat 28 preferably is compressible and lightweight but
`sufficiently resilient so that mat 28 will move back into place
`if a force is applied to and then removed from carpet 12. As
`shown in FIG. 1, carpet 12, membrane 20 and mat 28 have
`been partly peeled away from surface 30 to better illustrate
`the various layers in acoustical laminate 10.
`0034) A variety of airflow resistive membranes can be
`used in the invention. The membrane is semipermeable and
`thus as indicated above has an acoustical airflow resistance
`between about 50 and about 5000 mks Rayls. Preferred
`membranes have an acoustical airflow resistance of at least
`about 200 mks Rayls. Preferred membranes also have an
`acoustical airflow resistance less than about 3300 mks
`Rayls. More preferably, the membrane has an acoustical
`airflow resistance of at least about 600 mks Rayls. Most
`preferably, the membrane also has an acoustical airflow
`resistance less than about 1100 mks Rayls. The airflow
`resistive membrane is treated so that it has a low surface
`energy, viz., less than that of the hot melt adhesive, and
`preferably less than about 34 dynes/cm, more preferably
`less than about 30 dynes/cm, and most preferably less than
`about 28 dynes/cm. Preferably the airflow resistive mem
`brane has an elongation to break sufficient to enable the
`membrane to Survive deep cavity molding (e.g., at least
`about 20%), and a thermal resistance sufficient to withstand
`the rigors of high temperature molding processes (e.g., at
`least about 210° C.). Lightweight meltblown nonwoven
`membranes having basis weights less than 300 g/m are
`especially preferred, more preferably less than about 100
`g/m and most preferably less than about 70 g/m. Stiff or
`flexible membranes can be employed, with flexible mem
`branes being especially preferred for carpet applications. For
`example, the membrane can have a bending stiffness B as
`low as 0.005 Nm or less when measured according to ASTM
`D1388 using Option A. The selection and processing of
`suitable membrane materials will be familiar to those skilled
`in the art. Preferred membrane materials include polya
`mides, polyesters, polyolefins and the materials disclosed in
`U.S. Pat. Nos. 5,459,291, 5,824,973, 6,145,617 and 6,296,
`075, U.S. Published Patent Application No. US 2001/
`0036788 A1 and PCT Published Application No. WO
`
`MacNeil Exhibit 2163
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`US 2006/0237 130 A1
`
`Oct. 26, 2006
`
`99/44817 A1. Nylon 6 polyamide and polybutylene tereph
`thalate are especially preferred membrane materials.
`0035. The surface energy of the airflow resistive web can
`be reduced in a variety of ways, e.g., by topically applying
`a suitable fluorochemical (e.g., an organofluorocarbon or
`fluorosilicone) or organosilicone treatment using spraying,
`foaming, padding or any other convenient method; by melt
`addition of a suitable fluorochemical (e.g., those just listed)
`to the extrusion or meltblowing die when the membrane is
`formed; or via plasma fluorination treatment. Topical fluo
`rochemical treatments and fluorochemical melt additives are
`presently preferred. The fluorine add-on rate preferably is
`adjusted to provide the desired reduction in membrane
`Surface energy and pore clogging during lamination while
`minimizing overall use of fluorine. In general comparable
`fluorine add-on rates can the used for topical and melt
`addition since for melt addition the fluorochemical typically
`will migrate to the membrane's surface. The amount of
`fluorochemical add-on rate can be evaluated by measuring
`the Surface energy of the membrane or by analyzing the
`fluorine content at the membrane's surface before or pref
`erably after assembly of the acoustical laminate. The fluo
`rine content after assembly preferably is obtained after the
`layers of the assembled acoustical laminate have been
`manually pulled apart to expose the bond interfaces between
`individual layers. Preferred fluorochemical add-on rates are
`about 0.01 wt.% or more solids, and more preferably at
`about 0.3 to about 0.6 wt.% solids based on the membrane
`weight. Expressed on the basis of fluorine, the fluorochemi
`cal add-on rate preferably provides about 0.04 wt.% or more
`fluorine on the membrane, more preferably about 0.12 to
`about 0.24 wt.% fluorine. Melt application is especially
`preferred, as it may avoid capital costs for padding, drying
`or curing equipment and the associated processing steps that
`may be required for topical treatments.
`0.036
`Particularly preferred fluorochemicals for topical
`application include dispersions or Solutions of fluorinated
`urethane compounds comprising the reaction product of:
`0037 a) a fluorinated polyether having the formula:
`R-Q-T
`(I)
`0038
`wherein Rf represents a monovalent perfluori
`nated polyether group having a molecular weight of at
`least 750 g/mol, Q represents a chemical bond or a
`divalent or trivalent organic linking group, T represents
`a functional group capable of reacting with an isocy
`anate and k is 1 or 2;
`0039 b) an isocyanate component selected from a
`polyisocyanate compound that has at least 3 isocyanate
`groups or a mixture of polyisocyanate compounds
`wherein the average number of isocyanate groups per
`molecule is more than 2; and
`0040 c) optionally one or more co-reactants capable of
`reacting with an isocyanate group.
`0041) The perfluorinated polyether group R preferably
`has the formula:
`(II)
`R" O-R-(R)-
`wherein R'? represents a perfluorinated alkyl group, Rf
`represents a perfluorinated polyalkyleneoxy group consist
`ing of perfluorinated alkyleneoxy groups having 1, 2, 3 or 4
`carbon atoms or a mixture of Such perfluorinated alkyle
`
`neoxy groups, Rf represents a perfluorinated alkylene group
`and q is 0 or 1. The perfluorinated alkyl group R' fin formula
`(II) may be linear or branched and preferably has 1 to 10
`carbonatoms, more preferably 1 to 6 carbon atoms. A typical
`Such perfluorinated alkyl group is CF, CF, CF2 . The
`perfluoroalkyleneoxy group R, may be linear or branched.
`When the perfluoroalkyleneoxy group is composed of a
`mixture of different perfluoroalkyleneoxy units, the units
`can be present in a random configuration, an alternating
`configuration or as blocks. Typical perfluorinated polyalky
`leneoxy groups RF include —CF,
`CF O-,
`CF(CF)—CF O CF, CF (CF)—O—, —CF
`CF, CF O-,
`CF O-,
`CF(CF)-O-,
`CF, CF, CF, CF. O,
`CF, CF O-,
`—CF(CF)—CF. O), , —CFCF. Ol CFO) -
`and
`—CF, CF O-CF (CF)—CF. On ,
`wherein r is 4 to 25, n is 3 to 25 and i, l, m and jeach are
`2 to 25. The perfluorinated alkylene group R may be linear
`or branched and preferably has 1 to 6 carbon atoms. A
`typical Such perfluorinated alkylene group is —CF – or
`—CF (CF)—. Examples of linking groups Q in formula (I)
`include organic groups that comprise aromatic or aliphatic
`groups that may be interrupted by O., N or S, e.g., alkylene
`groups, oxy groups, thio groups, urethane groups, carboxy
`groups, carbonyl groups, amido groups, oxyalkylene groups,
`thioalkylene groups, carboxyalkylene and/or an amidoalky
`lene groups. Examples of functional groups T in formula (I)
`include thiol, hydroxy and amino groups.
`0042.
`In a preferred embodiment, the fluorinated poly
`ether of formula (I) has the formula:
`
`wherein R'r Q, Tand k are as defined above, n is an integer
`of 3 to 25 and A is a carbonyl group or CH. An especially
`preferred fluorinated polyether of formula (III) contains an
`R" group of the formula CF, CF, CF O-, and thus
`contains a moiety of the formula CF, CF, CF O
`CF (CF)—CFO. —CF(CF)— where n is an integer of
`3 to 25. This moiety has a molecular weight of 783 when in
`equals 3.
`0043 Representative examples of the moiety -A-Q-T in
`formula (III) include:
`0044) 1. CONR CHCHOHCH-OH wherein R
`is hydrogen or an alkyl group of for example 1 to 4
`carbon atoms;
`0045 2. – CONH-1,4-dihydroxyphenyl:
`0046) 3. CHOCHCHOHCH-OH:
`0047. 4. COOCHCHOHCH-OH; and
`0048, 5.–CONR (CH), OH where R is hydrogen
`or an alkyl group Such as methyl, ethyl, propyl, butyl,
`or hexyl and m is 2, 3, 4, 6, 8, 10 or 11.
`Especially preferred fluorinated polyethers of formula
`(III) contain-A-Q'-T moieties of the formula—CO—
`X Re(OH), wherein k is as defined above, R is an
`alkylene group of 1 to 15 carbon atoms and X is O or
`NR with R' representing hydrogen oran alkyl group of
`1 to 4 carbon atoms.
`0049 Preferred compounds according to formula (III)
`can be obtained by oligomerization of hexafluoropropylene
`oxide, yielding a perfluoropolyether carbonyl fluoride. This
`
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`Oct. 26, 2006
`
`carbonyl fluoride may be converted into an acid, ester or
`alcohol by reactions well known to those skilled in the art.
`The carbonyl fluoride or acid, ester or alcohol derived
`therefrom may then be reacted further to introduce the
`desired isocyanate reactive groups T according to known
`procedures. Compounds having the -A-Q-T moiety 1 listed
`above can be obtained by reacting the methyl ester deriva
`tive of a fluorinated polyether with 3-amino-2-hydroxy
`propanol. Compounds having the -A-Q-T moiety 5 listed
`above can be obtained in a similar way by using an amino
`alcohol that has only one hydroxy function. For example,
`reaction with 2-aminoethanol would yield a compound
`having the group 5 listed above with R being hydrogen and
`m being 2. European Patent Application No. EP 0 870 778
`also describes methods for producing compounds according
`to formula (III) having desired moieties -A-Q-T. Still
`further examples of compounds according to formula (I) or
`(III) are disclosed in U.S. Pat. No. 3,536,710.
`0050. The above-mentioned isocyanate component pref
`erably is a polyisocyanate having at least 3 isocyanate
`groups or a mixture of polyisocyanate compounds that on
`average has more than 2 isocyanate groups per molecule
`Such as for example a mixture of a diisocyanate compound
`and a polyisocyanate compound having 3 or more isocyan
`ate groups. The polyisocyanate compound may be aliphatic
`or aromatic and is conveniently a non-fluorinated com
`pound. Generally, the molecular weight of the polyisocyan
`ate compound will be not more than 1500 g/mol. Examples
`include hexamethylenediisocyanate; 2.2,4-trimethyl-1,6-
`hexamethylenediisocyanate;
`1.2-ethylenediisocyanate;
`dicyclohexylmethane-4,4'-diisocyanate; aliphatic triisocy
`anates Such as 1.3.6-hexamethylenetriisocyanate, cyclic tri
`mers of hexamethylenediisocyanate and cyclic trimers of
`isophorone diisocyanate (isocyanurates); aromatic polyiso
`cyanates Such as 4,4'-methylenediphenylenediisocyanate,
`4,6-di-(trifluoromethyl)-1,3-benzene diisocyanate, 2,4-tolu
`enediisocyanate, 2,6-toluene diisocyanate, o, m, and p-Xy
`lylene diisocyanate, 4,4'-diisocyanatodiphenylether, 3.3
`t-dichloro-4,4'-diisocyanatodiphenylmethane,
`4.5'-diphe
`nyldiisocyanate, 4,4'-diisocyanatodibenzyl, 3,3'-dimethoxy
`4,4'-diisocyanatodiphenyl, 3,3'-dimethyl-4,4'-diisocyanato
`diphenyl,
`2,2'-dichloro-5,5-dimethoxy-4,4'-diisocyanato
`diphenyl, 1,3-diisocyanatobenzene, 1.2-naphthylene diiso
`cyanate, 4-chloro-1,2-naphthylene diisocyanate, 1.3-naph
`thylene diisocyanate, and 1,8-dinitro-2.7-naphthylene diiso
`cyanate
`and
`aromatic
`triisocyanates
`Such
`as
`polymethylenepolyphenylisocyanate. Still further isocyan
`ates that can be used for preparing the fluorinated urethane
`compound include alicyclic diisocyanates Such as 3-isocy
`anatomethyl-3,5,5-trimethylcyclohexylisocyanate; aromatic
`tri-isocyanates Such as polymethylenepolyphenylisocyanate
`(PAPI) and cyclic diisocyanates such as isophorone diiso
`cyanate (IPDI). Also useful are isocyanates containing inter
`nal isocyanate-derived moieties such as biuret-containing
`tri-isocyanates such as DESMODURTM N-100 (commer
`cially available from Bayer), isocyanurate-containing tri
`isocyanates such IPDI-1890 (commercially available from
`Huls AG), and azetedlinedione-containing diisocyanates
`such as DESMODURTMTT (commercially available from
`Bayer). Also, other di- or tri-isocyanates such as DESMO
`DURTML and DESMODURTMW (both commercially avail
`able from Bayer), tri-(4-isocyanatophenyl)-methane (com
`
`mercially available from Bayer as DESMODURTM R) and
`DDI 1410 (commercially available from Henkel) are suit
`able.
`0051. The above-mentioned optional coreactant includes
`Substances such as water or a non-fluorinated organic com
`pound having one or more Zerewitinoff hydrogen atoms.
`Examples include non-fluorinated organic compounds that
`have at least one or two functional groups that are capable
`of reacting with an isocyanate group. Such functional groups
`include hydroxy, amino and thiol groups. Examples of Such
`organic compounds include aliphatic monofunctional alco
`hols, e.g., mono-alkanols having at least 1, preferably at
`least 6 carbon atoms, aliphatic monofunctional amines, a
`polyoxyalkylenes having 2, 3 or 4 carbon atoms in the
`oxyalkylene groups and having 1 or 2 groups having at least
`one Zerewitinoff hydrogen atom, polyols including diols
`Such as polyether diols, e.g., polytetramethylene glycol,
`polyester diols, dimer diols, fatty acid ester diols, polysi
`loxane diols and alkane diols such as ethylene glycol and
`polyamines. Examples of monofunctional alcohols include
`methanol, ethanol, n-propyl alcohol, isopropyl alcohol,
`n-butyl alcohol, isobutyl alcohol, t-butyl alcohol, n-amyl
`alcohol, t-amyl alcohol, 2-ethylhexanol, glycidol and (iso)S-
`tearyl alcohol. Fatty ester diols are preferably diols that
`include an ester function derived from a fatty acid, prefer
`ably a fatty acid having at least 5 carbon atoms and more
`preferably at least 8 carbon atoms. Examples of fatty ester
`diols include glycerol mono-oleate, glycerol mono-stearate,
`glycerol mono-ricinoleate, glycerol mono-tallow, long chain
`alkyl di-esters of pentaerythritol having at least 5 carbon
`atoms in the alkyl group. Suitable fatty ester diols include
`RILANITTM diols such as RILANITTM GMS, RILANITTM
`GMRO and RILANITTM HE (all commercially available
`from Henkel).
`0052 Suitable polysiloxane diols include polydialkylsi
`loxane diols and polyalkylarylsiloxane diols. The polymer
`ization degree of the polysiloxane diol is preferably between
`10 and 50 and more preferably between 10 and 30. Polysi
`loxane diols particularly include those that correspond to
`one of the following formulas:
`
`Ho-R-i-o-o-i-R-OH
`
`R3
`
`R5
`
`R7
`
`R-i-o-o:
`
`(IV)
`
`(V)
`
`wherein R' and R independently represent an alkylene
`group having 1 to 4 carbonatoms, R. R. R. R. R. Rand
`R’ independently represent an alkyl group having 1 to 4
`carbon atoms or an aryl group, L' represents a trivalent
`linking group and m represents a value of 10 to 50. L is for
`example a linear or branched alkylene group that may
`contain one or more catenary hetero atoms Such as oxygen
`or nitrogen.
`0053. Further suitable diols include polyester diols.
`Examples include linear UNIFLEXTM polyesters (commer
`
`MacNeil Exhibit 2163
`Yita v. MacNeil IP, IPR2020-01139, Page 7
`
`

`

`US 2006/0237 130 A1
`
`Oct. 26, 2006
`
`cially available from Union Camp) and polyesters derived
`from dimer acids or dimer diols. Dimer acids and dimer
`diols are well-known and are obtained by dimerisation of
`unsaturated acids or diols in particular of unsaturated long
`chain aliphatic acids or diols (e.g. at least 5 carbon atoms).
`Examples of polyesters obtainable from dimer acids or
`dimer diols include PRIPLASTTMO and PRIPOLTM diols
`(both commercially available from Uniqema).
`0054 According to a particularly preferred embodiment,
`the organic compound will include one or more water
`solubilizing groups or groups capable of forming water
`solubilizing groups so as to obtain a fluorinated compound
`that can more easily be dispersed in water. Additionally, by
`including water Solubilizing groups in the fluorinated com
`pound, beneficial stain release properties may be obtained
`on the fibrous substrate. Suitable water solubilizing groups
`include cationic, anionic and Zwitterionic groups as well as
`non-ionic water solubilizing groups. Examples of ionic
`water solubilizing groups include ammonium groups, phos
`phonium groups, Sulfonium groups, carboxylates, Sul
`fonates, phosphates, phosphonates or phosphinates.
`Examples of groups capable of forming a water Solubilizing
`group in water include groups that have the potential of
`being protonated in water Such as amino groups, in particu
`lar tertiary amino groups. Particularly preferred organic
`compounds are those organic compounds that have only one
`or two functional groups capable of reacting with NCO
`group and that further include a non-ionic water-solubilizing
`group. Typical non-ionic water solubilizing groups include
`polyoxyalkylene groups. Preferred polyoxyalkylene groups
`include those having 1 to 4 carbon atoms such as polyoxy
`ethylene, polyoxypropylene, polyoxytetramethylene and
`copolymers thereof Such as polymers having both oxyeth
`ylene and oxypropylene units. The polyoxyalkylene con
`taining organic compound may include one or two func
`tional groups such as hydroxy or amino groups. Examples of
`polyoxyalkylene containing compounds include alkyl ethers
`of polyglycols such as e.g. methyl or ethyl ether of poly
`ethyleneglycol, hydroxy terminated methyl or ethyl ether of
`a random or block copolymer of ethyleneoxide and propy
`leneoxide, amino terminated methyl or ethyl ether of poly
`ethyleneoxide, polyethylene glycol, polypropylene glycol, a
`hydroxy terminated copolymer (including a block copoly
`mer) of ethyleneoxide and propylene oxide, diamino termi
`nated poly(alkylene oxides) such as JEFFAMINETMED and
`JEFFAMINETM EDR-148 (both commercially available
`from Huntsman Performance Chemicals) and poly(oxyalky
`lene) thiols.
`0.055 The optional co-reactant may also include an iso
`cyanate blocking agent. The isocyanate blocking agent can
`be used alone or in combination with one or more other
`co-reactants described above. Blocking agents and their
`mechanisms have been described in detail in “Blocked
`isocyanates III.: Part. A. Mechanisms and chemistry” by
`Douglas Wicks and Zeno W. Wicks Jr., Progress in Organic
`Coatings, 36 (1999), pp. 14-172. Preferred blocking agents
`include arylalcohols such as phenols, lactams such as e-ca
`prolactam, Ö-Valerolactam, Y-butyrolactam, oximes such as
`formaldoxime, acetaldoxime, cyclohexanone oXime,
`acetophenone oxime, benzophenone oxime, 2-butanone
`Oxime or diethylglyoxime. Further Suitable blocking agents
`include bisulfite and triazoles.
`
`0056. Other suitable fluorochemical topical treatments
`for use in the present invention include ZONYLTM 7713 or
`7040 (commercially available from E. I. DuPont de Nem
`ours & Co.). Preferred fluorochemical melt additives include
`oxazolidinones such as those described in U.S. Pat. No.
`5,099,026.
`0057. A variety of hot melt adhesives can be used in the
`invention. Preferred adhesives include LDPEs, atactic
`polypropylenes, propylene? 1-butenefethylene terpolymers,
`and propylene/ethylene, 1-butene/ethylene, and 1-butene/
`propylene copolymers. Other useful adhesives include those
`described in U.S. Pat. Nos. 3,932,329, 4,081,415, 4,692,370,
`5,248,719, 5,869,5612 and 6,288,149. The adhesive can also
`be a low basis weight thermoplastic scrim such as SHAR
`NETTM hot melt adhesive web from Bostik-Findley Com
`pany. The selection and processing of the hot melt adhesive
`will be familiar to those skilled in the art. Usually a hot melt
`adhesive will be present on both sides of the airflow resistive
`membrane. When adhesive layers are present on both sides
`of the membrane, the adhesive layers can be the same or
`different.
`0058) A variety of insulating mats and other porous
`spacing layers can be used in the invention. Preferred
`spacing layers include those described in U.S. Pat. Nos.
`4,837,067, 5,459,291, 5,504,282, 5,749,993, 5,773.375,
`5,824,973, 5,866,235, 5,961,904, 6,145,617, 6,296,075,
`6,358,592, and Re. 36,323, U.S. Published Patent Applica
`tion No. US 2001/0036788 A1 and PCT Published Appli
`cation No. WO 99/44817 A1. Other Suitable materials
`include the cotton and synthetic fiber vinyl acetate copoly
`mers available as “shoddy”, MARATEXTM, MARA
`BONDTM or MARABOND5TM from Janesville Products,
`Inc. The spacing layer can also be a space containing air or
`other gas. Techniques for fabricating Suitable spacing layers
`will be familiar to those skilled in the art.
`0059. The acoustical laminates of the invention can be
`placed adjacent to (e.g., adhered to) a variety of Sound
`reflective surface