carpet or carpet in plates

专利摘要:
carpet or carpet tiles the present invention relates to carpet and carpet tiles. in one aspect, the carpet includes (a) a main lining material having a face and a back; (b) a plurality of fibers attached to the main lining material extending from the face of the main lining material and exposed on the back of the main lining material; (c) an adhesive liner; (d) a secondary liner adjacent to the adhesive liner; and (e) at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition having an internal growth stress at 40 ° C and a residual strain strain of 25%. Additional steps and procedures include washing or cleaning the main lining and fibers before the extrusion step, and using implosion agents. the preferred thermoplastic polymer is an olefinic block copolymer and more preferably ethylene based block interpolymers. the constructions and methods described herein are particularly suitable for making wide-loom tufted carpet having improved abrasion resistance.
公开号:BR112012000352B1
申请号:R112012000352
申请日:2010-07-07
公开日:2020-01-14
发明作者:Weeks Ronald；Jin Yi
申请人:Dow Global Technologies Llc；
IPC主号:

专利说明:

"CARPET OR CARPET ON PLATES
Field of the invention [0001] This invention relates to rugs, floor mats and carpet coverings. Despite the many existing attempts to join carpet fibers using various polymers, such as polyethylene and polypropylene, there remains a need for a polymer-based system that is easy to apply and still maintains sufficient flexibility while maintaining minimal growth especially at high temperatures.
Background of the invention [0002] The invention provides a carpet or slab carpet comprising a main lining material having one side and one back, a plurality of fibers attached to the main lining material extending from the face of the main and exposed lining material on the back of the main lining material, an optional pre-coating, an adhesive lining material, an optional dimensional stability layer, an optional covering lining material, and a secondary lining material adjacent to the dimensional stability layer or material adhesive liner, at least one of the plurality of fibers, the main liner material, the optional pre-coating layer, the adhesive liner material, the optional dimensional stability layer, or the optional secondary liner material comprises at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition having an internal growth stress at 40 ° C, less than about 25 psi and a residual strain strain of 25% less than about 63%, preferably at least one composition or
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2/51 non-polyvinyl and non-chlorinated thermoplastic polymer may have a residual strain in 25% less than about 60%, more preferably less than about 55%, and / or an internal growth stress at 40 ° C less than or equal to about 10 psi.
[0003] The at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition can be selected from the group consisting of ethylene / vinyl acetate (EVA) polymers, ethylene / methyl acrylate (EMA) polymers, polymers of amorphous poly-alphaolefins (APAO), block olefinic copolymers (OBC) and homogeneously branched ethylene polymers. The at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition may have a storage module (G ') greater than 4.3 MPa at 70 ° C. The at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition may further comprise at least one tackifier.
[0004] The carpet or plate mat may have an olefinic block copolymer comprising a block ethylene interpolymer distinguished by having at least one or more of the following characteristics: (a) having Mw / Mn of about 1.7 to about of 3.5, at least one melting point, Tm, in degrees Celsius (° C), and a density d, in grams / cubic centimeter (g / cm ³ ), with the numerical values of Tm and d corresponding to the relationship : (a) Tm> -2002.9 + 4538.5 (d) 2422.2 (d) ² ; or (b) have Mw / M _n from about 1.7 to about 3.5, and are distinguished by a heat of fusion, Δη, in J / g, and a delta amount, Δτ, in degrees Celsius, defined as the temperature difference between the maximum DSC peak and the peak
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3/51 maximum CRYSTAF, with the numerical values of ΔΤ and Δη having the following relationships: ΔΤ> -0, 1299 (ΔΗ) + 62.81 for Δη greater than zero and up to 130 J / g, ΔT> 48 ° C for Δη greater than 130 J / g, with the peak of CRYSTAF determined using at least 5 percent of the cumulative polymer, and if less than 5 percent of the polymer has an identifiable CRYSTAF peak, then the CRYSTAF temperature will be 30 ° C; or (c) distinguished by a percentage elastic recovery, Re, in 300 percent deformation, and 1 cycle, measured with a compression molded film of the ethylene / a-olefin interpolymer, and having a density, d, in gram per cubic centimeter, with the numerical values of Re ed satisfying the following relationship when the ethylene / α-olefin interpolymer is substantially free of a crosslinked phase: R _e > 1481 - 1629 (d); or (d) have a molecular fraction that elutes between 40 ° C and 130 ° C when fractionated using TREF, characterized by having a molar comonomer content of at least 5 percent, greater than that of a comparable random ethylene interpolymer fraction eluting between the same temperatures, the said comparable random ethylene interpolymer having the same comonomers and having a melting index, density, and molar comonomer content (based on the whole polymer) within the 10 percent range of that of the interpolymer ethylene / α-olefin; or (e) characterized by a storage module at 25 ° C, G '(25 ° C), and a storage module at 100 ° C, G' (100 ° C), with the ratio G '( 25 ° C) for G '(100 ° C) is about 1: 1 to about 9: 1 and, preferably, the ethylene / α-olefin block interpolymer is separated by mesophase as described in PCT / US09 / 032699 and
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4/51 in the provisional U.S. serial patent application No. 61/024674 for multiblocks and the cases of distribution of controlled sequences are in PCT / US09 / 032705 and in the provisional U.S. serial patent application No. 61/024688.
[0005] Preferably, the carpet or plate rug is not optional.
[0006] The carpet of the invention is disclosed, in which (I) the fibers, main lining, adhesive lining and optional secondary lining all comprise a multi-block polyolefinic polymer, (II) the olefinic monomer chemistry of the adhesive lining differs from that of the fibers and the main lining, and (III) the carpet includes a label or literature at the time of sale that indicates that the carpet is recyclable without discrimination of carpet components.
[0007] The carpet or carpet of sheets of the invention is disclosed, the covering coating material or adhesive lining material further comprising (a) at least one charge in an amount greater than 0% and up to about 90 % by weight, based on the total weight of the material, the load being selected from the group consisting of dust and coal ash, ATH, CaCO ₃ , talc, recycled glass, magnesium hydroxide, ground tires, and ground carpet, ( b) optionally, at least one other polymer selected from the group consisting of MAH-g-HDPE, EEA, and EAA, (c) optionally, at least one oil, (d) optionally a color additive such as carbon black, and (e) from 0 to about 15 weight percent of at least one tackifier.
Summary of the invention [0008] This invention relates to carpets and methods for making carpets, the carpets comprising at least
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5/51 a flexible ethylene polymer lining material. In a particular case, the invention relates to a mat and a method for making a mat by an extrusion coating technique, each mat comprising a liner material comprising at least one block olefinic copolymer, especially block copolymers based on ethylene.
[0009] The present invention relates to any carpet constructed with a main lining material and includes tufted or non-tufted carpet such as needle-pierced carpet. Although specific incorporations deal with tufted carpets or not tufted carpets, tufted carpets are preferred.
[0010] Carpet liner formulations, especially those using copolymers in ethylene blocks, have improved sustainability along with larger load loads.
[0011] The pre-coating liner material, the adhesive liner material or the covering liner material can comprise at least one olefinic block copolymer.
[0012] The precoat may comprise olefinic block copolymer applied as a polyolefin dispersion, as a hotmelt adhesive polyolefin dispersion, as a hotmelt adhesive, or applied as a single layer or multilayer extrusion.
[0013] The adhesive layer comprising olefinic block copolymer can be applied as an extrusion coating, either applied as a single layer or multilayer extrusion, or as a hotmelt.
[0014] The secondary lining layer or coating of
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6/51 coating comprising block olefinic copolymer can be applied as an extrusion coating, either applied as a single layer or multilayer extrusion, or as a hotmelt.
[0015] Tufted rugs are composite structures that include yarns (also known as fiber bundles), a main lining material having one side and a back, an adhesive lining layer and, optionally, a secondary lining material. To form the face surface of tufted carpet, the yarns form tufts through the main lining material such that the longest length of each seam extends across the face surface of the main lining material. Typically, the main lining material is made of a woven or non-woven material such as a thermoplastic polymer, most commonly polypropylene or polyester.
[0016] The face of the tufted rug can be made in three ways. First, for loop pile carpet, the yarn ties formed in the tufting phase process are left intact. Second, for cut pile rug, the yarn loops are cut, either during or after the tufting phase, to produce a lot of insulated yarn ends instead of loops. Third, some styles of rugs include both a bunch of bows and cut threads. A variety of this third hybrid is referred to as sheared pile rugs where loops of different lengths form tufts followed by shearing the carpet at a height to produce a mixture of uncut loops, partially cut loops and completely cut loops. Alternatively, the tufting machine can be configured according to
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7/51 so as to cut only some of the loops, thus leaving a pattern of cut and uncut loops. Whether loop, cut loop or hybrid, the yarn on the back of the main lining material comprises firm non-extended loops.
[0017] The combination of tufted yarn and a main lining material without the application of an adhesive lining material or secondary lining material is referred to in the carpet industry as unprocessed tufted carpet or raw fabric.
[0018] Raw fabric becomes finished tufted carpet with the application of an adhesive lining material and an optional secondary lining material on the back of the main lining material. The finished tufted rug can be prepared as a wide loom tufted rug in cylinders typically 6 or 12 feet wide.
[0019] Alternatively, the carpet can be prepared as a carpet in plates, typically 50 cm ² .
[0020] The adhesive lining layer is applied to the back of the main lining material to fix the threads in the main lining material. Typically, the adhesive liner material is applied by a disc applicator using a cylinder, a rotating cylinder or a bed, or a knife (also called a scalpel) on a rotating cylinder or bed. The properly applied adhesive liner materials do not substantially pass through the main liner material.
[0021] Very often, adhesive liner material is applied as a single coating or layer. The extent and toughness with which the wire is affixed is referred to as tuft lock or tuft bonding resistance. Carpets with
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8/51 sufficient tuff bond strength exhibits good wear resistance and, as such, has long service lives. Also, the adhesive liner material must substantially penetrate the exposed yarn (bundle of fibers) on the back of the adhesive liner material and must substantially consolidate individual fibers within the yarn.
[0022] Good penetration of the yarn and consolidation of fibers produces good resistance to abrasion. In addition, in addition to good tuft bonding resistance and abrasion resistance, the adhesive material should also provide or allow good flexibility to the carpet in order to facilitate easy installation of the carpet. Typically, the secondary lining material is a lightweight canvas made of woven or non-woven material such as a thermoplastic polymer, most commonly polypropylene. Optionally, the secondary lining material is applied to the back of the carpet over the main lining material, to provide mainly improved dimensional stability to the carpet structure as well as to provide more surface area for the application of direct bonding adhesives.
[0023] Alternative lining materials can also be applied on the back of the adhesive lining material and / or on the back of the secondary lining material, if present.
[0024] Alternative lining materials may include foam padding (eg, polyurethane foam) and pressure sensitive floor adhesives. Alternative lining materials can also be applied, for example, as a shoelace with improved surface area, to facilitate installation of direct bonding adhesives (for example, contraction treadmill, car mat and floor mat).
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9/51 airplanes where the need for padding is often minimal). Alternative lining materials can also be optionally applied to improve barrier protection against moisture, insects, and food products as well as providing or improving fire extinguishing, thermal insulation, and sound dampening properties.
[0025] Known adhesive liner materials include curable latex, urethane or vinyl systems, latex systems being very common. Conventional latex systems are low viscosity aqueous compositions that apply at high carpet production rates, and offer good fiber adhesion to the ceiling, good tuft bonding strength and adequate flexibility. Generally, excess water is removed and the latex is cured by passing it through a drying oven. Styrene / butadiene rubbers (SBR) are the most common polymers used as latex adhesive liner materials. Typically, the latex lining system is heavily loaded with an inorganic filler such as calcium carbonate or aluminum hydroxide and includes other ingredients such as antioxidants, antimicrobials, flame retardants, smoke eliminators, humectants, and sponge aids.
[0026] Conventional latex adhesive liner systems may have certain disadvantages. As an important disadvantage, typical latex adhesive liner systems do not provide a moisture barrier. Another possible drawback, particularly with a carpet having polypropylene yarns and polypropylene main and secondary lining materials, is that the polymer other than latex systems together with the inorganic filler can
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10/51 reduce the recycling capacity of the carpet.
[0027] In view of these disadvantages, some in the carpet industry have started looking for suitable substitutes for conventional latex adhesive liner systems. An alternative is the use of urethane adhesive liner systems. In addition to providing adequate adhesion to consolidate the carpet, urethane liners generally exhibit good flexibility and good barrier properties and, when in the form of foam, can eliminate the need for separate underlying quilting (ie they can constitute a lining system direct bonding unit). However, urethane lining systems can also have important disadvantages, including their relatively high cost and strict curing requirements that require application of low carpet production rates compared to latex systems.
[0028] Thermoplastic polyolefins such as ethylene / vinyl acetate copolymers (EVA) and low density polyethylene (LDPE) have been suggested as adhesive liner materials due in part to their low cost, good moisture stability and no requirement for moisture. cure. There are several methods available for applying polyolefin liner materials, including powder coating, hotmelt application and extruded film or foil lamination.
[0029] However, the use of polyolefins to replace latex adhesive liners also presents difficulties. For example, Table A in column 10 of U.S. Patent No. 5,240,530, indicates that usual polyolefin resins have inadequate adhesion for use in carpet making. In addition, in relation to yacht systems and other cured systems, common polyolefins have viscosities of
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11/51 relatively high application and relatively high thermal requirements. That is, common thermoplastic polyolefins are characterized by melt viscosities, relatively high and high recrystallization or solidification temperatures compared to typical aqueous viscosities and curing temperature requirements characteristic of latex systems and other cured (thermoset) systems .
[0030] Even common elastomeric polyolefins, i.e. polyolefins having low crystallinity, generally have relatively high viscosities and relatively high recrystallization temperatures. Relatively high recrystallization temperatures result in relatively short melting times during processing and, combined with high melt viscosities, can make it difficult to achieve adequate wire penetration, especially at conventional adhesive liner rates. One method to overcome the viscosity deficiencies and recrystallization of common polyolefins is to formulate the polyolefin resin as a hotmelt adhesive that usually involves formulating low molecular weight polyolefins with waxes, tackiness agents, various flow modifiers and / or other elastomeric materials. In formulating hotmelt adhesive liner compositions, for example, ethylene / vinyl acetate (EVA) copolymers have been used, and other polyolefin compositions have also been proposed as hotmelt liner compositions. For example, in U.S. Patent No. 3,982,051, Taft et al., Disclose that a composition comprising an ethylene / vinyl acetate copolymer, atactic polypropylene and vulcanized rubber, is useful as a
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12/51 hotmelt carpet lining adhesive.
[0031] Unfortunately, in general, hotmelt adhesive systems are not considered to be completely suitable substitutes for conventional latex adhesive liners. Typical hotmelt systems are based on EVA and other ethylene copolymers and unsaturated comonomers may require considerable formulation and still often produce inadequate tuft bond strengths. However, the most significant deficiency of a typical hotmelt system is its melt strength which is generally too low to allow application by a direct extrusion coating technique. As such, polyolefin hotmelt systems are typically applied to the main linings by relatively slow and less efficient techniques such as using heated scalpels or rotating cast cylinders.
[0032] Although it is possible to apply high pressure low density polyethylene (LDPE) by a conventional extrusion coating technique, LDPE resins typically have less flexibility which can result in excessive carpet stiffness.
[0033] On the other hand, those common polyolefins that have improved flexibility, such as ultra low density polyethylene (ULDPE) and ethylene / propylene interpolymers, do not yet have sufficient flexibility, have excessively low melt strengths and / or tend to resonate the stretching during extrusion coating. To overcome the difficulties of extrusion coating, common polyolefins with sufficient flexibility can be applied by lamination techniques to ensure adequate yarn adhesion
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13/51 to the lining; however, lamination techniques are typically expensive and can result in extended production rates over direct extrusion coating techniques.
[0034] Known examples of flexible polyolefin lining materials are disclosed in U.S. Patent Nos. 3,390,036, 3,583,936, 3,745,054, and 3,914,489. In general, these disclosures describe hotmelt adhesive liner compositions based on an ethylene copolymer, such as ethylene / vinyl acetate (EVA), and waxes. Known techniques for improving the penetration of hotmelt adhesive liner compositions through the yarns include applying pressure while the raw fabric is in contact with rotary melt transfer cylinders as described, for example, in U.S. Patent No. 3,551,231.
[0035] Another known technique for improving the effectiveness of hotmelt systems involves the use of pre-coating systems. For example, U.S. Patent Nos. 3,684,600, 3,583,936, and 3,745,054, describe the application of low viscosity aqueous precoats on the back of the main liner material prior to the application of a hotmelt adhesive composition.
[0036] The hotmelt adhesive liner systems disclosed in these patents are derived from the formulation of multicomponents based on functional ethylene polymers such as, for example, ethylene / ethyl acrylate (EEA) and ethylene / vinyl acetate (EVA) copolymers ).
[0037] Although there are several systems known to the carpet lining technique, there remains a need for a thermoplastic polyolefin carpet lining system that provides adequate tuft bond strength, good resistance to
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14/51 abrasion and good flexibility to replace cured latex liner systems. There is also a need for an application method that allows high rates of carpet production and, at the same time, achieves the desired characteristics of good tuft bonding strength, good abrasion resistance, good barrier properties and good flexibility. Finally, there is also a need to provide a carpet structure having fibers and lining materials that are easily recyclable without the need for extensive handling and discrimination of carpet component materials. According to one aspect of the present invention, a carpet comprises a plurality of fibers, a main lining material having a face and a back, an adhesive lining material and an optional secondary lining material, the plurality of fibers attached to the material of main lining and protruding from the face of the main lining material and exposed on the back of the main lining material, adhesive lining material arranged on the back of the main lining material and the optional secondary lining material adjacent to the adhesive lining material, at least one of the plurality of fibers, the main lining material, the adhesive lining material or the optional secondary lining material comprises at least one olefinic block copolymer. Another aspect of the present invention is a method of manufacturing a carpet, the carpet including a plurality of fibers, a main lining material having one side and a back, an adhesive lining material and an optional secondary lining material, the plurality of fibers attached to the main lining material and protruding from the face of the main lining material and exposed on the back of the lining material
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Main 15/51, the method comprising the step of extruding the adhesive lining material or the optional secondary lining material over the back of the main lining material, the adhesive lining material or the optional coated secondary lining material by extrusion comprises at least one block olefinic copolymer, especially ethylene-based block interpolymers, characterized by an average block index greater than zero and up to about 1.0 and a molecular weight distribution, M _w / M _n , greater than about 1.3. In another aspect, the invention relates to an ethylene / a-olefin interpolymer comprising polymerized ethylene and aolefin units, the average block index being greater than 0 (zero) but less than about 0.4 and a molecular weight distribution, Mw / Mn, greater than about 1.3. Preferably, the interpolymer is a linear multi-block copolymer with at least three blocks. Also preferably, the ethylene content in the interpolymer is at least 50 mole percent. [0038] Another aspect of the present invention is a method of manufacturing a carpet, the carpet having a matrix of non-expanded and deformed adhesive lining material and comprising yarns attached to a main lining material, the adhesive lining material comprising at least at least one ethylene polymer and in close contact with the main lining material and has the wires substantially penetrated and substantially consolidated, the method comprising the step of adding an effective amount of at least one implosion agent to the adhesive lining material and thereafter , activate the implosion agent during an extrusion coating step such that the melted or semi-melted polymer is
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16/51 forced in the free space of wires exposed on the back of the main lining material.
[0039] Another aspect of the present invention is a method of manufacturing a carpet, the carpet having a face and comprising yarns, a main lining material, an adhesive lining material and an optional secondary lining material, the material of which is main lining has a back side opposite the face of the carpet, the threads bond to the main lining material, the adhesive lining material is applied to the back of the main lining material, the method comprising the step of stripping, washing or sandblasting the back of the main liner material with water vapor, solvent and / or heat before applying the adhesive liner material to detach or remove substantially processing materials.
[0040] The terms, "intimate contact," substantial encapsulation, and / or "substantial consolidation are used here referring to mechanical adhesion or mechanical interactions (opposite to chemical bonding) between different components of the mat, regardless of one or more components whether or not they are capable of chemically interacting with another component of the mat. With respect to the interactions or mechanical adhesions of the present invention, there may be some effective amount of inter-mixing or inter-fusion of polymeric materials; however, there is no integral or continuous fusion of various components determined from visual inspection of photomicrographs (at 20x magnification) of the various interfaces of the carpet. Within this meaning, fusion of individual strands or bundles of fibers or fibers to one another within a bundle of fibers is not considered integral fusion in itself since the fibers
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17/51
are here referred to as a component of the carpet.[0041] O term “Intimate contact refers to the interaction mechanics between the back of the main lining material and O material in lining adhesive.[0042] O term “Substantial encapsulation refers to to material in lining adhesive that significantly surrounds the
yarns or bundles of fibers at or very close to the interface between the back of the main lining material and the adhesive lining material. The term "substantial consolidation" refers to the overall integrity and dimensional stability of the carpet that is achieved by substantially encapsulating the strands or bundles of fibers and intimately contacting the back of the main lining material with the adhesive lining material. A substantially consolidated carpet has good component cohesion and good resistance to delamination with respect to the various components of the carpet.
[0043] The term “integral melting with the same sense known in the art is used here and refers to the thermal bonding of carpet components using a temperature above the melting point of the adhesive liner material. Integral fusion occurs when the adhesive liner material comprises the same polymer as the fibers or the main liner material or both.
[0044] However, integral fusion does not occur when the adhesive lining material comprises a polymer different from that of the fibers and the main lining material. The term “same polymer means that the monomer units of the polymers are chemically the same, although their molecular or morphological attributes may differ. On the other hand, the term “different polymer means that, regardless of
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18/51 of any molecular or morphological differences, the monomer units of the polymers are chemically different. Thus, according to the various definitions of the present invention, a polypropylene backing material and a polyethylene adhesive backing material would not fully melt because these carpet components are chemically different. The term “carpet component” is used here to refer separately to the fiber bundles of the carpet, the main lining material, the adhesive lining material and the optional secondary lining material.
[0045] The term “extrusion coating in its conventional sense is used here to refer to an extrusion technique in which a polymeric composition is heated, usually in the form of pellets, in an extruder at an elevated temperature above its temperature melting and then forced through a die of fine extrudates to form a web of semi-melted or fused polymer. The semifused or fused polymer web is continuously stretched over a raw fabric fed continuously to coat the back of the raw fabric with the polymeric composition. An extrusion process can be useful in the present invention, where, in lamination, the face of the raw fabric is oriented in the direction of the laminating cylinder and the back of the adhesive liner material is oriented in the direction of the laminating pressure cylinder. Extrusion coating is distinct from a lamination technique.
[0046] The term “lamination technique in its conventional sense is used here to refer to the application of adhesive liner materials to raw fabrics forming, first, the
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19/51 adhesive liner material such as a solidified or substantially solidified sheet or film and thereafter, in a separate processing step, reheating or raising the temperature of the sheet or film before applying it to the back of the main liner material. The term “heat content” is used here to refer to the mathematical product of the thermal capacity and relative density of a load. Loads characterized by having high heat content are used in specific embodiments of the present invention to extend the solidification or melting time of the adhesive liner materials. The manual for chemical technicians, by Howard J. Strauss and Milton Kaufmann, McGraw Hill Book Company, 1976, sections 1-4 and 2-1, provides information regarding the thermal capacity and relative density of selected mineral fillers. The fillers suitable for use in the present invention do not change their physical state (i.e., remain a solid material) over all the extrusion coating processing temperature ranges of the present invention.
[0047] Preferred loads with high content of heat have a combination of high density relative it's from elevated thermal capacity. [0048] The term is used here "agent in implosion for
refer to the use of conventional blowing agents or other compounds that eliminate gases or cause degassing when activated by heat, usually at some particular activation temperature. In the present invention, implosion agents are used to implode or force the adhesive liner material into spaces free of threads or bundles of fibers.
[0049] The term “processing material is used here to refer to substances such as finishing waxes
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20/51 per rotation, equipment oils, finishing agents and the like, which may interfere with the physical or adhesive interfacial interactions of the adhesive liner materials. The processing materials can be removed or displaced by a stripping or washing technique of the present invention through which improved mechanical bonding is performed. The terms "polypropylene carpet and" raw polypropylene fabric are used here to mean a raw carpet or fabric comprised substantially of polypropylene fibers, regardless of whether the main lining material for the carpet or for the raw fabric is comprised of polypropylene or some other material.
[0050] The terms "nylon carpet and" raw nylon fabric are used here meaning a carpet or raw fabric comprised substantially of nylon fibers, regardless of whether the main lining material for the carpet or the raw fabric is understood made of nylon or some other material.
[0051] The term “linear, when used to describe ethylene polymers, is used here to mean that the polymeric main chain of the ethylene polymer is devoid of measurable or demonstrable long chain branches, for example, the polymer is replaced with less than 0.01 long chain branch / 1000 carbons.
[0052] The term "homogeneous ethylene polymer, when used to describe ethylene polymers, is used in the conventional sense according to the original disclosure by Elston in US patent No. 3,645,992 to refer to an ethylene polymer in which the comonomer is randomly distributed within a given polymer molecule and in the
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21/51 which substantially all of the polymer molecules have substantially the same molar ratio of ethylene to comonomer. As defined herein, both substantially linear ethylene polymers and homogeneously branched linear ethylene polymers are homogeneous ethylene polymers.
[0053] Olefinic block copolymers, especially ethylene-based block interpolymers, are described and claimed in several patent applications, including US patent No. 7,355,089 (Chang et al.), Incorporated herein by reference, WO 2005 / 090425, WO 2005/090426 and WO 2005/090427.
[0054] We have found that olefinic block copolymers, especially ethylene-based block interpolymers, offer unique advantages for extrusion-coated carpet lining applications, especially for commercial and residential carpet markets. Block olefinic copolymers, especially block interpolymers based on ethylene, have low solidification temperatures, good adhesion to polypropylene, and low modulus compared to conventional ethylene polymers such as low density polyethylene (LDPE), linear low density polyethylene heterogeneously branched (LLDPE), high density polyethylene (HDPE) and heterogeneously branched ultra low density polyethylene (ULDPE). As such, olefinic block copolymers, especially ethylene-based block interpolymers, are useful for manufacturing carpet fibers, main lining materials, adhesive lining materials and optional secondary lining materials. However, olefinic block copolymers, especially
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22/51 ethylene-based block interpolymers are particularly useful as adhesive liner materials for tufted and non-tufted carpets (eg needle-pierced carpet) and are especially useful for tufted carpets.
[0055] In the present invention, during extrusion coating of the carpet lining to apply an adhesive lining material, interpolymers in appropriately selected ethylene blocks show good penetration of carpet yarns (fiber bundles) and also good consolidation of the fibers within of the wires.
[0056] When used in tufted carpets, the tuft bonding resistance and abrasion resistance of the carpet are increased by the penetration of interpolymers in ethylene blocks in the threads. Preferably, a tuft bond strength (or tuft lock) greater than or equal to 1.5 kg (3.25 pounds) is achieved, more preferably greater than or equal to
2.3 kg (5 pounds) and most preferably greater than or equal to
3.4 kg (7.5 pounds). In addition to increased penetration of the threads, it is also possible to increase the bond strength of tufts by increasing the molecular weight of the polymer. However, a higher molecular weight of polymer selected to improve tuft bond strength is against the requirement for a lower molecular weight that is generally required for good wire penetration and good extrusion coating capacity. Also, higher polymer densities are desirable to improve chemical and barrier resistance, since higher densities invariably produce rigid carpets. As such, the polymer properties should be chosen such that a balance is maintained between the
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23/51 extrusion coating capacity and abrasion resistance as well as between chemical resistance and the flexibility of the carpet.
[0057] When raw carpet fabrics are lined with interpolymers in appropriately selected blocks of ethylene, the low flexural modulus of these polymers offers advantages in the easy installation of the carpet and in the general handling of the carpet.
[0058] In particular, interpolymers in ethylene blocks when used as adhesive lining material show better mechanical adhesion to polypropylene which improves the consolidation and resistance to delamination of the various layers of carpet and components, that is, polypropylene fibers, bundles fibers, the main lining material, the adhesive lining material and the secondary lining material when optionally employed. Consequently, abrasion resistance and exceptionally good tuft bond strength can be obtained. Good abrasion resistance is especially important in commercial carpet cleaning operations as good abrasion resistance generally improves the durability of the carpet.
[0059] Interpolymers in appropriately selected ethylene blocks can allow the elimination of secondary liner materials and as such can result in significant savings in manufacturing costs. In addition, carpets adhesive-lined with an interpolymer in ethylene blocks can provide a substantial fluid and particle barrier which improves the hygienic properties of the carpet. An interpolymer adhesive liner material in ethylene blocks can allow the production of carpets
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24/51 fully recyclable particularly where the carpet comprises polypropylene fibers.
[0060] Furthermore, mixing an interpolymer in ethylene blocks with a polypropylene resin suitable for fibers can result in an impact-modified recycling composition that is useful for injection molding and other molding applications as well as reuse in carpet making , for example, as the main lining material or as a mixing component of the polymer composition of adhesive lining material. That is, mixtures of olefinic polymers may involve polymer chemistries, compatibility, and / or miscibility sufficiently similar to allow good recyclability without having sufficient similarities to allow integral melting.
[0061] Preferred block olefinic copolymers, especially ethylene block copolymers have a single melting peak between -30 ° C and 150 ° C, determined using differential scanning calorimetry (DSC). Preferably, the ethylene-based block interpolymer has a single melting peak measured by DSC between -30 ° C and 150 ° C, usually between about 100 and about 130 ° C. The ethylene-based block interpolymers used in the present invention are characterized by a single melting peak by DSC. The single melting peak is determined using a differential scanning calorimeter standardized with indium and deionized water. The method involves sample sizes of 5-7 mg, a “first heating to about 140 ° C that is maintained for 4 minutes, a cooling at a rate of 10 ° C / min to -30 ° C, which is maintained for 3 minutes and a heating at a rate of 10 ° C / min to 150 ° C for the “second heating. The single melting peak is taken from the
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25/51 heat flow curve of “second heating against temperature. The total heat of melting of the polymer is calculated from the area under the curve.
[0062]
All samples of the product polymer and individual polymeric components are analyzed by gel permeation chromatography (GPC) in a Waters 150 high temperature chromatographic unit equipped with three mixed porosity columns (10 ³ , 104, 10 ⁵ and 10 ⁶ Â), operating at a system temperature of 140 ° C. The solvent is 1,2,4trichlorobenzene, from which solutions of 0.3 percent by weight of the samples for injection are prepared. The flow rate is 1 mL / min and the injection volume is given in microliters (pL). Molecular weights are calculated using polystyrene narrow molecular weight distribution standards (from Polymer Laboratories) together with their elution volumes. the equivalent molecular weights of polyethylene are determined using appropriate Mark-Houwink coefficients for polyethylene and polystyrene (as described in Williams and Ward in the Journal of Polymer Science, Polymer Letters, Vol. 6, p. 621 (1968)) to derive the following equation ^M polyethylene ^{a (M} poly styrene in which a = 0.4315 and b = 1.0.
[0063]
The numerical average molecular weight, Mn, is calculated in the usual way according to the following formula:
M _n = Σ n _i M _i / Z n _i = w / Σ (w _i / M _i ) where n _i = number of molecules with molecular weight M _i ; w = total material weight; and Σ n _i = total number of molecules.
[0064] The weight average molecular weight, M _w , is calculated in the usual way according to the formula:
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26/51
M _w = Σ Wi * Mi where w _i * and M _i are, respectively, the weight fraction and molecular weight, of the i-th fraction eluting from the GPC column. The block index and the hard segment / soft segment ratio can be measured according to US 11 / 376,835 and EP 1 716 190 B1.
[0065] Suitable block olefinic copolymers, especially block copolymers based on ethylene for use in the present invention include interpolymers of ethylene and at least one alpha-olefin prepared by solution polymerization, gas or mud ( semi-fluid paste) or combinations thereof. The appropriate alpha-olefins are represented by the following formula: CH2 = CHR * where R * is a hydrocarbyl radical. In addition, R * can be a hydrocarbyl radical having from one to twenty carbon atoms and, as such, the formula includes C3-C20 alpha-olefins. Alpha-olefins suitable for use as comonomers include propylene, 1-butene, 1-isobutylene, 1-pentene, 1hexene, 4-methyl-1-pentene, 1-heptene and 1-octene, as well as other types of comonomers such as styrene, styrenes substituted with halogen or alkyl, tetrafluoroethylene, vinyl benzocyclobutane, 1,4-hexadiene, 1,7-octadiene, and cycloalkenes, for example, cyclopentene, cyclohexene and cyclooctene. Preferably, the comonomer will be 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-heptene, 1-octene or mixtures thereof, since adhesive liner materials comprising higher alpha-olefins will have toughness especially improved. The term interpolymer means that the main (dominant) monomer is copolymerized with at least one other comonomer. So the
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27/51 term interpolymer can refer to a copolymer as well as to terpolymers (3 monomers) and the like. However, most preferably, the comonomer will be 1-octene and the ethylene polymer will be prepared in a solution process.
[0066] The density of interpolymers in ethylene-based blocks, measured according to ASTM D-792, will generally not exceed 0.92 g / cm ³ , and is generally in the range of about 0.85 g / cm3 to about 0.92 g / cm3, preferably from about 0.86 g / cm ³ to about 0.92 g / cm ³ , and especially from about 0.86 g / cm ³ to about 0, 90 g / cm ³ . The molecular weight of the ethylene-based block copolymer is conveniently indicated using a melt index measure according to ASTM D-1238, Condition 190 ° C / 2.16 kg (formerly known as Condition (E) and also known as I2). The melt index is inversely proportional to the molecular weight of the polymer. Consequently, the higher the molecular weight, the lower the melting index, although the relationship is not linear. In general, the melting index of the interpolymers in ethylene-based blocks is from about 1 g / 10 min to about 500 g / 10 min, preferably from about 2 g / 10 min to about 300 g / 10 min, more preferably from about 5 g / 10 min to about 100 g / 10 min, especially from about 10 g / 10 min to about 50 g / 10 min, and most especially from about 25 g / 10 min at about 35 g / 10 min. Another useful measure in characterizing the molecular weight of ethylene-based block interpolymers is conveniently indicated using a melt index measure according to ASTM D-1238, Condition 190 ° C / 10 kg (formerly known as Condition (N) and also known as I ₁₀ ). The ratio of the fusion indices I ₁₀ and I ₂ is the melt flow ratio,
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28/51 designated as I ₁₀ / I ₂ . The I ₁₀ / I ₂ ratio of the ethylene-based block interpolymers is at least 6.5, preferably at least 7, especially at least 8.
[0067] The preferred ethylene polymers for use in the present invention have relatively low modulus. That is, the ethylene polymer is characterized by having an elasticity modulus of 2% less than 163.3 MPa (24,000 psi), especially less than 129.3 MPa (19,000 psi) and much less than 95.2 MPa (14,000 psi), measured according to ASTM D 790.
[0068] The preferred ethylene polymers for use in the present invention are substantially amorphous or totally amorphous. That is, the ethylene polymer is characterized by having a percentage of crystallinity less than 40 percent, preferably less than 30 percent, more preferably less than 20 percent and most preferably less than 10 percent, measured by differential calorimetry of scan using the equation:% crystallinity = (Hf / 292) * 100, where Hf is the heat of fusion in Joule / gram (J / g). The olefinic block copolymer, especially ethylene block interpolymers can be used alone or can be mixed or combined with one or more natural or synthetic polymeric materials. Polymers suitable for combining or mixing with olefinic block copolymers, especially ethylene-based block interpolymers used in the present invention include, but are not limited to, other olefinic block copolymers, especially block interpolymers of ethylene, low density polyethylene, Heterogeneously branched LLDPE, Heterogeneously branched ULDPE, medium density polyethylene, high density polyethylene
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29/51 density, grafted polyethylene (for example, heterogeneously branched linear low density polyethylene grafted by extrusion with maleic anhydride or branched ultra low density polyethylene grafted with maleic anhydride (MAH-g)), ethylene / acrylic acid copolymer, copolymer ethylene / vinyl acetate, ethylene / ethyl acrylate copolymer, polystyrene, polypropylene, polyester, polyurethane, polybutylene, polyamide, polycarbonate, rubbers, ethylene / propylene polymers, ethylene / styrene polymers, styrene block copolymers, and vulcanates. The actual combination or blending of various polymers can conveniently be performed by any method known in the art including, but not limited to, melt extrusion composition, dry blending, lamination, melt blending as in a Banbury mixer and polymerization in multiple reactors. Preferred combinations and mixtures include a block olefinic copolymer, especially ethylene-based block interpolymers and a heterogeneously branched ethylene / alpha-olefin interpolymer in which the alpha-olefin is a C3-C8 alpha-olefin prepared using two reactors operated in parallel or in series with different catalytic systems employed in each reactor.
[0069] A range of resin properties, processing conditions and equipment configurations were found for carpet lining systems capable of being extruded coated that perform similarly or better than latex and polyurethane systems in use. Pre-coatings, laminate coatings, and polyolefin foam coatings can be prepared by known methods
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30/51 of those with usual knowledge in the art of preparing such linings. Pre-coatings, laminate coatings, and foam coatings prepared from such dispersions are described in P. L. Fitzgerald, “Integral
Dispersion Foam Carpet Cushioning, J. Coat. Fab. 1977, volume 7 (pp. 107-120), and in R. P . Brentin, "Dispersion Coating Systems for Carpet Backing , J. Coat. Fab. 1982, volume 12 (pp. 82-91). [0070] Preferably, extrude if two layers in
resin, each layer comprising a different resin, with the layer applied directly to the back of the main lining material (first layer) having a melting index higher than the second layer that is applied to the back of the first layer. Since the first layer that is entrusted to encapsulate and penetrate the strands, this layer must have a sufficiently high melt index (melt viscosity low enough) to promote encapsulation and penetration of the strands. The second layer, which is generally not relied on to encapsulate and penetrate the threads, can be used either as the bottom surface of the carpet or to facilitate the application of an optional secondary lining material. For both of these uses, it is preferred to have a lower melt index to provide greater resistance after cooling. Furthermore, because it is not relied on to encapsulate or penetrate the bundles of fibers, a resin of lesser quality and / or less tightly controlled properties can be used in the second layer. In a preferred embodiment, the second layer is a recycled raw material.
[0071] Likewise, the first layer and the second layer may consist of polymer compositions or chemicals
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Different 31/51. For example, the first layer may be comprised of an adhesive polymer (as an additive or as the entire layer composition) such as, but not limited to, an ethylene / vinyl acetate copolymer, an ethylene / acrylic acid copolymer or an ethylene polymer graft with maleic anhydride (preferably an ethylene block interpolymer grafted by extrusion with maleic anhydride or a high density polyethylene grafted by extrusion with maleic anhydride) and the second layer may comprise a non-polar polymer such as an olefinic block copolymer, spatially block copolymers based on ethylene, a low density polyethylene or an ultra low density polyethylene. Alternatively, the first layer can comprise a non-polar polymer and the second layer can comprise an adhesive polymer. Preferably, the first layer has an I2 melt index between about 5 and about 175 g / 10 minutes, and the second layer has an I2 melt index between about 1 and about 70 g / 10 minutes. Most preferably, the first layer has an I2 melt index between about 30 and about 70 g / 10 minutes, and the second layer has an I2 melt index between about 10 and about 30 g / 10 minutes. It is also preferred to extrude two layers of a single polymer composition in order to have greater control over the thickness or weight of the resin applied to the carpet.
[0072] In alternative embodiments, three or more layers of the resin can be extruded on the back of the main lining material to achieve even greater coating weights and / or to obtain a more gradual transition between the first and the last applied layer. Preferably, it is used
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32/51 a double edge matrix to apply two layers. Alternatively, two or more extrusion stations or a single edge co-extrusion die can be used to apply these two or more layers. Another aspect of the present invention is the use of modified olefinic block copolymer, especially ethylene-based block interpolymers. Appropriate grafting techniques are described in U.S. Patent Nos. 4,762,890, 4,927,888, 4,230,830, 3,873,643, and 3,882,194, the disclosure of each of which is incorporated herein entirely by reference.
Preferred adhesive polymeric additives for use in the present invention are maleic anhydride grafts in which maleic anhydride is grafted onto an ethylene polymer in a concentration of about 0.1 to about 5.0 weight percent, preferably about 0.5 to about 1.5 weight percent. The use of maleic anhydride grafts in ethylene polymer as an adhesive polymeric additive in the present invention significantly improves the performance and the operational window of the adhesive lining material, especially for polar polymer such as, but not limited to, face-faced carpets nylon and polyester. The improvement relates to substantially greater comparative tuft bond strength and abrasion resistance. The improvement was surprising due to the fact that grafted adhesives are generally known to require extended fused or semi-melted contact times for improved performance and function when interlayer adhesives for films and coatings where there is a continuous substrate opposite the existing discontinuous interface in carpet manufacturing. The preferred ethylene polymers for use as the
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The grafted host polymer includes low density polyethylene (LDPE), high density polyethylene (HDPE), heterogeneously branched linear low density polyethylene (LLDPE), homogeneously branched linear ethylene polymers and substantially linear ethylene polymers. Preferred host ethylene polymers have a density greater than or equal to 0.915 g / cm ³ and most preferably greater than or equal to 0.92 g / cm ³ . Block interpolymers based on ethylene and high density polyethylene are the preferred host ethylene polymers.
[0074] In this aspect of the present invention, the polymeric adhesive additive is added to the olefinic block copolymer, especially ethylene-based block copolymers, at a level in the range of about 0.5 to about 30 weight percent, preferably from about 1 to about 20 weight percent, more preferably from about 5 to about 15 weight percent, based on the total weight of the polymer. For maleic anhydride grafts in preferred ethylene polymers, the additions must provide a final maleic anhydride concentration in the range of about 0.01 to about 0.5 weight percent, preferably from about 0.05 to about 0.2 percent by weight, based on the total weight of the polymer. Extruded polymers can be used neat or they can have one or more additives included. A preferred additive is an inorganic filler, more preferably, an inorganic filler with a high heat content. Examples of such charges include, but are not limited to, coal dust and ash, calcium carbonate, aluminum hydroxide, talc, barite. Loads with high heat content are believed to be advantageous in
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34/51 invention because such loads allow the extrudate to remain longer at elevated temperatures with the beneficial result of providing better encapsulation and penetration. That is, charges are usually added to the carpet lining materials merely to increase the volume (i.e., as extenders) or to impart insulation and sound-damping characteristics. However, we have found that inorganic mineral fillers that have high heat content surprisingly improve yarn encapsulation and penetration, which in turn improves the abrasion resistance performance and the bond strength of tufts of extruded coated carpet samples.
[0075] Preferably, a load with a high heat content is added at a level between about 1 and about 75 weight percent of the total extrudate, preferably between about 15 and about 60 weight percent and most preferably between about 20 and about 50 weight percent. Such charges will have a specific heat content greater than or equal to 1.8 Joule-cm ³ / ° C (0.4 cal-cm ³ / ° C), preferably greater than or equal to 2 Joule-cm ³ / ° C (0, 5 cal-cm ³ / ° C), more preferably greater than or equal to 2.5 Joule-cm ³ / ° C (0.6 calcm ³ / ° C) and most preferably greater than or equal to about 2.9 Joule- cm ³ / ° C (0.7 cal-cm ³ / ° C). Representative examples of high heat content fillers for use in the present invention include, but are not limited to, limestone (mainly CaCO3), marble, quartz, silica and barite (mainly BaSO4). Loads with a high heat content must be ground or precipitated to a size that can be conveniently incorporated into an extrusion coating melt stream. Particle sizes
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Appropriate 35/51 ranges from about 1 to about 100 microns. If a foam lining is desired on the mat, an expansion agent can be added to the adhesive lining material and / or to the optional secondary lining material. If used, the blowing agents are preferably conventional heat-activated blowing agents such as azodicarbonamide, toluene sulfonyl semicarbazide, and oxy bis (benzene sulfonyl) hydrazide. The amount of blowing agent added depends on the degree of sponging sought. A typical level of blowing agent is between about 0.1 and about 1.0 weight percent.
[0076] Other additives can be included in the adhesive liner material, to the extent that they do not interfere with the improved properties discovered by the applicants. For example, antioxidants such as sterically hindered phenols, sterically hindered amines and phosphites can be used. Suitable antioxidants include IRGANOX ™ 1010 from Ciba-Geigy which is a hindered phenol and IRGAFOS ™ 168 from CibaGeigy which is a phosphite. Other possible additives include non-stick additives, pigments and dyes, antistatic agents, antimicrobial agents (such as quaternary ammonium salts) and chilled lamination cylinder release additives (such as fatty acid amides). As noted above, the carpet of the invention preferably also includes a secondary lining material. Preferably, the secondary lining material is laminated directly to the extruded layers while the extrudate is still melted after extrusion coating. It has been found that this technique can improve the penetration of the extrusion coating into the main lining.
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36/51 [0077] Alternatively, the secondary lining material can be laminated at a later stage by reheating and / or re-melting at least the outermost portion of the extruded layer or by a co-extrusion coating technique using at least two applied extruders. Also, the secondary lining material can be laminated by some other means, such as by interposing a layer of a polymeric adhesive material between the adhesive lining material and the secondary lining material.
[0078] Suitable polymeric adhesive materials include, but are not limited to, ethylene / acrylic acid (EAA) copolymers, ionomers and polyethylene compositions grafted with maleic anhydride. The manufacture of extruded carpet and the methods described herein are particularly suitable for making carpet tiles. In a preferred incorporation of slab mat, the mat includes from about 176.8 to about 7,074 cm ³ / m ² (from about 5 to 200 OSY) of extruded adhesive liner. More preferably the plate mat includes from about 1061 to about 2,830 cm ³ / m ² (from about 30 to 80 OSY) of extruded fabric, more preferably 1,768 cm ³ / m ² (50 OSY). Preferably, the carpet plate mat receives its extruded liner in two passes, that is, to apply two layers of the extruded liner. The application of the extruded liner in two passes allows the opportunity to apply a first and a second layer that have different physical and / or chemical properties. As noted above, it is sometimes preferable to apply a polymer with a higher melt index adjacent to the main liner, and a polymer with a lower melt index in the layer following the main liner and an extrudate with a higher load content.
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37/51 elevated in the layer below that. In a preferred embodiment, the layer following the main liner includes a loading amount of 30 weight percent and the layer below that includes a loading amount of 60 weight percent. It is believed that the lower load content provides better penetration of the main lining and back seams in the carpet by the extrudate.
[0079] The carpet board may include a secondary lining cloth below the second layer of extruded lining. Materials suitable for the secondary lining cloth include those described above. However, it is currently not preferred to include a secondary lining cloth on the carpet board. Typically, the carpet plate is manufactured by producing a length of lined carpet and then cutting the carpet into squares of appropriate sizes. In the United States, the most common size is 45.7 cm2 (18 inches ² ). In the rest of the world the most common size is 50 cm ² .
[0080] Carpet tiles have a tendency to grow in hot and humid environments. This is a significant problem when the boards are installed edge to edge with no room for expansion. Warping of the plate system can occur even if the expansions are as low as 0.08%. The amount of growth in plaques is related to the inherent growth of the various layers of the plaque. The threads are often made of nylon which is known to swell when exposed to humid environments. This swelling is often retained by the pre-coating which can hold the pre-coated carpet composite in place at most of all temperatures observed in the application. However, they can
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38/51 consequences will arise if the layers of lining or adhesive or covering coating expand due to exposure to heat. For this reason, layers of non-woven fiberglass, which are seated between the adhesive layer and the covering coating, are often added. However, despite such efforts, the plates are known to grow due to the inherent growth of that polymer. The coefficient of linear thermal expansion (CLTE or CTE) is a measure of this growth trend.
[0081] CLTE is only part of the prediction of the growth of layers of polymeric linings on carpet tiles. This is because the classic CLTE measurement is done with little or no force applied to the sample. Particularly with soft materials such as those used to line carpets, even small forces applied to the sample by test devices such as dilatometers and TMA devices can alter the measured growth. Growth can occur in the X (transverse) direction, in the Y (machine) direction or in the Z (thickness) direction. In the case of the carpet plate present, the directional growth X and Y is limited by the pre-coated carpet, the layer of glass laid down and the floor to which it adheres. These restrictions tend to force the thermal expansion of the adhesive coating and the covering coating in the Z direction, which is the “minimum resistance path. The degree to which this runs is related to the amount of force with which a material grows, hereinafter called “growth stress. Such soft materials with a high growth stress will expand more in the X and Y directions than materials with low growth stress.
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39/51
Growth stress measurement [0082] Growth stress is measured using an RSA III from TA Instruments (Rheometric Solid Analyzer III). Compression-molded sheets of each 0.8-1 mm thick sample are cut into a 12.7 mm wide rectangular shape and loaded onto the instrument. During the test, the deformation and tension are adjusted in order to fix the fastener distance at 20 mm. A temperature rise ramp is programmed to operate from room temperature to melting at 20 ° C / min. The force is recorded during the temperature rise ramp, from which the growth tension is calculated according to equation 1.
_{σ (M} Pa) = ^F = F (gO * 0-0098 (N / gf)
Area t (mm) * W (mm) (D where σ is the growth stress, F is the growth force, Area is the cross-sectional area of the film, t is the film thickness, and W is the width The growth stress value at 40 ° C is used for comparison between different samples This procedure is performed three times and the average growth stress for each sample is recorded.
Residual stress measurement [0083] Residual stress properties are measured using a small drawbar according to the sample geometry of ASTM D 1708 using Instron. The sample is stretched to 100% / mi to 25% and maintained at 25% for 30 min, during which the tension is recorded over time. The test is carried out in an environmental chamber, which is adjusted to 40 ° C, to represent an extreme temperature in an experience of installation force.
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40/51
The percentage of residual stress after 30 min is used for comparison between different samples. This procedure is performed twice and the average residual stress is recorded for each sample.
Table 1: Growth stress at 40 ° C
psi Comparative Example 1 15 Example 1 5 Example 1 (repeated) 10
[0084] Comparative Example 1 is a formulation comprising 24 weight percent of a substantially linear ethylene / 1-octene copolymer having a melt index of about 30 g / 10 minutes and a density of about 0.885 g / cm ³ ; about 4 weight percent AMPLIFY GR 204, which is an ethylene polymer having a melt index of 65 g / 10 minutes and a density of about 0.952 g / cm ³ subsequently grafted with about 1 maleic anhydride, 2 weight percent maleic anhydride and a final melt index of about 12 g / 10 minutes; about 60 weight percent of cargo; about 1 weight percent oil (Chevron / Phillips Paralux 6001); and about 11 weight percent stickiness agent (see top example of column 59 of US 7,338,698). This formulation of Comparative Example 1 has a storage module (G ') of about 7.8 MPa at 70 ° C. G 'is obtained from dynamic mechanical spectroscopy data of compression molded composite films. G 'is measured using ARES dynamic-mechanical analyzer from Rheometrics torsion mode. The test is performed from a temperature below Tg to 200 ° C at a frequency of 10 rad / s. The G 'value is recorded at 70 ° C.
[0085] Example 1 is a formulation comprising 24 per
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41/51 weight percent of a copolymer in ethylene / 1octene multiblocks having a melt index of about 15 g / 10 minutes, a density of about 0.877 g / cm3, about 25% of hard segments, about 75% of soft segments and a block index of about 0.4 to about 0.6; about 4 weight percent AMPLIFY GR 204, which is an ethylene polymer having a melting index of 65 g / 10 minutes and a density of about 0.952 g / cm3 subsequently grafted with maleic anhydride of about 1.2 weight percent maleic anhydride and a final melt index of about 12 g / 10 minutes; about 60 weight percent coal ash; about 1 weight percent oil (Chevron / Phillips Paralux 6001); and about 11 weight percent of the tacking agent EASTOTAC H115R.
[0086] Other properties of the copolymer in ethylene / 1-octene multiblocks include those listed below:
I10 I10 / I2 Tm Tc Mn Mw Mw / Mn Heat of fusion g / 10 min° C ° C g / mol g / molJ / g 113 7, 6 120 104 11760 63850 5, 4 50, 4
Crystallinity 1—1 co d ° £-P Soft segment ofC8 C8 hard segment % of soft segments % of hard segments % by weight molar% molar% molar% 00 0% 17.4 13, 1 18, 5 0, 9 75 25
Table 2: Percentage of residual stress in deformation of 25%
ο% Comparative Example 1 67 Example 1 54
[0087] Comparative Example 1 is the same formulation described above.
[0088] Example 1 is the same formulation described above.
[0089] Combinations of low growth stresses and low residual stresses can be achieved using
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42/51 low modules. These low modules can be carried out by plasticizing as in the case with PVC or using very low crystallinity materials such as ethylene copolymers with high levels of copolymer. However, these very low crystallinity materials typically melt at low temperatures. For carpet and carpet tile applications, loading temperatures can reach as high as 80 ° C. Therefore, the melting points of lining materials must be kept in this range or higher.
[0090] For polymers with lower melting points, curing or crosslinking can be used to increase the molecular weight to prevent polymer flow at high temperatures, preferably without significantly affecting the growth stress and residual stress character. This can be done with peroxide crosslinking, electronic beam and other similar methods.
[0091] In yet another alternative incorporation, a pressure sensitive adhesive is applied to the bottom surface of the lined carpet and a release sheet is included. In this way, a “self-adhesive film mat” is produced. This is particularly advantageous when the carpet will be cut into sheets. Examples of suitable pressure-sensitive adhesives include ethylene / vinyl acetate copolymers and substantially linear ethylene polymers and polymers in ethylene-based multiblocks formulated with tackiness agents and polymeric waxes. The release sheet can be made with conventional polymers and / or paper products. Preferably, the release sheet is made of a polyester / wax formulation. it was determined that the pressure sensitive adhesive is better
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43/51 applied directly to the adhesive liner material while the adhesive liner material is still at an elevated temperature from the extrusion coating process. A preferred technique is to extrude the pressure sensitive adhesive by extruding the adhesive liner material; that is, apply the pressure sensitive adhesive to the slide. Alternatively, the adhesive liner material can be reheated before applying the pressure sensitive adhesive.
[0092] OBC is very compatible with fully hydrogenated tackifiers with molecular weights less than 2500 g / mol (Mz). The best tackiness agents for use with OBC are: (1) hydrogenated aromatics such as REGALITE R1090 and R1100 (produced by Eastman Chemical); (2) fully hydrogenated hydrocarbons such as EASTOTAC H100L and ESCOREZ 5600 series; (3) partially hydrogenated hydrocarbons such as ESCOREZ 5400 series; and (4) hydrogenated pure monomer resins such as REGALREZ 1085 and 1094.
[0093] Appropriate oil: A selection of mineral and naphthenic oils was formulated with the tacking agent OBC. The best candidates include PARALUX 6001 (paraffinic) from Chevron-Phillips, HYPRENE P100N (hydrogenated paraffinic) from West Virginia, KAYDOL mineral oils from Crompton-Witco and HYDROBRITE 550 from Sonneborn (62-67.5% paraffinic).
[0094] Appropriate waxes: Waxes, including waxes manufactured from refining crude oil, such as paraffin wax, microcrystalline wax, and synthetic waxes, such as Fischer-Tropsch waxes.
Appropriate fillers [0095] Glass filler: Powder glass is typically produced by recycling post-consumer glass products, in particular
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44/51 automotive and architectural glass, also known as slab glass. However, other types of glass can also be used, such as crystal (lead glass), E glass, boron silicate glass, brown glass (bottle glass), and green glass (bottle glass) and combinations thereof, to form the glass powder. Therefore, to ensure adequate dispersion of the glass powder in the load while still maintaining adequate viscosities, the average size of the glass powder can vary from approximately 100 mesh to 400 mesh. More particularly, in some embodiments, the average size of the glass powder can be approximately 200 mesh.
[0096] Other charges: The glass powder can constitute up to 100% of the charge. Additionally, glass powder can be used together with conventional fillers to form a composite filler. For example, in some embodiments, the glass powder can be mixed with carbonates such as calcium carbonate (CaCO3), cesium carbonate (Cs ₂ CO3), strontium carbonate (SrCO3), and magnesium carbonate (MgCO3); sulfates such as barium sulfate (BaSO4); oxides such as dust and ash, iron oxide (Fe2O3), aluminum oxide (Al2O3), tungsten oxide (W2O3), titanium oxide (Ti2O3), and silicon oxide (Si2O3); silicates, such as clay; metallic salts; dust and ash; and the like.
[0097] Surfactants: The adhesive compound may also include additional additives. For example, these additives can include a surfactant to help keep the charge evenly dispersed in the adhesive. Suitable surfactants include nonionic, anionic and fluorine surfactants. In addition to uniformly dispersing the charge throughout the adhesive compound, surfactants can also be used as a
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45/51 foaming aid to increase adhesive emulsification.
[0098] Antioxidants: When polymeric adhesives are heated, especially hotmelt adhesives, they can become susceptible to degradation by thermo-oxidation. Therefore, to reduce the possibility of degradation by thermo-oxidation, the adhesive composition of the present invention can also contain an antioxidant such as IRGANOX 1010, 1092, etc.
Tracks suitable for PSA and HMA compositions:
[0099] Load: 40-70%; Stickiness resin: 20-40%; Oil: 10%; OBC: balance to reach 100%.
[0100] Waxes useful in embodiments of the present invention include Fischer-Propsch waxes, petroleum-derived waxes, and synthetic waxes. These waxes are commercially obtainable, for example, from Sasol Company. Major oil companies such as Shell Oil, ExxonMobil, and other oil refiners provide oil waxes for use in this application. Mountain waxes (lignite waxes) form another type of suitable waxes. Most of these waxes are obtained in the lubricating oil refining process, where the waxes are separated from the lubricating oil stock and refined into various wax fractions including paraffins and microcrystalline waxes. Formulators such as Astor Wax, IGI, and Moore & Munger also provide waxes suitable for these applications. These waxes are resold as they are from the oil companies and / or are formulated and repackaged to meet the specific needs of consumers.
[0101] In addition to synthetic waxes and / or derived from
Petition 870190031104, dated 04/01/2019, p. 50/61
46/51 petroleum, a number of other natural waxes can be used, such as carnauba waxes, and higher triglyceride waxes commercially obtainable from processing commodities containing natural oil such as soybeans, coconut and other crops from which they can get oils.
[0102] Appropriate waxes can be obtained from Archer Daniels, Midland (DECATUR I11) designated by product number 86-197-0; Cargill Incorporated (WAYZATA, Mn) designated by its product number 800mrcs0000u; and other
sources under O name generic of oil Soy hydrogenated. Coconut oil can be obtained from Custom Shortenings & Oils (Richmond, Go) and is designated as Master Chief Stable Flake- P. Wax in Soy It is also distributed per Marcus Oil &
Chemical Corp. (Houston, Texas) under the name of Marcus Nat 155. These waxes can also be used as food additives. In incorporations involving PSAs, the waxes listed above can be replaced by oils (which can be made up similarly).
[0103] Stickiness resins useful in the present invention include aliphatic, cycloaliphatic, and aromatic and modified hydrocarbons and hydrogenated versions; terpenes and modified terpenes and hydrogenated versions; and resins and resin derivatives and hydrogenated versions; and mixtures thereof. These tackiness resins have a ball and ring softening point of 70 ° C to 150 ° C and will typically have a viscosity at 177 ° C (350 ° F), measured using a Brookfield viscometer, of no more than 200 centipoise . They are also obtainable with different levels of hydrogenation, or unsaturation, which is
Petition 870190031104, dated 04/01/2019, p. 51/61
47/51 another commonly used term.
[0104] Useful examples include EASTTOTAC ™ H-100, H-115 and H130 from Eastman Chemical Company (Kingsport, TN), especially when incorporated at levels of up to about 15 weight percent of the total composition, which are resins of petroleum hydrocarbons, partially hydrogenated cycloaliphatics with softening points of 110 ° C, 115 ° C, and 130 ° C, respectively. These are obtainable in grade E, grade R, grade L and grade W, indicating different levels of hydrogenation with E without the least hydrogenated and W being the most hydrogenated. Grade E has a bromine index of 15, grade R has a bromine index of 5, grade L has a bromine index of 3, and grade W has a bromine index of 1. EASTOTAC ™ H-142R from Eastman Chemical
Company has a softening point of about 140 ° C. Other useful tackiness resins include ESCOREZ ™ 5300, 5400, and 5637, petroleum hydrocarbon resins, partially hydrogenated cycloaliphatics; and ESCOREZ ™ 5600, a partially hydrogenated aromatic petroleum hydrocarbon resin, which are obtainable from Exxon Chemical Company (Houston, Texas); and WINGTACK ™ Extra, which is an aromatic, aliphatic hydrocarbon resin obtainable from Goodyear Chemical Company (Akron, Ohio).
[0105] There are numerous types of resins and modified resins obtainable with different levels of hydrogenation including gum resins, wood resins, tallow resins, distilled resins, dimerized resins, and polymerized resins. Some specific modified resins include glycerol and pentaerythritol esters from wood resins and tallow resins. Degrees commercially obtainable
Petition 870190031104, dated 04/01/2019, p. 52/61
48/51 include, but are not limited to, SYLVATAC ™ 1103, a pentaerythritol resin ester obtainable from Union Camp (Wayne, NJ); PERMALYN ™ 305, an erythritol modified wood resin obtainable from Hercules, Inc. (Brunswick, GA) and FORAL 105, which is a very hydrogenated pentaerythritol ester ester also obtainable from Hercules, Inc. (Brunswick, GA). SYLVATAC ™ R-85 and 295 are melting point resin acids of 85 ° C and 95 ° C, obtainable from Arizona Chemical Company and FORAL AX is a hydrogenated resin acid of melting point of 70 ° C obtained from Hercules , Inc. NIREZ V-2040 is a phenolic modified terpene resin obtainable from Arizona Chemical Company.
[0106] Another exemplary tackifier, PICCOTAC ™ 115, obtainable from Eastman Chemical Company, has a viscosity at 177 ° C (350 ° F) of about 1600 centipoise. Other typical tacking agents have viscosities at 177 ° C (350 ° F) much less than 1600 centipoise, for example, from 50 to 300 centipoise.
[0107] Exemplary aliphatic resins include those obtainable under the trade names EASTOTAC ™, ESCOREZ ™, PICCOTAC ™, MERCURES ™, WINGTACK ™, HI-REZ ™, QUINTONE ™, TACKIROL ™, etc. Exemplary polyiterpene resins include those obtainable under the trade names NIREZ ™, PICCOLYTE ™, WINGTACK ™, ZONAREZ ™, etc. Exemplary hydrogenated resins include those obtainable under the trade names ESCOREZ ™, ARKON ™, CLEARON ™, etc. These tackifiers can be used with the polymers of the present invention, as long as they are used at compatible levels.
[0108] In certain applications of the present invention,
Petition 870190031104, dated 04/01/2019, p. 53/61
49/51 it is envisaged that an adhesive can be prepared without the use of a tackifier or with a minimal amount of tackifier. An adhesive can also be prepared without a wax, such as a mixture of a polymer and a sticky resin.
[0109] The tacking agents added to the adhesives can be characterized by parameters such as their softening points, relative densities, or by acid number. A tackifier can be selected from a variety of tackifiers, as described above but not limited to them, and tackifier agents characterized by a range of acidity indices, such as acidity indices between 0 and 100, plus preferably an acid number between 0 and 25.8, and most preferably a tackifier having an acid number between 3 and 10.
[0110] In embodiments of the present invention, the polymer and / or wax, tackiness resin, oil, and dispersant typically comprise from about 1 to about 74 volume percent of the total dispersion. Therefore, water typically comprises between about 26 and 99 percent by volume. However, various percentages of dispersants, additives, biocides, and other compounds explained below may also be present. All intermediate bands, for example, 5 to 50 volume percent polymer / wax / tackiness resin / oil are included in the present disclosure. Specific ranges include 50 to 60 percent polymer and / or wax, tackiness resin, oil and dispersant, from the total dispersion.
[0111] The adhesives of the present invention may contain
Petition 870190031104, dated 04/01/2019, p. 54/61
50/51 also a number of additional components, such as stabilizer, plasticizer, pigment, filler, or antioxidant. Among the applicable stabilizers or antioxidants that can be included in the adhesive composition of the present invention are multifunctional phenols and high molecular weight hindered phenols, such as sulfur-containing and phosphorus-containing phenols. Impeded phenols, known to those skilled in the art, can be described as phenolic compounds, which also contain sterically bulky radicals very close to the phenolic hydroxyl group. Specifically, terciobutyl groups are generally substituted on the benzene ring in at least one of the ortho positions relative to the phenolic hydroxyl group. The presence of these sterically substituted radicals bulky neighbors of the hydroxyl group serves to delay its stretching frequency, and correspondingly, its reactivity. It is this impediment that provides the stabilizing properties of these phenolic compounds.
[0112] Representative hindered phenols include, but are not limited to, 2,4,6-trialkylated monohydroxy phenols;
1.3.5- trimethyl-2,4,6-tris- (3,5-ditherciobutyl-4-hydroxy benzyl) -benzene, tetrakis-3 (3,5-ditherciobutyl-4-hydroxy phenyl) -pentaerythritol propionate, obtainable commercially under the trade name IRGANOX® 1010; N-octadecyl (3,5ditditiobutyl-4-hydroxy phenyl) -propionate; 4,4'-methylene-bis (4-methyl-6-terciobutyl-phenol); 4,4'-thiobis (6-terciobutyl-o-cresol); 2,6-ditherciobutyl phenol; 6- (4-hydroxy phenoxy) -2,4-bis (n-octylthio) -1,3,5-triazine; 2- (n-octyl thio) ethyl 3,5diterciobutyl-4-hydroxy-benzoate;
3.5- di-n ditherciobutyl-4-hydroxybenzyl phosphonate
Petition 870190031104, dated 04/01/2019, p. 55/61
51/51 octadecyl; and sorbitol hexa (3,3,5-ditherciobutyl-4-hydroxyphenyl) propionate. Antioxidants include, but are not limited to, butylated hydroxy anisol (BHA) or butylated hydroxy toluene (BHT) which can also be used to make the formulation thermally more stable. These stabilizers and antioxidants can be added in amounts ranging from approximately 0.01% to approximately 5% by weight of the formulation. Other additives known in the adhesive industry can also be used in conjunction with embodiments of the present invention. The scope of the present invention is not intended to be limited by any formulation presented above or below, but is instead governed by the claims. Other typical additives may include, but are not limited to, nucleating agents, chemicals used to delay crystallization, thickeners, rheology modifiers, oils and other additives.

权利要求:
Claims (14)
[1]
1. Carpet or plate rug, characterized by the fact that it comprises a main lining material having a face and a back, a plurality of fibers connected to the main lining material extending from the face of the main lining material and exposed on the back of the main lining material, an optional pre-coating, an adhesive lining material, an optional dimensional stability layer, an optional covering lining material, and an optional secondary lining material adjacent to the dimensional stability layer or lining material adhesive, with at least one of the plurality of fibers, the main lining material, the optional pre-coating layer, the adhesive lining material, the optional dimensional stability layer, or the optional secondary lining material comprises at least a non-polyvinyl and non-chlorinated thermoplastic polymer or composition having an internal growth stress at 40 ° C less than 0.17 MPa (25 psi) and a residual strain in 25% less than 63%, with at least one non-polyvinyl and non-chlorinated thermoplastic polymer or composition being an olefinic block copolymer (OBC); and the covering lining material or adhesive lining material further comprising 24% by weight of the CBO, (a) at least one charge in an amount of 60% by weight, based on the total weight of the material, the cargo is selected from the group consisting of dust and coal ash, ATH, CaCO3, talc, recycled glass, hydroxide
Petition 870190099835, of 10/04/2019, p. 7/13
[2]
2/4 magnesium, ground tires, and ground carpet;
(b) 4% by weight of at least one high density polyethylene grafted with maleic anhydride (MAH-g-HDPE);
(c) 1% by weight of at least one oil;
(d) optionally, a color additive; and (e) 11% by weight of at least one tackifier.
2. Carpet or plate mat according to claim 1, characterized in that the at least one non-chlorinated and non-chlorinated butyral thermoplastic polymer or polymer has an internal growth stress at 40 ° C, less than 0.14 MPa (20 psi).
[3]
3. Carpet or plate rug according to claim 1, characterized in that the at least one non-chlorinated and non-chlorinated butyral thermoplastic polymer or polymer has a residual deformation stress of 25% less than 60%.
[4]
4. Carpet or carpet in plates according to claim 1, characterized in that the at least one non-chlorinated and non-chlorinated butyral thermoplastic polymer or polymer has an internal growth tension at 40 ° C, less than or equal to 0 .7 MPa (10 psi).
[5]
5. Carpet or plate rug according to claim 1, characterized in that the at least one non-chlorinated and non-chlorinated butyral thermoplastic polymer or polymer has a residual deformation stress of 25% less than 55%.
[6]
6. Carpet or plate mat according to claim 1, characterized in that the at least one non-chlorinated and non-chlorinated butyral thermoplastic polymer or polymer has a storage module (G ') greater than 4.3 MPa
Petition 870190099835, of 10/04/2019, p. 8/13
3/4 to 70 ° C.
[7]
7. Carpet or slab mat according to claim 1, characterized in that the olefinic block copolymer comprises a block ethylene interpolymer distinguished by having an average block index greater than zero and up to 1.0 and a molecular weight distribution, Mw / Mn, greater than 1.3.
[8]
8. Carpet or carpet tiles, according to claim 1, characterized in that the pre-coating is not optional.
[9]
9. Carpet according to claim 1, characterized in that (I) the fibers, main lining, adhesive lining and optional secondary lining all comprise a multi-block polyolefin polymer, (II) the olefinic monomer chemistry of the adhesive lining differs that of the fibers and the main lining, and (III) the carpet includes a label or literature at the time of sale that indicates that the carpet is recyclable without discrimination of carpet components.
[10]
10. Carpet or slab mat according to claim 1, characterized in that the olefinic block copolymer has an M _w / M _n of 5.4.
[11]
11. Carpet or plate mat according to claim 1, characterized in that the olefinic block copolymer comprises 25% of hard segments and 75% of soft segments.
[12]
12. Carpet or plate mat according to claim 1, characterized in that the olefinic block copolymer has a block index of 0.4 to 0.6.
[13]
13. Carpet or carpet tiles, according to claim 1, characterized by the fact that MAH-g-HDPE comprises 1.2%
Petition 870190099835, of 10/04/2019, p. 9/13
4/4 by weight of maleic anhydride.
[14]
14. Carpet or carpet tiles, according to the claim
1, characterized by the fact that MAH-g-HDPE has a final melting index of 12 g / 10 minutes.

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EP3908691A1|2019-01-09|2021-11-17|Interface, Inc.|Surface coverings including carbon sequestering materials and methods of making|

法律状态:
2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|

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2019-01-29| B06T| Formal requirements before examination|

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2019-07-09| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|

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2019-11-05| B09A| Decision: intention to grant|

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2020-01-14| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 07/07/2010, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US12/499,667|US9885149B2|2009-07-08|2009-07-08|Carpet and carpet backing|

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PCT/US2010/041167|WO2011005828A1|2009-07-08|2010-07-07|Carpet and carpet backing|

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