US20180162109A1 - Roofing membranes, compositions, and methods of making the same - Google Patents

Roofing membranes, compositions, and methods of making the same Download PDF

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Publication number
US20180162109A1
US20180162109A1 US15/836,417 US201715836417A US2018162109A1 US 20180162109 A1 US20180162109 A1 US 20180162109A1 US 201715836417 A US201715836417 A US 201715836417A US 2018162109 A1 US2018162109 A1 US 2018162109A1
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United States
Prior art keywords
silane
roofing membrane
polyolefin
polyolefin elastomer
aspects
Prior art date
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Abandoned
Application number
US15/836,417
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English (en)
Inventor
Krishnamachari Gopalan
Robert J. Lenhart
Gending Ji
Roland Herd-Smith
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cooper Standard Automotive Inc
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Cooper Standard Automotive Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Priority to US15/836,417 priority Critical patent/US20180162109A1/en
Assigned to COOPER-STANDARD AUTOMOTIVE INC. reassignment COOPER-STANDARD AUTOMOTIVE INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOPALAN, KRISHNAMACHARI, HERD-SMITH, Roland, JI, Gending, LENHART, ROBERT J.
Application filed by Cooper Standard Automotive Inc filed Critical Cooper Standard Automotive Inc
Publication of US20180162109A1 publication Critical patent/US20180162109A1/en
Priority to US16/144,719 priority patent/US11684115B2/en
Priority to US16/213,600 priority patent/US20190105883A1/en
Assigned to DEUTSCHE BANK AG NEW YORK BRANCH reassignment DEUTSCHE BANK AG NEW YORK BRANCH SECURITY AGREEMENT Assignors: COOPER-STANDARD AUTOMOTIVE INC.
Assigned to U.S. BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT reassignment U.S. BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT PATENT SECURITY AGREEMENT Assignors: COOPER-STANDARD AUTOMOTIVE INC.
Assigned to BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT reassignment BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT PATENT SECURITY AGREEMENT Assignors: COOPER-STANDARD AUTOMOTIVE INC.
Priority to US17/202,625 priority patent/US20210198465A1/en
Assigned to COOPER-STANDARD AUTOMOTIVE INC reassignment COOPER-STANDARD AUTOMOTIVE INC TERMINATION AND RELEASE OF SECURITY INTEREST PREVIOUSLY RECORDED AT REEL/FRAME (052788/0392) Assignors: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION (SUCCESSOR IN INTEREST TO U.S. BANK NATIONAL ASSOCIATION), AS COLLATERAL AGENT
Assigned to COOPER-STANDARD AUTOMOTIVE INC. reassignment COOPER-STANDARD AUTOMOTIVE INC. TERMINATION AND RELEASE OF SECURITY INTEREST PREVIOUSLY RECORDED AT REEL/FRAME (052788/0158) Assignors: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
Assigned to U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT reassignment U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT PATENT SECURITY AGREEMENT (1ST LIEN) Assignors: COOPER-STANDARD AUTOMOTIVE INC., COOPER-STANDARD INDUSTRIAL AND SPECIALTY GROUP, LLC
Assigned to U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT reassignment U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT PATENT SECURITY AGREEMENT (3RD LIEN) Assignors: COOPER-STANDARD AUTOMOTIVE INC., COOPER-STANDARD INDUSTRIAL AND SPECIALTY GROUP, LLC
Abandoned legal-status Critical Current

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    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
    • A43B13/00—Soles; Sole-and-heel integral units
    • A43B13/02—Soles; Sole-and-heel integral units characterised by the material
    • A43B13/04—Plastics, rubber or vulcanised fibre
    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
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    • A43B13/14—Soles; Sole-and-heel integral units characterised by the constructive form
    • A43B13/18—Resilient soles
    • A43B13/187—Resiliency achieved by the features of the material, e.g. foam, non liquid materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00—Crosslinking
    • C08L2312/08—Crosslinking by silane
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09K2200/0617—Polyalkenes

Definitions

  • the present disclosure generally relates to compositions that may be used to form thermoplastic roofing membranes, and more particularly, to silane-grafted polyolefin elastomer compositions used to form thermoplastic roofing membranes and methods for manufacturing these compositions and roofing membranes.
  • Thermoplastic roofing membranes may be a single layer or may be composed of multiple layers and may contain a reinforcing fabric or scrim reinforcement material in the center between any two of the layers of the roofing membrane.
  • Each of the respective layers in the roofing membrane needs to demonstrate a variety of different material properties in order to be suited for use on a roof where the material will be exposed to the sun and the elements.
  • the material properties of the polymer layers should exhibit good adhesion, UV resistance, weatherability (durability), flame retardance, flexibility, chemical resistance and longevity.
  • roofing membranes should preferably be capable of forming hot-air welded seams.
  • TPO thermoplastic polyolefin
  • EPDM ethylene propylene diene monomer
  • PVC polyvinyl chloride
  • TPO membranes are widely available, affordable, and typically white, but are susceptible to deterioration when exposed to high heat and/or solar UV radiation.
  • EPDM membranes are made from the readily available EPDM synthetic rubber, but roughly 95% of all EPDM roofing membranes produced are black while federal and state building regulators are starting to push for white roofing membranes.
  • PVC membranes are widely available and offer excellent puncture, heat-weldability, colorability, and heat resistant qualities, but these membranes can be expensive to manufacture and suffer from variability in properties as produced by different manufacturers.
  • a roofing membrane is disclosed.
  • the single ply roofing membrane includes a top layer comprising a flame retardant and first silane-crosslinked polyolefin elastomer having a density less than 0.90 g/cm 3 ; a scrim layer; and a bottom layer comprising a flame retardant and a second silane-crosslinked polyolefin elastomer having a density less than 0.90 g/cm 3 .
  • the top and bottom layers of the roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according to ASTM D 395 (22 hrs @ 70° C.).
  • a method of making a roofing membrane includes: extruding a first silane-crosslinkable polyolefin elastomer to form a top layer; extruding a second silane-crosslinkable polyolefin elastomer to form a bottom layer; calendaring a scrim layer between the top and the bottom layers to form an uncured roofing membrane element; and crosslinking the silane-crosslinkable polyolefin elastomers of the top and the bottom layers in the uncured roofing membrane element at a curing temperature and a curing humidity to form the roofing membrane.
  • the top and bottom layers of the roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according to ASTM D 395 (22 hrs @ 70° C.).
  • a method of making a high-load flame retardant thermoplastic polyolefin (TPO) roofing membrane includes: adding a silane-grafted polyolefin elastomer, a fire retardant, and a condensation catalyst to a reactive single screw extruder to produce a silane-crosslinkable polyolefin elastomer; calendaring the silane-crosslinkable polyolefin elastomer to form a top layer and a bottom layer; calendaring a scrim layer between the top and the bottom layers to form an uncured roofing membrane element; and crosslinking the silane-crosslinkable polyolefin elastomers of the top and the bottom layers in the uncured roofing membrane element at an ambient temperature and an ambient humidity to form the thermoplastic polyolefin (TPO) roofing membrane.
  • the top and bottom layers of the thermoplastic polyolefin (TPO) roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%,
  • FIG. 1 is a cross-sectional view of a roofing membrane according to some aspects of the present disclosure
  • FIG. 2 is a schematic reaction pathway used to produce a silane-crosslinked polyolefin elastomer according to some aspects of the present disclosure
  • FIG. 3 is a flow diagram of a method for making a single ply roofing membrane with a silane-crosslinked polyolefin elastomer using a two-step Sioplas approach according to some aspects of the present disclosure
  • FIG. 4A is a schematic cross-sectional view of a reactive twin-screw extruder according to some aspects of the present disclosure
  • FIG. 4B is a schematic cross-sectional view of a single-screw extruder according to some aspects of the present disclosure
  • FIG. 5 is a flow diagram of a method for making a single ply roofing membrane with a silane-crosslinked polyolefin elastomer using a one-step Monosil approach according to some aspects of the present disclosure
  • FIG. 6 is a schematic cross-sectional view of a reactive single-screw extruder according to some aspects of the present disclosure
  • FIG. 7 is a graph illustrating the stress/strain behavior of a silane-crosslinked polyolefin elastomer, according to aspects of the disclosure, as compared to conventional EPDM compounds;
  • FIG. 8 is a relaxation plot of an exemplary silane-crosslinked polyolefin elastomer, suitable for a roofing membrane according to aspects of the disclosure, and comparative EPDM cross-linked materials;
  • FIG. 9 is a compression set plot of an exemplary silane-crosslinked polyolefin elastomer suitable for a roofing membrane, and a comparative EPDM cross-linked material.
  • the terms “upper,” “lower,” “right,” “left,” “rear,” “front,” “vertical,” “horizontal,” and derivatives thereof shall relate to the roofing membranes of the disclosure as shown in FIG. 1 .
  • the device may assume various alternative orientations and step sequences, except where expressly specified to the contrary.
  • the specific devices and processes illustrated in the attached drawings, and described in the following specification are simply exemplary embodiments of the inventive concepts defined in the appended claims. Hence, specific dimensions and other physical characteristics relating to the embodiments disclosed herein are not to be considered as limiting, unless the claims expressly state otherwise.
  • a value modified by a term or terms, such as “about” and “substantially,” may not be limited to the precise value specified.
  • the approximating language may correspond to the precision of an instrument for measuring the value.
  • the modifier “about” should also be considered as disclosing the range defined by the absolute values of the two endpoints. For example, the expression “from about 2 to about 4” also discloses the range “from 2 to 4.”
  • the term “and/or,” when used in a list of two or more items, means that any one of the listed items can be employed by itself, or any combination of two or more of the listed items can be employed.
  • the composition can contain A alone; B alone; C alone; A and B in combination; A and C in combination; B and C in combination; or A, B, and C in combination.
  • a roofing membrane 10 is disclosed.
  • the roofing membrane 10 includes a top layer 14 having a flame retardant and a first silane-crosslinked polyolefin elastomer with a density less than 0.90 g/cm 3 ; a scrim layer 26 ; and a bottom layer 38 having a flame retardant and a second silane-crosslinked polyolefin elastomer with a density less than 0.90 g/cm 3 .
  • the top and bottom layers of the roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according to ASTM D 395 (22 hrs @ 70° C.).
  • a TPO roofing membrane must exhibit at least the following mechanical properties as outlined by the ASTM specification for TPO roofing membranes: 1) a tensile strength (CD and MD) greater than 10 MPa; 2) an elongation at break (CD and MD) greater than 500%; 3) an elastic modulus (CD and MD) of less than 100 MPa; and 4) a flame retardance rating of classification D as measured in accordance with the EN ISO 11925-2 surface exposure test.
  • the single ply roofing membrane 10 includes the top layer 14 with a first and a second surface 18 , 22 .
  • the scrim layer 26 (also referred to as scrim 26 ) has a third and a fourth surface 30 , 34 where the third surface 30 of the scrim 26 is coupled to the second surface 22 of the top layer 14 .
  • the single ply roofing membrane 10 additionally includes a bottom layer 38 with a fifth and a sixth surface 42 , 46 , where the fifth surface 42 of the bottom layer 38 is coupled to the fourth surface 34 of the scrim 26 .
  • the roofing membrane 10 may include the single ply roofing membrane, a double ply roofing membrane, or a higher number of plies. Unless otherwise denoted, roofing membrane 10 and single ply roofing membrane 10 both mean a single ply made from the top layer 14 , scrim layer 26 , and bottom layer 38 .
  • the scrim layer 26 disposed between the top and bottom layers 14 , 38 can serve as a reinforcement in the roofing membrane, thus adding to its structural integrity.
  • Materials that can be used for the scrim layers 26 may include, for example, woven and/or non-woven fabrics, fiberglass, and/or polyester.
  • additional materials that can be used for the scrim layers 26 can include synthetic materials such as polyaramids, KEVLARTM, TWARONTM, polyamides, polyesters, RAYONTM, NOMEXTM, TECHNORATM, or a combination thereof.
  • the scrim layer 26 may include aramids, polyamides, and/or polyesters.
  • a tenacity of the scrim layer 26 may range from about 100 to about 3000 denier.
  • the scrim layers 26 may have a tenacity ranging from about 500 to about 1500 denier. In still other aspects, scrim layers 26 may have a tenacity of about 1000 denier. In some aspects, scrim layers 26 may have a tensile strength of greater than about 14 kN per meter (80 pounds force per inch). In other aspects, the scrim layers 26 may have a tensile strength of greater than about 10 kN per meter, greater than about 15 kN per meter, greater than about 20 kN per meter, or greater than about 25 kN per meter. Depending on the desired properties of the final single ply roofing membrane 10 , the scrim layers 26 may be varied as needed to suit particular roofing membrane designs. One of ordinary skill in the art would appreciate that such characteristics can be varied without departing from the present disclosure.
  • the single ply roofing membranes 10 disclosed herein may have a variety of different dimensions.
  • single ply roofing membranes 10 may have a length from about 30 feet to about 200 feet and a width from about 4 feet to about 12 feet.
  • the roofing membranes 10 may have a width of about 10 feet. Variations in the width may provide for various advantages. For example, in some aspects, roofing membranes 10 having smaller widths may advantageously allow for greater ease in assembly of a roofing structure. Smaller widths may also advantageously allow for greater ease in rolling or packaging of a manufactured membrane. Larger widths may advantageously allow for greater structure integrity, fast installation and/or improve the stability of a roofing structure comprising these membranes.
  • magnesium hydroxide may provide flame retardant properties in the layers 14 , 38 .
  • Magnesium hydroxide may be extruded or blended with the silane-grafted polyolefin elastomer to ensure complete dispersal in the composition blend.
  • the magnesium hydroxide is blended with the silane-grafted polyolefin elastomer in an amount up to 70 wt % magnesium hydroxide.
  • the magnesium hydroxide in the silane-grafted polyolefin elastomer can make up between about 20 wt % and 75 wt % of the roofing membrane composition.
  • the disclosure focuses on the composition, method of making the composition, methods of making roofing membranes with these compositions, and the corresponding material properties for the silane-crosslinked polyolefin elastomer used to make single ply roofing membranes 10 (as depicted in FIG. 1 ), along with other roofing membranes 10 consistent with the principles of this disclosure.
  • the roofing membrane 10 is formed from a silane-grafted polyolefin where the silane-grafted polyolefin may have a catalyst added to form a silane-crosslinkable polyolefin elastomer. This silane-crosslinkable polyolefin may then be crosslinked upon exposure to moisture and/or heat to form the final silane-crosslinked polyolefin elastomer or blend.
  • the silane-crosslinked polyolefin elastomer or blend includes the first polyolefin having a density less than 0.90 g/cm 3 , the second polyolefin having a crystallinity of less than 40%, the silane crosslinker, the graft initiator, and the condensation catalyst.
  • the first polyolefin can be a polyolefin elastomer including an olefin block copolymer, an ethylene/ ⁇ -olefin copolymer, a propylene/ ⁇ -olefin copolymer, EPDM, EPM, or a mixture of two or more of any of these materials.
  • Exemplary block copolymers include those sold under the trade names INFUSETM, an olefin block co-polymer (the Dow Chemical Company) and SEPTONTM V-SERIES, a styrene-ethylene-butylene-styrene block copolymer (Kuraray Co., LTD.).
  • Exemplary ethylene/ ⁇ -olefin copolymers include those sold under the trade names TAFMERTM (e.g., TAFMER DF710) (Mitsui Chemicals, Inc.), and ENGAGETM (e.g., ENGAGE 8150) (the Dow Chemical Company).
  • Exemplary propylene/ ⁇ -olefin copolymers include those sold under the trade name VISTAMAXXTM 6102 grades (Exxon Mobil Chemical Company), TAFMERTM XM (Mitsui Chemical Company), and VERSIFYTM (Dow Chemical Company).
  • the EPDM may have a diene content of from about 0.5 to about 10 wt %.
  • the EPM may have an ethylene content of 45 wt % to 75 wt %.
  • olefin comonomers refers to olefin comonomers which are suitable for being polymerized with olefin monomers, such as ethylene or propylene monomers.
  • Comonomers may comprise but are not limited to aliphatic C 2 -C 20 ⁇ -olefins. Examples of suitable aliphatic C 2 -C 20 ⁇ -olefins include ethylene, propylene, 1-butene, 4-methyl-1-pentene, 1-hexene, 1-octene, 1-decene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene and 1-eicosene.
  • the comonomer is vinyl acetate.
  • copolymer refers to a polymer, which is made by linking more than one type of monomer in the same polymer chain.
  • homopolymer refers to a polymer which is made by linking olefin monomers, in the absence of comonomers.
  • the amount of comonomer can, in some embodiments, be from greater than 0 wt %to about 12 wt % based on the weight of the polyolefin, including from greater than 0 wt % to about 9 wt %, and from greater than 0 wt % to about 7 wt %.
  • the comonomer content is greater than about 2 mol % of the final polymer, including greater than about 3 mol % and greater than about 6 mol %.
  • the comonomer content may be less than or equal to about 30 mol %.
  • a copolymer can be a random or block (heterophasic) copolymer.
  • the polyolefin is a random copolymer of propylene and ethylene.
  • the first polyolefin is selected from the group consisting of: an olefin homopolymer, a blend of homopolymers, a copolymer made using two or more olefins, a blend of copolymers each made using two or more olefins, and a combination of olefin homopolymers blended with copolymers made using two or more olefins.
  • the olefin may be selected from ethylene, propylene, 1-butene, 1-propene, 1-hexene, 1-octene, and other higher 1-olefin.
  • the first polyolefin may be synthesized using many different processes (e.g., using gas phase and solution based metallocene catalysis and Ziegler-Natta catalysis) and optionally using a catalyst suitable for polymerizing ethylene and/or ⁇ -olefins.
  • a metallocene catalyst may be used to produce low density ethylene/ ⁇ -olefin polymers.
  • the polyethylene used for the first polyolefin can be classified into several types including, but not limited to, LDPE (Low Density Polyethylene), LLDPE (Linear Low Density Polyethylene), and HDPE (High Density Polyethylene).
  • the polyethylene can be classified as Ultra High Molecular Weight (UHMW), High Molecular Weight (HMW), Medium Molecular Weight (MMW) and Low Molecular Weight (LMW).
  • the polyethylene may be an ultra-low density ethylene elastomer.
  • the first polyolefin may include a LDPE/silane copolymer or blend.
  • the first polyolefin may be polyethylene that can be produced using any catalyst known in the art including, but not limited to, chromium catalysts, Ziegler-Natta catalysts, metallocene catalysts or post-metallocene catalysts.
  • the first polyolefin may have a molecular weight distribution M w /M n of less than or equal to about 5, less than or equal to about 4, from about 1 to about 3.5, or from about 1 to about 3.
  • the first polyolefin may be present in an amount of from greater than 0 to about 100 wt % of the composition. In some embodiments, the amount of polyolefin elastomer is from about 30 wt % to about 70 wt %. In some aspects, the first polyolefin fed to an extruder can include from about 50 wt % to about 80 wt % of an ethylene/ ⁇ -olefin copolymer, including from about 60 wt % to about 75 wt %, and from about 62 wt % to about 72 wt %.
  • the first polyolefin may have a melt viscosity in the range of from about 2,000 cP to about 50,000 cP as measured using a Brookfield viscometer at a temperature of about 177° C. In some embodiments, the melt viscosity is from about 4,000 cP to about 40,000 cP, including from about 5,000 cP to about 30,000 cP and from about 6,000 cP to about 18,000 cP.
  • the first polyolefin may have a melt index (T2), measured at 190° C. under a 2.16 kg load, of from about 20.0 g/10 min to about 3,500 g/10 min, including from about 250 g/10 min to about 1,900 g/10 min and from about 300 g/10 min to about 1,500 g/10 min.
  • T2 melt index
  • the first polyolefin has a fractional melt index of from 0.5 g/10 min to about 3,500 g/10 min.
  • the density of the first polyolefin is less than 0.90 g/cm 3 , less than about 0.89 g/cm 3 , less than about 0.88 g/cm 3 , less than about 0.87 g/cm 3 , less than about 0.86 g/cm 3 , less than about 0.85 g/cm 3 , less than about 0.84 g/cm 3 , less than about 0.83 g/cm 3 , less than about 0.82 g/cm 3 , less than about 0.81 g/cm 3 , or less than about 0.80 g/cm 3 .
  • the density of the first polyolefin may be from about 0.85 g/cm 3 to about 0.89 g/cm 3 , from about 0.85 g/cm 3 to about 0.88 g/cm 3 , from about 0.84 g/cm 3 to about 0.88 g/cm 3 , or from about 0.83 g/cm 3 to about 0.87 g/cm 3 .
  • the density is at about 0.84 g/cm 3 , about 0.85 g/cm 3 , about 0.86 g/cm 3 , about 0.87 g/cm 3 , about 0.88 g/cm 3 , or about 0.89 g/cm 3 .
  • the percent crystallinity of the first polyolefin may be less than about 60%, less than about 50%, less than about 40%, less than about 35%, less than about 30%, less than about 25%, or less than about 20%.
  • the percent crystallinity may be at least about 10%. In some aspects, the crystallinity is in the range of from about 2% to about 60%.
  • the second polyolefin can be a polyolefin elastomer including an olefin block copolymer, an ethylene/ ⁇ -olefin copolymer, a propylene/ ⁇ -olefin copolymer, EPDM, EPM, or a mixture of two or more of any of these materials.
  • exemplary block copolymers include those sold under the trade names INFUSETM (the Dow Chemical Company) and SEPTONTM V-SERIES (Kuraray Co., LTD.).
  • Exemplary ethylene/ ⁇ -olefin copolymers include those sold under the trade names TAFMERTM (e.g., TAFMER DF710) (Mitsui Chemicals, Inc.) and ENGAGETM (e.g., ENGAGE 8150) (the Dow Chemical Company).
  • Exemplary propylene/ ⁇ -olefin copolymers include those sold under the trade name TAFMERTM XM grades (Mitsui Chemical Company) and VISTAMAXXTM (e.g., VISTAMAXX 6102) (Exxon Mobil Chemical Company).
  • the EPDM may have a diene content of from about 0.5 to about 10 wt %.
  • the EPM may have an ethylene content of 45 wt % to 75 wt %.
  • the second polyolefin is selected from the group consisting of: an olefin homopolymer, a blend of homopolymers, a copolymer made using two or more olefins, a blend of copolymers each made using two or more olefins, and a blend of olefin homopolymers with copolymers made using two or more olefins.
  • the olefin may be selected from ethylene, propylene, 1-butene, 1-propene, 1-hexene, 1-octene, and other higher 1-olefin.
  • the first polyolefin may be synthesized using many different processes (e.g., using gas phase and solution based metallocene catalysis and Ziegler-Natta catalysis) and optionally using a catalyst suitable for polymerizing ethylene and/or ⁇ -olefins.
  • a metallocene catalyst may be used to produce low density ethylene/ ⁇ -olefin polymers.
  • the second polyolefin may include a polypropylene homopolymer, a polypropylene copolymer, a polyethylene-co-propylene copolymer, or a mixture thereof.
  • Suitable polypropylenes include but are not limited to polypropylene obtained by homopolymerization of propylene or copolymerization of propylene and an ⁇ -olefin comonomer.
  • the second polyolefin may have a higher molecular weight and/or a higher density than the first polyolefin.
  • the second polyolefin may have a molecular weight distribution M w /M n of less than or equal to about 5, less than or equal to about 4, from about 1 to about 3.5, or from about 1 to about 3.
  • the second polyolefin may be present in an amount of from greater than 0 wt % to about 100 wt % of the composition. In some embodiments, the amount of polyolefin elastomer is from about 30 wt % to about 70 wt %. In some embodiments, the second polyolefin fed to the extruder can include from about 10 wt % to about 50 wt % polypropylene, from about 20 wt % to about 40 wt % polypropylene, or from about 25 wt % to about 35 wt % polypropylene. The polypropylene may be a homopolymer or a copolymer.
  • the second polyolefin may have a melt viscosity in the range of from about 2,000 cP to about 50,000 cP as measured using a Brookfield viscometer at a temperature of about 177° C.
  • the melt viscosity is from about 4,000 cP to about 40,000 cP, including from about 5,000 cP to about 30,000 cP and from about 6,000 cP to about 18,000 cP.
  • the second polyolefin may have a melt index (T2), measured at 190° C. under a 2.16 kg load, of from about 20.0 g/10 min to about 3,500 g/10 min, including from about 250 g/10 min to about 1,900 g/10 min and from about 300 g/10 min to about 1,500 g/10 min.
  • T2 melt index
  • the polyolefin has a fractional melt index of from 0.5 g/10 min to about 3,500 g/10 min.
  • the density of the second polyolefin is less than 0.90 g/cm 3 , less than about 0.89 g/cm 3 , less than about 0.88 g/cm 3 , less than about 0.87 g/cm 3 , less than about 0.86 g/cm 3 , less than about 0.85 g/cm 3 , less than about 0.84 g/cm 3 , less than about 0.83 g/cm 3 , less than about 0.82 g/cm 3 , less than about 0.81 g/cm 3 , or less than about 0.80 g/cm 3 .
  • the density of the first polyolefin may be from about 0.85 g/cm 3 to about 0.89 g/cm 3 , from about 0.85 g/cm 3 to about 0.88 g/cm 3 , from about 0.84 g/cm 3 to about 0.88 g/cm 3 , or from about 0.83 g/cm 3 to about 0.87 g/cm 3 .
  • the density is at about 0.84 g/cm 3 , about 0.85 g/cm 3 , about 0.86 g/cm 3 , about 0.87 g/cm 3 , about 0.88 g/cm 3 , or about 0.89 g/cm 3 .
  • the percent crystallinity of the second polyolefin may be less than about 60%, less than about 50%, less than about 40%, less than about 35%, less than about 30%, less than about 25%, or less than about 20%.
  • the percent crystallinity may be at least about 10%. In some aspects, the crystallinity is in the range of from about 2% to about 60%.
  • the silane-crosslinked polyolefin elastomers or blends e.g., as employed in roofing membranes 10 (e.g., within the top and bottom layers 14 , 38 as shown in FIG. 1 ), includes both the first polyolefin and the second polyolefin.
  • the second polyolefin is generally used to modify the hardness and/or processability of the first polyolefin having a density less than 0.90 g/cm 3 .
  • more than just the first and second polyolefins may be used to form the silane-crosslinked polyolefin elastomer or blend.
  • one, two, three, four, or more different polyolefins having a density less than 0.90 g/cm 3 , less than 0.89 g/cm 3 , less than 0.88 g/cm 3 , less than 0.87 g/cm 3 , less than 0.86 g/cm 3 , or less than 0.85 g/cm 3 may be substituted and/or used for the first polyolefin.
  • one, two, three, four, or more different polyolefins, polyethylene-co-propylene copolymers may be substituted and/or used for the second polyolefin.
  • the blend of the first polyolefin having a density less than 0.90 g/cm 3 and the second polyolefin having a crystallinity less than 40% is used because the subsequent silane grafting and crosslinking of these first and second polyolefin materials together are what form the core resin structure in the final silane-crosslinked polyolefin elastomer.
  • any polyolefins added to the blend having a crystallinity equal to or greater than 40% are not chemically or covalently incorporated into the crosslinked structure of the final silane-crosslinked polyolefin elastomer.
  • the first and second polyolefins may further include one or more TPVs and/or EPDM with or without silane graft moieties where the TPV and/or EPDM polymers are present in an amount of up to 20 wt % of the silane-crosslinker polyolefin elastomer/blend.
  • a grafting initiator (also referred to as “a radical initiator” in the disclosure) can be utilized in the grafting process of at least the first and second polyolefins by reacting with the respective polyolefins to form a reactive species that can react and/or couple with the silane crosslinker molecule.
  • the grafting initiator can include halogen molecules, azo compounds (e.g., azobisisobutyl), carboxylic peroxyacids, peroxyesters, peroxyketals, and peroxides (e.g., alkyl hydroperoxides, dialkyl peroxides, and diacyl peroxides).
  • the grafting initiator is an organic peroxide selected from di-t-butyl peroxide, t-butyl cumyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di(t-butyl-peroxy)hexyne-3,1,3-bis(t-butyl-peroxy-isopropyl)benzene, n-butyl-4,4-bis(t-butyl-peroxy)valerate, benzoyl peroxide, t-butylperoxybenzoate, t-butylperoxy isopropyl carbonate, and t-butylperbenzoate, as well as bis(2-methylbenzoyl)peroxide, bis(4-methylbenzoyl)peroxide, t-butyl peroctoate, cumene hydroperoxide, methyl ethyl ketone peroxide, lauryl peroxide, tert-butyl peroxide,
  • the grafting initiator is present in an amount of from greater than 0 wt % to about 2 wt % of the composition, including from about 0.15 wt % to about 1.2 wt % of the composition.
  • the amount of initiator and silane employed may affect the final structure of the silane grafted polymer (e.g., the degree of grafting in the grafted polymer and the degree of crosslinking in the cured polymer).
  • the reactive composition contains at least 100 ppm of initiator, or at least 300 ppm of initiator.
  • the initiator may be present in an amount from 300 ppm to 1500 ppm or from 300 ppm to 2000 ppm.
  • the silane:initiator weight ratio may be from about 20:1 to 400:1, including from about 30:1 to about 400:1, from about 48:1 to about 350:1, and from about 55:1 to about 333:1.
  • the grafting reaction can be performed under conditions that optimize grafts onto the interpolymer backbone while minimizing side reactions (e.g., the homopolymerization of the grafting agent).
  • the grafting reaction may be performed in a melt, in solution, in a solid-state, and/or in a swollen-state.
  • the silanation may be performed in a wide-variety of equipment (e.g., twin screw extruders, single screw extruders, Brabenders, internal mixers such as Banbury mixers, and batch reactors).
  • the polyolefin, silane, and initiator are mixed in the first stage of an extruder.
  • the melt temperature i.e., the temperature at which the polymer starts melting and begins to flow
  • a silane crosslinker can be used to covalently graft silane moieties onto the first and second polyolefins and the silane crosslinker may include alkoxysilanes, silazanes, siloxanes, or a combination thereof.
  • the grafting and/or coupling of the various potential silane crosslinkers or silane crosslinker molecules is facilitated by the reactive species formed by the grafting initiator reacting with the respective silane crosslinker.
  • the silane crosslinker is a silazane where the silazane may include, for example, hexamethyldisilazane (HMDS) or Bis(trimethylsilyl)amine.
  • the silane crosslinker is a siloxane where the siloxane may include, for example, polydimethylsiloxane (PDMS) and octamethylcyclotetrasiloxane.
  • the silane crosslinker is an alkoxysilane.
  • alkoxysilane refers to a compound that comprises a silicon atom, at least one alkoxy group and at least one other organic group, wherein the silicon atom is bonded with the organic group by a covalent bond.
  • the alkoxysilane is selected from alkylsilanes; acryl-based silanes; vinyl-based silanes; aromatic silanes; epoxy-based silanes; amino-based silanes and amines that possess —NH 2 , —NHCH 3 or —N(CH 3 ) 2 ; ureide-based silanes; mercapto-based silanes; and alkoxysilanes which have a hydroxyl group (i.e., —OH).
  • An acryl-based silane may be selected from the group comprising beta-acryloxyethyl trimethoxysilane; beta-acryloxy propyl trimethoxysilane; gamma-acryloxyethyl trimethoxysilane; gamma-acryloxypropyl trimethoxysilane; beta-acryloxyethyl triethoxysilane; beta-acryloxypropyl triethoxysilane; gamma-acryloxyethyl triethoxysilane; gamma-acryloxypropyl triethoxysilane; beta-methacryloxyethyl trimethoxysilane; beta-methacryloxypropyl trimethoxysilane; gamma-methacryloxyethyl trimethoxysilane; gamma-methacryloxypropyl trimethoxysilane; beta-methacryloxyethyl trimethoxysilane; beta-methacryloxypropyl
  • a vinyl-based silane may be selected from the group comprising vinyl trimethoxysilane; vinyl triethoxysilane; p-styryl trimethoxysilane, methylvinyldimethoxysilane, vinyldimethylmethoxysilane, divinyldimethoxysilane, vinyltris(2-methoxyethoxy)silane, and vinylbenzylethylenediaminopropyltrimethoxysilane.
  • An aromatic silane may be selected from phenyltrimethoxysilane and phenyltriethoxysilane.
  • An epoxy-based silane may be selected from the group comprising 3-glycydoxypropyl trimethoxysilane; 3-glycydoxypropylmethyl diethoxysilane; 3-glycydoxypropyl triethoxysilane; 2-(3,4-epoxycyclohexyl)ethyl trimethoxysilane, and glycidyloxypropylmethyldimethoxysilane.
  • An amino-based silane may be selected from the group comprising 3-aminopropyl triethoxysilane; 3-aminopropyl trimethoxysilane; 3-aminopropyldimethyl ethoxysilane; 3-aminopropylmethyldiethoxysilane; 4-aminobutyltriethoxysilane; 3-aminopropyldiisopropyl ethoxysilane; 1-amino-2-(dimethylethoxysilyl)propane; (aminoethylamino)-3-isobutyldimethyl methoxysilane; N-(2-aminoethyl)-3-aminoisobutylmethyl dimethoxysilane; (aminoethylaminomethyl)phenetyl trimethoxysilane; N-(2-aminoethyl)-3-aminopropylmethyl dimethoxysilane; N-(2-amino
  • An ureide-based silane may be 3-ureidepropyl triethoxysilane.
  • a mercapto-based silane may be selected from the group comprising 3-mercaptopropylmethyl dimethoxysilane, 3-mercaptopropyl trimethoxysilane, and 3-mercaptopropyl triethoxysilane.
  • An alkoxysilane having a hydroxyl group may be selected from the group comprising hydroxymethyl triethoxysilane; N-(hydroxyethyl)-N-methylaminopropyl trimethoxysilane; bis(2-hydroxyethyl)-3-aminopropyl triethoxysilane; N-(3-triethoxysilylpropyl)-4-hydroxy butylamide; 1,1-(triethoxysilyl)undecanol; triethoxysilyl undecanol; ethylene glycol acetal; and N-(3-ethoxysilylpropyl)gluconamide.
  • the alkylsilane may be expressed with a general formula: R n Si(OR′) 4-n wherein: n is 1, 2 or 3; R is a C 1-20 alkyl or a C 2-20 alkenyl; and R′ is an C 1-20 alkyl.
  • R n Si(OR′) 4-n wherein: n is 1, 2 or 3; R is a C 1-20 alkyl or a C 2-20 alkenyl; and R′ is an C 1-20 alkyl.
  • alkyl by itself or as part of another substituent, refers to a straight, branched or cyclic saturated hydrocarbon group joined by single carbon-carbon bonds having 1 to 20 carbon atoms, for example 1 to 10 carbon atoms, for example 1 to 8 carbon atoms, preferably 1 to 6 carbon atoms.
  • the subscript refers to the number of carbon atoms that the named group may contain.
  • C 1-6 alkyl means an alkyl of one to six carbon atoms.
  • alkyl groups are methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, f-butyl, 2-methylbutyl, pentyl, iso-amyl and its isomers, hexyl and its isomers, heptyl and its isomers, octyl and its isomer, decyl and its isomer, dodecyl and its isomers.
  • C 2-20 alkenyl by itself or as part of another substituent, refers to an unsaturated hydrocarbyl group, which may be linear, or branched, comprising one or more carbon-carbon double bonds having 2 to 20 carbon atoms.
  • Examples of C 2-6 alkenyl groups are ethenyl, 2-propenyl, 2-butenyl, 3-butenyl, 2-pentenyl and its isomers, 2-hexenyl and its isomers, 2,4-pentadienyl and the like.
  • the alkylsilane may be selected from the group comprising methyltrimethoxysilane; methyltriethoxysilane; ethyltrimethoxysilane; ethyltriethoxysilane; propyltrimethoxysilane; propyltriethoxysilane; hexyltrimethoxysilane; hexyltriethoxysilane; octyltrimethoxysilane; octyltriethoxysilane; decyltrimethoxysilane; decyltriethoxysilane; dodecyltrimethoxysilane: dodecyltriethoxysilane; tridecyltrimethoxysilane; dodecyltriethoxysilane; hexadecyltrimethoxysilane; hexadecyltriethoxysilane; octade
  • the alkylsilane compound may be selected from triethoxyoctylsilane, trimethoxyoctylsilane, and a combination thereof.
  • the silane crosslinker can include, but is not limited to, unsaturated silanes which include an ethylenically unsaturated hydrocarbyl group (e.g., a vinyl, allyl, isopropenyl, butenyl, cyclohexenyl or a gamma-(meth)acryloxy allyl group) and a hydrolyzable group (e.g., a hydrocarbyloxy, hydrocarbonyloxy, or hydrocarbylamino group).
  • unsaturated silanes which include an ethylenically unsaturated hydrocarbyl group (e.g., a vinyl, allyl, isopropenyl, butenyl, cyclohexenyl or a gamma-(meth)acryloxy allyl group) and a hydrolyzable group (e.g., a hydrocarbyloxy, hydrocarbonyloxy, or hydrocarbylamino group).
  • Non-limiting examples of hydrolyzable groups include, but are not limited to, methoxy, ethoxy, formyloxy, acetoxy, proprionyloxy, and alkyl, or arylamino groups.
  • the silane crosslinkers are unsaturated alkoxy silanes which can be grafted onto the polymer.
  • additional exemplary silane crosslinkers include vinyltrimethoxysilane, vinyltriethoxysilane, 3-(trimethoxysilyl)propyl methacrylate gamma-(meth)acryloxypropyl trimethoxysilane), and mixtures thereof.
  • the silane crosslinker may be present in the silane-grafted polyolefin elastomer in an amount of from greater than 0 wt % to about 10 wt %, including from about 0.5 wt % to about 5 wt %.
  • the amount of silane crosslinker may be varied based on the nature of the olefin polymer, the silane itself, the processing conditions, the grafting efficiency, the application, and other factors.
  • the amount of silane crosslinker may be at least 2 wt %, including at least 4 wt % or at least 5 wt %, based on the weight of the reactive composition.
  • the amount of silane crosslinker may be at least 10 wt %, based on the weight of the reactive composition.
  • the silane crosslinker content is at least 1% based on the weight of the reactive composition.
  • the silane crosslinker fed to the extruder may include from about 0.5 wt % to about 10 wt % of silane monomer, from about 1 wt % to about 5 wt % silane monomer, or from about 2 wt % to about 4 wt % silane monomer.
  • a condensation catalyst can facilitate both the hydrolysis and subsequent condensation of the silane grafts on the silane-grafted polyolefin elastomer to form crosslinks.
  • the crosslinking can be aided by the use of an electron beam radiation.
  • the condensation catalyst can include, for example, organic bases, carboxylic acids, and organometallic compounds (e.g., organic titanates and complexes or carboxylates of lead, cobalt, iron, nickel, zinc, and tin).
  • the condensation catalyst can include fatty acids and metal complex compounds such as metal carboxylates; aluminum triacetyl acetonate, iron triacetyl acetonate, manganese tetraacetyl acetonate, nickel tetraacetyl acetonate, chromium hexaacetyl acetonate, titanium tetraacetyl acetonate and cobalt tetraacetyl acetonate; metal alkoxides such as aluminum ethoxide, aluminum propoxide, aluminum butoxide, titanium ethoxide, titanium propoxide and titanium butoxide; metal salt compounds such as sodium acetate, tin octylate, lead octylate, cobalt octylate, zinc octylate, calcium octylate, lead naphthenate, cobalt naphthenate, dibutyltin dioctoate, di
  • the condensation catalyst can include ibutyltindilaurate, dioctyltinmaleate, dibutyltindiacetate, dibutyltindioctoate, stannous acetate, stannous octoate, lead naphthenate, zinc caprylate, and cobalt naphthenate.
  • a single condensation catalyst or a mixture of condensation catalysts may be utilized.
  • the condensation catalyst(s) may be present in an amount of from about 0.01 wt % to about 1.0 wt %, including from about 0.25 wt % to about 8 wt %, based on the total weight of the silane-grafted polyolefin elastomer/blend composition.
  • a crosslinking system can include and use one or all of a combination of radiation, heat, moisture, and additional condensation catalyst.
  • the condensation catalyst may be present in an amount of from 0.25 wt % to 8 wt %. In other aspects, the condensation catalyst may be included in an amount of from about 1 wt % to about 10 wt % or from about 2 wt % to about 5 wt %.
  • the silane-crosslinked polyolefin elastomer may optionally include one or more fillers.
  • the filler(s) may be extruded with the silane-grafted polyolefin and in some aspects may include additional polyolefins having a crystallinity greater than 20%, greater than 30%, greater than 40%, or greater than 50%.
  • the filler(s) may include metal oxides, metal hydroxides, metal carbonates, metal sulfates, metal silicates, clays, talcs, carbon black, and silicas. Depending on the application and/or desired properties, these materials may be fumed or calcined.
  • the metal of the metal oxide, metal hydroxide, metal carbonate, metal sulfate, or metal silicate may be selected from alkali metals (e.g., lithium, sodium, potassium, rubidium, caesium, and francium); alkaline earth metals (e.g., beryllium, magnesium, calcium, strontium, barium, and radium); transition metals (e.g., zinc, molybdenum, cadmium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, yttrium, zirconium, niobium, technetium, ruthernium, rhodium, palladium, silver, hafnium, taltalum, tungsten, rhenium, osmium, indium, platinum, gold, mercury, rutherfordium, dubnium, seaborgium, bohrium, hassium, and copernicium
  • alkali metals
  • the filler(s) of the silane-crosslinked polyolefin elastomer or blend may be present in an amount of from greater than 0 wt % to about 50 wt %, including from about 1 wt % to about 20 wt %, and from about 3 wt % to about 10 wt %.
  • the silane-crosslinked polyolefin elastomer and/or the respective articles formed may also include waxes (e.g., paraffin waxes, microcrystalline waxes, HDPE waxes, LDPE waxes, thermally degraded waxes, byproduct polyethylene waxes, optionally oxidized Fischer-Tropsch waxes, and functionalized waxes).
  • the wax(es) are present in an amount of from about 0 wt % to about 10 wt %.
  • Tackifying resins e.g., aliphatic hydrocarbons, aromatic hydrocarbons, modified hydrocarbons, terpens, modified terpenes, hydrogenated terpenes, rosins, rosin derivatives, hydrogenated rosins, and mixtures thereof
  • the tackifying resins may have a ring and ball softening point in the range of from 70° C. to about 150° C. and a viscosity of less than about 3,000 cP at 177° C.
  • the tackifying resin(s) are present in an amount of from about 0 wt % to about 10 wt %.
  • the silane-crosslinker polyolefin elastomer may include one or more oils.
  • oils include white mineral oils and naphthenic oils.
  • the oil(s) are present in an amount of from about 0 wt % to about 10 wt %.
  • the silane-crosslinked polyolefin elastomer may include one or more filler polyolefins having a crystallinity greater than 20%, greater than 30%, greater than 40%, or greater than 50%.
  • the filler polyolefin may include polypropylene, poly(ethylene-co-propylene), and/or other ethylene/ ⁇ -olefin copolymers.
  • the use of the filler polyolefin may be present in an amount of from about 5 wt % to about 60 wt %, from about 10 wt % to about 50 wt %, from about 20 wt % to about 40 wt %, or from about 5 wt % to about 20 wt %.
  • the addition of the filler polyolefin may increase the Young's modulus by at least 10%, by at least 25%, or by at least 50% for the final silane-crosslinked polyolefin elastomer.
  • the silane-crosslinker polyolefin elastomer of the present disclosure may include one or more stabilizers (e.g., antioxidants).
  • the silane-crosslinked polyolefin elastomer may be treated before grafting, after grafting, before crosslinking, and/or after crosslinking.
  • Other additives may also be included.
  • additives include antistatic agents, dyes, pigments, UV light absorbers, nucleating agents, fillers, slip agents, plasticizers, fire retardants, lubricants, processing aides, smoke inhibitors, anti-blocking agents, and viscosity control agents.
  • the antioxidant(s) may be present in an amount of less than 0.5 wt %, including less than 0.2 wt % of the composition.
  • titanium dioxide a white pigment
  • the titanium dioxide may be added to the formulation to provide opacity and color.
  • the titanium dioxide also may provide ultraviolet light protection.
  • the titanium dioxide may be pre-blended with the first and/or second polyolefins (of the type set forth above) to ensure complete dispersal of the titanium dioxide throughout the composition.
  • the titanium dioxide may be pre-blended with the first and/or second polyolefins in an amount up to 30 wt %, up to 20 wt %, or up to 10 wt %.
  • the synthesis/production of the silane-crosslinked polyolefin elastomer may be performed by combining the respective components in one extruder using a single-step Monosil process or in two extruders using a two-step Sioplas process, which eliminates the need for additional steps of mixing and shipping rubber compounds prior to extrusion.
  • the general chemical process used during both the single-step Monosil process and two-step Sioplas process used to synthesize the silane-crosslinked polyolefin elastomer starts with a grafting step that includes initiation from a grafting initiator followed by propagation and chain transfer with the first and second polyolefins.
  • the grafting initiator in some aspects a peroxide or azo compound, homolytically cleaves to form two radical initiator fragments that transfer to one of the first and second polyolefins chains through a propagation step.
  • the free radical now positioned on the first or second polyolefin chain, can then transfer to a silane molecule and/or another polyolefin chain. Once the initiator and free radicals are consumed, the silane grafting reaction for the first and second polyolefins is complete.
  • a crosslinking catalyst may then be added to the first and second silane-grafted polyolefins to form the silane-grafted polyolefin elastomer.
  • the crosslinking catalyst may first facilitate the hydrolysis of the silyl group grafted onto the polyolefin backbones to form reactive silanol groups.
  • the silanol groups may then react with other silanol groups on other polyolefin molecules to form a crosslinked network of elastomeric polyolefin polymer chains linked together through siloxane linkages.
  • the density of silane crosslinks throughout the silane-grafted polyolefin elastomer can influence the material properties exhibited by the elastomer.
  • the method 200 may begin with a step 204 that includes extruding (e.g., with a twin screw extruder 252 ) a first polyolefin 240 having a density less than 0.86 g/cm 3 , a second polyolefin 244 , and a silan cocktail 248 including the silane crosslinker (e.g., vinyltrimethoxy silane, VTMO) and the grafting initiator (e.g. dicumyl peroxide) together to form a silane-grafted polyolefin blend.
  • extruding e.g., with a twin screw extruder 252
  • a first polyolefin 240 having a density less than 0.86 g/cm 3 e.g., a twin screw extruder 252
  • a second polyolefin 244 e.g., a second polyolefin 244
  • a silan cocktail 248 including the silane crosslinker (e.g
  • the first polyolefin 240 and second polyolefin 244 may be added to a reactive twin screw extruder 252 using an addition hopper 256 .
  • the silan cocktail 248 may be added to the twin screws 260 further down the extrusion line to help promote better mixing with the blend of the first and second polyolefins 240 , 244 .
  • a forced volatile organic compound (VOC) vacuum 264 may be used on the reactive twin screw extruder 252 to help maintain a desired reaction pressure.
  • the twin screw extruder 252 is considered reactive because the radical initiator and silane crosslinker are reacting with and forming new covalent bonds with both the first and second polyolefins 240 , 244 .
  • the melted silane-grafted polyolefin blend can exit the reactive twin screw extruder 252 using a gear pump 268 that injects the molten silane-grafted polyolefin blend into a water pelletizer 272 that can form a pelletized silane-grafted polyolefin blend 276 .
  • the molten silane-grafted polyolefin blend 276 may be extruded into pellets, pillows, or any other configuration prior to the incorporation of the condensation catalyst 280 (see FIG. 4B ) and formation of the final article (e.g., a roofing membrane 10 as depicted in FIG. 1 ).
  • the reactive twin screw extruder 252 can be configured to have a plurality of different temperature zones (e.g., Z 0 -Z 12 as shown in FIG. 4A ) that extend for various lengths of the twin screw extruder 252 .
  • the respective temperature zones may have temperatures ranging from about room temperature to about 180° C., from about 120° C. to about 170° C., from about 120° C. to about 160° C., from about 120° C. to about 150° C., from about 120° C. to about 140° C., from about 120° C. to about 130° C., from about 130° C. to about 170° C., from about 130° C. to about 160° C., from about 130° C.
  • Z 0 may have a temperature from about 60° C. to about 110° C. or no cooling;
  • Z 1 may have a temperature from about 120° C. to about 130° C.;
  • Z 2 may have a temperature from about 140° C. to about 150° C.;
  • Z 3 may have a temperature from about 150° C. to about 160° C.;
  • Z 4 may have a temperature from about 150° C.
  • Z 5 may have a temperature from about 150° C. to about 160° C.
  • Z 6 may have a temperature from about 150° C. to about 160° C.
  • Z 7 may have a temperature from about 150° C. to about 160° C.
  • Z 8 -Z 12 may have a temperature from about 150° C. to about 160° C.
  • the number average molecular weight of the silane-grafted polyolefin elastomers may be in the range of from about 4,000 g/mol to about 30,000 g/mol, including from about 5,000 g/mol to about 25,000 g/mol and from about 6,000 g/mol to about 14,000 g/mol.
  • the weight average molecular weight of the grafted polymers may be from about 8,000 g/mol to about 60,000 g/mol, including from about 10,000 g/mol to about 30,000 g/mol.
  • the method 200 next includes a step 208 of extruding the silane-grafted polyolefin blend 276 and the condensation catalyst 280 together to form a silane-crosslinkable polyolefin blend 298 .
  • one or more optional additives 284 may be added with the silane-grafted polyolefin blend 276 and the condensation catalyst 280 to adjust the final material properties of the silane-crosslinkable polyolefin blend 298 .
  • the silane-grafted polyolefin blend 276 is mixed with a silanol forming condensation catalyst 280 to form reactive silanol groups on the silane grafts that can subsequently crosslink when exposed to humidity and/or heat.
  • the condensation catalyst 280 can include a mixture of sulfonic acid, antioxidant, process aide, and carbon black for coloring where the ambient moisture is sufficient for this condensation catalyst 280 to crosslink the silane-crosslinkable polyolefin blend 298 over a longer time period (e.g., about 48 hours).
  • the silane-grafted polyolefin blend 276 and the condensation catalyst 280 may be added to a reactive single screw extruder 288 using an addition hopper (similar to addition hopper 256 shown in FIG. 4A ) and an addition gear pump 296 .
  • the combination of the silane-grafted polyolefin blend 276 and the condensation catalyst 280 , and in some aspects one or more optional additives 284 may be added to a single screw 292 of the reactive single screw extruder 288 .
  • the single screw extruder 288 is considered reactive because the silane-grafted polyolefin blend 276 and the condensation catalyst 280 are melted and combined together to mix the condensation catalyst 280 thoroughly and evenly throughout the melted silane-grafted polyolefin blend 276 .
  • the melted silane-crosslinkable polyolefin blend 298 can exit the reactive single screw extruder 288 through a die that can inject the molten silane-crosslinkable polyolefin blend 298 into the form of an uncured roofing membrane element.
  • the silane-crosslinkable polyolefin blend 298 may be about 25% cured, about 30% cured, about 35% cured, about 40% cured, about 45% cured, about 50% cured, about 55% cured, about 60% cured, bout 65% cured, or about 70% cured, where a gel test (ASTM D2765) can be used to determine the amount of crosslinking in the final silane-crosslinked polyolefin elastomer.
  • a gel test ASTM D2765
  • the method 200 further includes a step 212 of extruding and/or calendaring the silane-crosslinkable polyolefin elastomer or blend 298 to form the top and bottom layers 14 , 38 , as comprising the uncured silane-crosslinkable polyolefin elastomer.
  • the silane-crosslinkable polyolefin elastomer or blend 298 is in a melted or molten state where it can flow and be shaped as it exits the reactive single screw extruder 288 .
  • a calendar system 302 is a device having two or more rollers (the area between the rollers is called a nip) used to process the melted silane-crosslinkable polyolefin elastomer blend 298 into a sheet or film.
  • a nip the area between the rollers used to process the melted silane-crosslinkable polyolefin elastomer blend 298 into a sheet or film.
  • the melted silane-crosslinkable polyolefin elastomer blend 298 leaves the reactive single screw extruder 288 , it forms a pool of silane-crosslinkable polyolefin elastomer 306 at a first nip point of the calendar system 302 .
  • the pool of silane-crosslinkable polyolefin elastomer 306 is then pressed or rolled into the top or bottom layer 14 , 38 respectively.
  • the scrim layer 26 may be added to the top or bottom layer 14 , 38 , respectively, at any point during the calendaring process using a scrim roll 318 .
  • the scrim layer 26 as coupled to the top or bottom layer 14 , 38 , forms a partial scrim membrane 322 .
  • the partial scrim membrane 322 may be further calendared and pressed with the respectively missing top or bottom layer 14 , 38 to form the uncured roofing membrane element.
  • the method 200 can further include a step 216 of crosslinking the silane-crosslinkable polyolefin blend 298 or the roofing membrane element in an uncured form at an ambient temperature and/or an ambient humidity to form the roofing membrane 10 (see FIG. 1 ) having a density from about 0.85 g/cm 3 to about 0.89 g/cm 3 .
  • the water hydrolyzes the silane of the silane-crosslinkable polyolefin elastomer to produce a silanol.
  • the silanol groups on various silane grafts can then be condensed to form intermolecular, irreversible Si—O—Si crosslink sites.
  • the amount of crosslinked silane groups, and thus the final polymer properties, can be regulated by controlling the production process, including the amount of catalyst used.
  • the crosslinking/curing of step 216 of the method 200 may occur over a time period of from greater than 0 to about 20 hours.
  • curing takes place over a time period of from about 1 hour to about 20 hours, 10 hours to about 20 hours, from about 15 hours to about 20 hours, from about 5 hours to about 15 hours, from about 1 hour to about 8 hours, or from about 3 hours to about 6 hours.
  • the temperature during the crosslinking/curing may be about room temperature, from about 20° C. to about 25° C., from about 20° C. to about 150° C., from about 25° C. to about 100° C., or from about 20° C. to about 75° C.
  • the humidity during curing may be from about 30% to about 100%, from about 40% to about 100%, or from about 50% to about 100%.
  • an extruder setting is used that is capable of extruding thermoplastic, with long L/D, 30 to 1, at an extruder heat setting close to TPV processing conditions wherein the extrudate crosslinks at ambient conditions becoming a thermoset in properties.
  • this process may be accelerated by steam exposure.
  • the gel content also called the crosslink density
  • the gel content may be about 60%, but after 96 hrs at ambient conditions, the gel content may reach greater than about 95%.
  • one or more reactive single screw extruders 288 may be used to form the uncured roofing membrane element (and corresponding single ply roofing membrane 10 ) that has one or more types of silane-crosslinked polyolefin elastomers.
  • one reactive single screw extruder 288 may be used to produce and extrude a first silane-crosslinked polyolefin elastomer associated employed in a top layer 14 of a roofing membrane 10 (see FIG. 1 ), while a second reactive single screw extruder 288 may be used to produce and extrude a second silane-crosslinked polyolefin elastomer employed in a bottom layer 38 of the roofing membrane 10 .
  • the complexity, architecture and property requirements of the roofing membrane 10 will determine the number and types of reactive single screw extruder 288 necessary to fabricate it.
  • the method 400 may begin with a step 404 that includes extruding (e.g., with a single screw extruder 444 ) the first polyolefin 240 having a density less than 0.86 g/cm 3 , the second polyolefin 244 , the silan cocktail 248 including the silane crosslinker (e.g., vinyltrimethoxy silane, VTMO) and grafting initiator (e.g. dicumyl peroxide), and the condensation catalyst 280 together to form the crosslinkable silane-grafted polyolefin blend 298 .
  • the silane crosslinker e.g., vinyltrimethoxy silane, VTMO
  • grafting initiator e.g. dicumyl peroxide
  • the first polyolefin 240 , second polyolefin 244 , and silan cocktail 248 may be added to the reactive single screw extruder 444 using an addition hopper 440 .
  • the silan cocktail 248 may be added to a single screw 448 further down the extrusion line to help promote better mixing with the first and second polyolefin 240 , 244 blend.
  • one or more optional additives 284 may be added with the first polyolefin 240 , second polyolefin 244 , condensation catalyst 280 and silan cocktail 248 to adjust the final material properties of the silane-crosslinkable polyolefin blend 298 .
  • the single screw extruder 444 is considered reactive because the grafting initiator and silane crosslinker of the silan cocktail 248 are reacting with and forming new covalent bonds with both the first and second polyolefins 240 , 244 .
  • the reactive single screw extruder 444 mixes the condensation catalyst 280 in together with the melted silane-grafted polyolefin blend comprising the first and second polyolefins 240 , 244 , silan cocktail 248 and any optional additives 284 .
  • the resulting melted silane-crosslinkable polyolefin blend 298 can exit the reactive single screw extruder 444 using a gear pump (not shown) and/or die that can eject the molten silane-crosslinkable polyolefin blend 298 into the form of an uncured roofing membrane element.
  • the silane-crosslinkable polyolefin blend 298 may be about 25% cured, about 30% cured, about 35% cured, about 40% cured, about 45% cured, about 50% cured, about 55% cured, about 60% cured, bout 65% cured, or about 70% as it leaves the reactive single screw extruder 444 .
  • the gel test (ASTM D2765) can be used to determine the amount of crosslinking in the final silane-crosslinked polyolefin elastomer.
  • the reactive single screw extruder 444 can be configured to have a plurality of different temperature zones (e.g., Z 0 -Z 7 as shown in FIG. 6 ) that extend for various lengths along the extruder.
  • the respective temperature zones may have temperatures ranging from about room temperature to about 180° C., from about 120° C. to about 170° C., from about 120° C. to about 160° C., from about 120° C. to about 150° C., from about 120° C. to about 140° C., from about 120° C. to about 130° C., from about 130° C. to about 170° C., from about 130° C. to about 160° C., from about 130° C. to about 150° C., from about 130° C.
  • Z 0 may have a temperature from about 60° C. to about 110° C. or no cooling;
  • Z 1 may have a temperature from about 120° C. to about 130° C.;
  • Z 2 may have a temperature from about 140° C. to about 150° C.;
  • Z 3 may have a temperature from about 150° C. to about 160° C.;
  • Z 4 may have a temperature from about 150° C.
  • Z 5 may have a temperature from about 150° C. to about 160° C.
  • Z 6 may have a temperature from about 150° C. to about 160° C.
  • Z 7 may have a temperature from about 150° C. to about 160° C.
  • the number average molecular weight of the silane-grafted polyolefin elastomers may be in the range of from about 4,000 g/mol to about 30,000 g/mol, including from about 5,000 g/mol to about 25,000 g/mol and from about 6,000 g/mol to about 14,000 g/mol.
  • the weight average molecular weight of the grafted polymers may be from about 8,000 g/mol to about 60,000 g/mol, including from about 10,000 g/mol to about 30,000 g/mol.
  • the method 400 further includes a step 408 of extruding and/or calendaring the silane-crosslinkable polyolefin elastomer or blend 298 to form the top and bottom layers 14 , 38 , as comprising the uncured silane-crosslinkable polyolefin elastomer.
  • the silane-crosslinkable polyolefin elastomer or blend 298 is in a melted or molten state where it can flow and be shaped as it exits the reactive single screw extruder 444 .
  • the calendar system 302 is a device having two or more rollers (the area between the rollers is called a nip) used to process the melted silane-crosslinkable polyolefin elastomer blend 298 into a sheet or film.
  • a nip the area between the rollers used to process the melted silane-crosslinkable polyolefin elastomer blend 298 into a sheet or film.
  • the melted silane-crosslinkable polyolefin elastomer blend 298 leaves the reactive single screw extruder 444 , it forms a pool of silane-crosslinkable polyolefin elastomer 306 at a first nip point of the calendar system 302 .
  • the pool of silane-crosslinkable polyolefin elastomer 306 is then pressed or rolled into the top or bottom layer 14 , 38 , respectively.
  • the scrim layer 26 may be added to the top or bottom layer 14 , 38 respectively at any point during the calendaring process using a scrim roll 318 .
  • the scrim layer 26 as coupled to the top or bottom layer 14 , 38 , forms a partial scrim membrane 322 .
  • the partial scrim membrane 322 may be further calendared and pressed with the respectively missing top or bottom layer 14 , 38 to form an uncured roofing membrane element.
  • the method 400 can further include a step 412 of crosslinking the silane-crosslinkable polyolefin blend 298 of the uncured roofing membrane element at an ambient temperature and an ambient humidity to form the element into the roofing membrane 10 (see FIG. 1 ) having a density from about 0.85 g/cm 3 to about 0.89 g/cm 3 .
  • the amount of crosslinked silane groups, and thus the final polymer properties of the roofing membrane 10 can be regulated by controlling the production process, including the amount of catalyst used.
  • the step 412 of crosslinking the silane-crosslinkable polyolefin blend 298 may occur over a time period of from greater than 0 to about 20 hours.
  • curing takes place over a time period of from about 1 hour to about 20 hours, 10 hours to about 20 hours, from about 15 hours to about 20 hours, from about 5 hours to about 15 hours, from about 1 hour to about 8 hours, or from about 3 hours to about 6 hours.
  • the temperature during the crosslinking and curing may be about room temperature, from about 20° C. to about 25° C., from about 20° C. to about 150° C., from about 25° C. to about 100° C., or from about 20° C. to about 75° C.
  • the humidity during curing may be from about 30% to about 100%, from about 40% to about 100%, or from about 50% to about 100%.
  • an extruder setting is used that is capable of extruding thermoplastic, with long L/D, 30 to 1, at an extruder heat setting close to TPV processing conditions wherein the extrudate crosslinks at ambient conditions becoming a thermoset in properties.
  • this process may be accelerated by steam exposure.
  • the gel content also called the crosslink density
  • the gel content may be about 60%, but after 96 hrs at ambient conditions, the gel content may reach greater than about 95%.
  • one or more reactive single screw extruders 444 may be used to form the roofing membrane 10 that has one or more types of silane-crosslinked polyolefin elastomers.
  • one reactive single screw extruder 444 may be used to produce and extrude a first silane-crosslinked polyolefin elastomer associated with the top layer 14 of the roofing membrane 10 (see FIG. 1 ), while a second reactive single screw extruder 444 may be used to produce and extrude a second silane-crosslinked polyolefin elastomer associated with the bottom layer 38 of the roofing membrane 10 .
  • the complexity, architecture and required properties of the final roofing membrane 10 will determine the number and types of reactive single screw extruders 444 employed according to the method 400 depicted in FIG. 5 .
  • thermoplastic is defined to mean a polymer that softens when exposed to heat and returns to its original condition when cooled to room temperature.
  • thermoset is defined to mean a polymer that solidifies and irreversibly “sets” or “crosslinks” when cured. In either of the Monosil or Sioplas processes described above, it is important to understand the careful balance of thermoplastic and thermoset properties of the various different materials used to produce the final thermoset silane-crosslinked polyolefin elastomer or roofing membrane 10 .
  • Each of the intermediate polymer materials mixed and reacted using a reactive twin screw extruder, and/or a reactive single screw extruder are thermosets.
  • the silane-grafted polyolefin blend 276 and the silane-crosslinkable polyolefin blend 298 are thermoplastics and can be softened by heating so the respective materials can flow.
  • the silane-crosslinkable polyolefin blend 298 can begin to crosslink or cure at an ambient temperature and an ambient humidity to form the roofing membrane 10 (or other end product form), as comprising one or more silane-crosslinked polyolefin blends.
  • thermoplastic/thermoset behavior of the silane-crosslinkable polyolefin blend 298 and corresponding silane-crosslinked polyolefin blend are important for the various compositions and articles disclosed herein (e.g., roofing membrane 10 shown in FIG. 1 ) because of the potential energy savings provided using these materials.
  • a manufacturer can save considerable amounts of energy by being able to cure the silane-crosslinkable polyolefin blend 298 at an ambient temperature and an ambient humidity. This curing process is typically performed in the industry by applying significant amounts of energy to heat or steam treat crosslinkable polyolefins 298 .
  • the ability to cure the inventive silane-crosslinkable polyolefin blend 298 with ambient temperature and/or ambient humidity is not a capability necessarily intrinsic to crosslinkable polyolefins. Rather, this capability or property is dependent on the relatively low density of the silane-crosslinkable polyolefin blend 298 . In some aspects, no additional curing overs, heating ovens, steam ovens, or other forms of heat producing machinery other than what was provided in the extruders are used to form the silane-crosslinked polyolefin elastomers.
  • the specific gravity of the silane-crosslinked polyolefin elastomer of the present disclosure may be lower than the specific gravities of existing TPV and EPDM formulations used in the art.
  • the reduced specific gravity of these materials can lead to lower weight parts, thereby facilitating additional ease-of-assembly for roofers and other individuals charged with installing the roofing membranes 10 of the disclosure.
  • the specific gravity of the silane-crosslinked polyolefin elastomer of the present disclosure may be from about 0.80 g/cm 3 to about 1.50 g/cm 3 , from about 1.25 g/cm 3 to about 1.45 g/cm 3 , from about 1.30 g/cm 3 to about 1.40 g/cm 3 , about 1.25 g/cm 3 , about 1.30 g/cm 3 , about 1.35 g/cm 3 , about 1.40 g/cm 3 , about 1.45 g/cm 3 , about 1.50 g/cm 3 , less than 1.75 g/cm 3 , less than 1.60 g/cm 3 , less than 1.50 g/cm 3 , or less than 1.45 g/cm 3 , as compared to conventional TPV materials which may have a specific gravity greater than 2.00 g/cm 3 and conventional EPDM materials which may have a specific gravity of from 2.0 g/cm 3
  • FIG. 7 displays a smaller area between the stress/strain curves for the silane-crosslinked polyolefin of the disclosure (labeled as “Silane Cross-linked Polyolefin Elastomer” in FIG. 7 ), as compared to the areas between the stress/strain curves of EPDM compound A and EPDM compound B. This smaller area between the stress/strain curves for the silane-crosslinked polyolefin elastomer can be desirable for roofing membranes 10 .
  • Elastomeric materials typically have non-linear stress/strain curves with a significant loss of energy when repeatedly stressed.
  • the silane-crosslinked polyolefin elastomers of the present disclosure may exhibit greater elasticity and less viscoelasticity (e.g., have linear curves and exhibit very low energy loss).
  • Embodiments of the silane-crosslinked polyolefin elastomers described herein do not have any filler or plasticizer incorporated into these materials so their corresponding stress/strain curves do not have or display any Mullins effect and/or Payne effect.
  • the lack of Mullins effect for these silane-crosslinked polyolefin elastomers is due to the lack of any filler or plasticizer added to the silane-crosslinked polyolefin blend so the stress/strain curve does not depend on the maximum loading previously encountered where there is no instantaneous and irreversible softening.
  • the lack of Payne effect for these silane-crosslinked polyolefin elastomers is due to the lack of any filler or plasticizer added to the silane-crosslinked polyolefin blend so the stress/strain curve does not depend on the small strain amplitudes previously encountered where there is no change in the viscoelastic storage modulus based on the amplitude of the strain.
  • the silane-crosslinked polyolefin elastomer or roofing membrane 10 can exhibit a compression set of from about 5.0% to about 30.0%, from about 5.0% to about 25.0%, from about 5.0% to about 20.0%, from about 5.0% to about 15.0%, from about 5.0% to about 10.0%, from about 10.0% to about 25.0%, from about 10.0% to about 20.0%, from about 10.0% to about 15.0%, from about 15.0% to about 30.0%, from about 15.0% to about 25.0%, from about 15.0% to about 20.0%, from about 20.0% to about 30.0%, or from about 20.0% to about 25.0%, as measured according to ASTM D 395 (22 hrs @ 23° C., 70° C., 80° C., 90° C., 125° C., and/or 175° C.).
  • the silane-crosslinked polyolefin elastomer or roofing membrane 10 can exhibit a compression set of from about 5.0% to about 20.0%, from about 5.0% to about 15.0%, from about 5.0% to about 10.0%, from about 7.0% to about 20.0%, from about 7.0% to about 15.0%, from about 7.0% to about 10.0%, from about 9.0% to about 20.0%, from about 9.0% to about 15.0%, from about 9.0% to about 10.0%, from about 10.0% to about 20.0%, from about 10.0% to about 15.0%, from about 12.0% to about 20.0%, or from about 12.0% to about 15.0%, as measured according to ASTM D 395 (22 hrs @ 23° C., 70° C., 80° C., 90° C., 125° C., and/or 175° C.).
  • the silane-crosslinked polyolefin elastomer or roofing membrane 10 may exhibit a crystallinity of from about 5% to about 40%, from about 5% to about 25%, from about 5% to about 15%, from about 10% to about 20%, from about 10% to about 15%, or from about 11% to about 14% as determined using density measurements, differential scanning calorimetry (DSC), X-Ray Diffraction, infrared spectroscopy, and/or solid state nuclear magnetic spectroscopy. As disclosed herein, DSC was used to measure the enthalpy of melting in order to calculate the crystallinity of the respective samples.
  • the silane-crosslinked polyolefin elastomer or roofing membrane 10 may exhibit a glass transition temperature of from about ⁇ 75° C. to about ⁇ 25° C., from about ⁇ 65° C. to about ⁇ 40° C., from about ⁇ 60° C. to about ⁇ 50° C., from about ⁇ 50° C. to about ⁇ 25° C., from about ⁇ 50° C. to about ⁇ 30° C., or from about ⁇ 45° C. to about ⁇ 25° C. as measured according to differential scanning calorimetry (DSC) using a second heating run at a rate of 5° C./min or 10° C./min.
  • DSC differential scanning calorimetry
  • the silane-crosslinked polyolefin elastomer or roofing membrane 10 may exhibit a weathering color difference of from about 0.25 ⁇ E to about 2.0 ⁇ E, from about 0.25 ⁇ E to about 1.5 ⁇ E, from about 0.25 ⁇ E to about 1.0 ⁇ E, or from about 0.25 ⁇ E to about 0.5 ⁇ E, as measured according to ASTM D2244.
  • the roofing membrane 10 may be a high-load flame retardant thermoplastic polyolefin (TPO) having the above weathering properties.
  • Example 1 (Ex. 1) or ED76-4A was produced by extruding 82.55 wt % ENGAGETM 8842 and 14.45 wt % MOSTENTM TB 003 together with 3.0 wt % SILAN RHS 14/032 or SILFIN 29 to form a silane-grafted polyolefin elastomer, according to one of the foregoing methods outlined in the disclosure.
  • the Example 1 silane-grafted polyolefin elastomer was then extruded using various condensation catalysts and fillers to form a silane-crosslinkable polyolefin elastomer, as suitable for top and bottom layers 14 , 38 of a roofing membrane (as described below in Example 2).
  • the composition of the Example 1 silane-grafted polyolefin elastomer is provided in Table 1 below.
  • top and bottom layers 14 , 38 were used to produce an embodiment of a single ply roofing membrane 10 .
  • the top and bottom layers 14 38 were produced by extruding 29.0 wt % silane-grafted polyolefin elastomer (from Example 1) and 70.0 wt % vinyl silane coated magnesium dihydroxide, Mg(OH) 2 (MDH), together with 1.0 wt % dioctyltin dilaurate (DOTL) condensation catalyst to form a silane-crosslinkable polyolefin elastomer blend.
  • the blend was then extruded and calendared to provide the respective top and bottom layers 14 , 38 of an uncured roofing membrane element.
  • the silane-crosslinkable polyolefin elastomer of the layers 14 , 38 of the uncured roofing membrane element was then cured at ambient temperature and humidity to form the roofing membrane 10 .
  • the composition of the roofing membrane 10 formed in this example is provided in Table 2 below.
  • top and bottom layers 14 , 38 were used to produce another embodiment of a single ply roofing membrane 10 .
  • the top and bottom layers 14 , 38 were produced by extruding 29.0 wt % silane-grafted polyolefin elastomer (from Example 1) and 70.0 wt % stearic acid coated magnesium dihydroxide, Mg(OH) 2 (MDH), together with 1.0 wt % dioctyltin dilaurate (DOTL) condensation catalyst to form a silane-crosslinkable polyolefin elastomer blend.
  • the blend was then extruded and calendared to provide the respective top and bottom layers 14 , 38 of an uncured roofing membrane element.
  • the silane-crosslinkable polyolefin elastomer of the layers 14 , 38 of the uncured roofing membrane element was then cured at ambient temperature and humidity to form the roofing membrane 10 .
  • the composition of the roofing membrane 10 formed in this example is also provided in Table 2 below.
  • Example 1 can retain nearly 90% of its elastic properties at 150° C. for greater than 500 hrs.
  • the retention of elastic properties as provided in Example 1 is representative of each of the inventive silane-crosslinked polyolefin elastomers disclosed herein.
  • the roofing member made from these silane-crosslinked polyolefin elastomers may retain up to 60%, 70%, 80%, or 90% of its elastic properties as determined by using Stress Relaxation measurements at 150° C. for greater than 100 hrs, greater than 200 hrs, greater than 300 hrs, greater than 400 hrs, and greater than 500 hrs.
  • the compression set values are provided across a time period of 4,000 hrs for Ex. 1 that demonstrates the superior long term retention of elastic properties of the silane-crosslinked polyolefin elastomer material used to make the roofing membrane 10 .
  • the Ex. 1 silane-crosslinked polyolefin elastomer material maintains a compression set of 35% or lower as measured according to ASTM D 395 (30% @ 110° C.).
  • ASTM D 395 30% @ 110° C.
  • the ability of these silane-crosslinked polyolefin elastomer materials used in roofing membranes 10 to retain its elasticity (compression set %) over a long period of time upon exposure to heat that simulates exterior weathering or aging is provided by this representative example of these roofing membrane 10 materials.
  • the term “coupled” in all of its forms, couple, coupling, coupled, etc. generally means the joining of two components directly or indirectly to one another. Such joining may be stationary in nature or movable in nature. Such joining may be achieved with the two components and any additional intermediate members being integrally formed as a single unitary body with one another or with the two components. Such joining may be permanent in nature or may be removable or releasable in nature unless otherwise stated.
  • elements shown as integrally formed may be constructed of multiple parts or elements shown as multiple parts may be integrally formed, the operation of the interfaces may be reversed or otherwise varied, the length or width of the structures and/or members or connector or other elements of the system may be varied, the nature or number of adjustment positions provided between the elements may be varied.
  • the elements and/or assemblies of the system may be constructed from any of a wide variety of materials that provide sufficient strength or durability, in any of a wide variety of colors, textures, and combinations. Accordingly, all such modifications are intended to be included within the scope of the present innovations. Other substitutions, modifications, changes, and omissions may be made in the design, operating conditions, and arrangement of the desired and other exemplary embodiments without departing from the spirit of the present innovations.
  • Embodiment A is a roofing membrane comprising: a top layer comprising a flame retardant and a first silane-crosslinked polyolefin elastomer having a density less than 0.90 g/cm 3 ; a scrim layer; and a bottom layer comprising a flame retardant and a second silane-crosslinked polyolefin elastomer having a density less than 0.90 g/cm 3 , wherein the top and bottom layers of the single ply roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according to ASTM D 395 (22 hrs @ 70° C.).
  • the roofing membrane of Embodiment A wherein the compression set is from about 10% to about 30%.
  • first and second silane-crosslinked polyolefin elastomers each comprise a first polyolefin having a density less than 0.86 g/cm 3 , a second polyolefin, a silane crosslinker, a grafting initiator, and a condensation catalyst.
  • Embodiment B is a method of making a roofing membrane, the method comprising: extruding a first silane-crosslinkable polyolefin elastomer to form a top layer; extruding a second silane-crosslinkable polyolefin elastomer to form a bottom layer; calendaring a scrim layer between the top and the bottom layers to form an uncured roofing membrane element; and crosslinking the silane-crosslinkable polyolefin elastomers of the top and the bottom layers in the uncured roofing membrane element at a curing temperature and a curing humidity to form the single ply roofing membrane, wherein the top and bottom layers of the single ply roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according to ASTM D 395 (22 hrs @ 70° C.).
  • Embodiment B wherein the first silane-crosslinkable polyolefin elastomer and the second silane-crosslinkable polyolefin elastomer are chemically distinct from each other.
  • Embodiment B or Embodiment B with any of the intervening features wherein the curing humidity is an ambient humidity.
  • first and second silane-crosslinkable polyolefin elastomers each comprise a first polyolefin having a density less than 0.86 g/cm 3 , a second polyolefin, a silane crosslinker, a grafting initiator, and a condensation catalyst.
  • Embodiment C is a method of making a high-load flame retardant thermoplastic polyolefin (TPO) roofing membrane, the method comprising: adding a silane-grafted polyolefin elastomer, a flame retardant, and a condensation catalyst to a reactive single screw extruder to produce a silane-crosslinkable polyolefin elastomer; calendaring the silane-crosslinkable polyolefin elastomer to form a top layer and a bottom layer; calendaring a scrim layer between the top and the bottom layers to form an uncured roofing membrane element; and crosslinking the silane-crosslinkable polyolefin elastomers of the top and the bottom layers in the uncured roofing membrane element at an ambient temperature and an ambient humidity to form the thermoplastic polyolefin (TPO) roofing membrane, wherein the top and bottom layers of the thermoplastic polyolefin (TPO) roofing membrane both exhibit a compression set of from about 5.0% to about 35.0%, as measured according
  • the silane-grafted polyolefin elastomer comprises a first polyolefin having a density less than 0.86 g/cm 3 , a second polyolefin, a silane crosslinker, a grafting initiator.
  • thermoplastic polyolefin (TPO) roofing membrane exhibits a weathering color difference of from about 0.25 ⁇ E to about 2.0 ⁇ E, as measured according to ASTM D2244.

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US11242684B2 (en) 2015-02-06 2022-02-08 Firestone Building Products Company, Llc Thermoplastic roofing membranes for fully-adhered roofing systems
US11555312B2 (en) 2015-12-31 2023-01-17 Holcim Technology Ltd Polyolefin thermoplastic roofing membranes with improved burn resistivity
US12044013B2 (en) 2015-12-31 2024-07-23 Holcim Technology Ltd Polyolefin thermoplastic roofing membranes with improved burn resistivity
CN111108630A (zh) * 2018-07-26 2020-05-05 株式会社Lg化学 交联的聚烯烃隔膜及其制造方法
US11718723B2 (en) 2018-07-26 2023-08-08 Lg Chem, Ltd. Crosslinked polyolefin separator and manufacturing method therefor
EP3849802A4 (fr) * 2018-09-13 2022-07-27 3M Innovative Properties Company Membrane polymère utile en tant que membrane de toiture commerciale
CN113614120A (zh) * 2018-10-02 2021-11-05 博里利斯股份公司 接枝塑性体的高速交联
US11981781B2 (en) 2018-10-02 2024-05-14 Borealis Ag High speed cross-linking of grafted plastomers
US11987986B2 (en) 2019-01-14 2024-05-21 Holcim Technology Ltd Multi-layered thermoplastic roofing membranes
US11987025B2 (en) 2019-02-10 2024-05-21 Holcim Technology Ltd Thermoplastic roofing membranes for fully-adhered roofing systems

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KR20200103852A (ko) 2020-09-02
KR102161086B1 (ko) 2020-10-05
JP7316408B2 (ja) 2023-07-27
EP3411438A1 (fr) 2018-12-12
US11684115B2 (en) 2023-06-27
CN109563329A (zh) 2019-04-02
JP6792645B2 (ja) 2020-11-25
MX2019006664A (es) 2019-10-09
EP3551453A1 (fr) 2019-10-16
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US20190029361A1 (en) 2019-01-31
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EP3551003A1 (fr) 2019-10-16

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