EP3601422A1 - Articles en polytétrafluoroéthylène expansé thermiquement isolants - Google Patents

Articles en polytétrafluoroéthylène expansé thermiquement isolants

Info

Publication number
EP3601422A1
EP3601422A1 EP18718277.9A EP18718277A EP3601422A1 EP 3601422 A1 EP3601422 A1 EP 3601422A1 EP 18718277 A EP18718277 A EP 18718277A EP 3601422 A1 EP3601422 A1 EP 3601422A1
Authority
EP
European Patent Office
Prior art keywords
thermally insulative
insulative material
expanded
aerogel
ptfe
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP18718277.9A
Other languages
German (de)
English (en)
Inventor
Greg D. D'arcy
James R. Hanrahan
Steven R. Alberding
Joseph W. Henderson
Kevin J. MABE
Anit Dutta
Gregory D. Culler
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.)
WL Gore and Associates Inc
Original Assignee
WL Gore and Associates 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.)
Filing date
Publication date
Priority claimed from US15/472,819 external-priority patent/US20170203552A1/en
Application filed by WL Gore and Associates Inc filed Critical WL Gore and Associates Inc
Publication of EP3601422A1 publication Critical patent/EP3601422A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2437/00—Clothing
    • B32B2437/02—Gloves, shoes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00—Containers; Receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00—Containers; Receptacles
    • B32B2439/70—Food packaging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00—Containers; Receptacles
    • B32B2439/80—Medical packaging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2509/00—Household appliances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/22—Expandable microspheres, e.g. Expancel®
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene

Definitions

  • the present disclosure relates generally to thermally insulative materials and articles thereof, and more specifically to thermally insulative materials containing thermally insulative particles, such as aerogel particles, a polymer matrix and
  • Insulation having larger pore sizes such as foam, batting, wool, and other common thermally insulating materials, has a thermal conductivity of about 40 mW/m K, which is higher than that of air due to the contribution of radiation and solid conduction. Aerogel powders and beads are known to have a thermal conductivity of about 9 to 20 mW/m K. However, such highly porous and low density material is not useful for many applications in the form of a powder due to the extensive dusting which makes
  • the methods often include the steps of pouring an aerogel precursor liquid into a mold, drying the aerogel liquid to form a highly porous gel structure with a variety of liquid exchanges, and using supercritical fluid extraction to form an aerogel monolith. Processes, such as those using supercritical fluid extraction, are very time consuming and expensive. Further, the structures produced are rigid and have low mechanical strength and have limited ability to be further molded or formed into desired shapes after the aerogel material is formed. These materials often crack or shatter upon flexing and are known for shedding or "dusting" of fine aerogel particles.
  • U.S. Patent Publication 2002/0094426 teach aerogel materials combined with a reinforcing structure, specifically a lofty fibrous batting.
  • the aerogel is reinforced by a fibrous batting structure in combination with randomly oriented microfibers and/or conductive layers.
  • an aerogel- forming precursor liquid is poured into the batting and supercritically dried to form an aerogel. It is taught that the resulting reinforced aerogel structure is drapable, less prone to shattering upon flexing and less prone to shedding of fine aerogel particles.
  • applications for such materials are limited due to a lack of moldability and formability of these structures, as well as the costs associated with supercritical extraction steps.
  • an aerogel composite material having a layer of fiber web and aerogel particles is preferably formed as a mat or panel.
  • the fiber web comprises a bicomponent fiber material of two firmly interconnected polymers having lower and higher temperature melting regions into which aerogel particles are sprinkled.
  • the fibers of the web are bonded to each other as well as to the aerogel particles.
  • the resulting composites are relatively stiff structures, and upon the application of mechanical stress, granules break or become detached from the fiber so that aerogel fragments may fall out from the web.
  • U.S. Pat. No. 7,118,801 to Ristic-Lehmann et al., teaches a material that is useful in multiple applications including insulation applications for garments, containers, pipes, electronic devices and the like.
  • the material of the '801 disclosure comprising aerogel particles and polytetrafluoroethylene (PTFE), is fbrmable, having low particle shedding and low thermal conductivity. Composites made from the material may be flexed, stretched, and twisted, with little or no shedding of aerogel particles or loss of conductive properties.
  • PTFE polytetrafluoroethylene
  • insulative material that overcomes problems inherent in aerogel powders and composites, such as the lack of formability of aerogel powder and the lack of flexibility of composites, as well as the shedding or dusting of aerogel particles upon application of mechanical stress.
  • insulative material which may be formed into articles (e.g., expanded PTFE articles) that are hydrophobic, highly breathable, possess high strength, and which may be used in non-static, highly flexible applications.
  • insulative articles which are flexible, stretchable, and bendable with little to no shedding or dusting of fine particles.
  • the present disclosure is directed, in one embodiment, to a thermally insulative material comprising an polymer matrix, aerogel particles and expanded microspheres; wherein the aerogel particles are present in an amount of 30% by weight or greater, the polymer matrix is present in an amount of greater than or equal to 20% by weight and the expanded microspheres are present in an amount of 0.5% to 15% by weight, wherein the percentages by weight are based on the total weight of the polymer matrix, the aerogel particles and the expanded microspheres; and wherein the thermal conductivity of the thermally insulative material is less than 40 mW/m K at atmospheric conditions.
  • the polymer matrix may comprise a
  • the thermally insulative material when tested according to a 3-second exposure to a vertical flame, exhibits no melting, no dripping and/or no burnthrough.
  • the thermally insulative material has a thermal conductivity of the matrix which is greater than 27 mW/m K and less than 39 mW/m K at atmospheric conditions.
  • the thermally insulative material is in the form of a sheet or a film, wherein the matrix further comprises one or more layers on the first side, the second side or both the first and the second side.
  • the one or more layers may comprise a polymer layer, a woven layer, a knit layer, a nonwoven layer or a combination thereof.
  • the one or more layers may comprise a
  • the one or more layers of the thermally insulative material may be adhered to the expanded polymer matrix using a continuous or discontinuous adhesive, and the adhesive optionally comprises a flame resistant material.
  • thermally insulative material comprising the thermally insulative material described.
  • such articles may include in certain embodiments, but not be limited to, a glove insulation insert, a footwear insulation insert, a garment, a garment insert, pipe insulation, cryogenic insulation, an electronic device, cookware, a home appliance, a storage container, a food package, a pharmaceutical package, an immersion suit, an acoustic insulation, a thermal insulation and an electrical insulation.
  • a thermally insulative material comprising an expanded PTFE (ePTFE) incorporating thermally insulative particles, said material having a thermal conductivity of less than or equal to 25 mW/m K at atmospheric conditions.
  • the thermally insulative material exhibits an endotherm at about 380°C.
  • the thermally insulative material is monolithic.
  • the thermally insulative material comprises an ePTFE having a tensile strength in the length direction of at least 0.35 MPa and a tensile strength in the transverse direction of at least 0.19 MPa.
  • the thermally insulative material may comprise less than 40% by weight thermally insulative particles and greater than 60% by weight
  • polytetrafluoroethylene ePTFE
  • said composite material has a thermal conductivity of less than or equal to 25 mW/m K at atmospheric conditions.
  • the thermally insulative material incorporates thermally insulative particles
  • the particles may be selected from silica aerogel particles, fumed silica, and combinations thereof.
  • the thermally insulative material comprises expanded PTFE having a node and fibril structure and having a thermal conductivity of less than or equal to 25 mW/m K at atmospheric conditions. Further, the insulative material may comprise an expanded PTFE which exhibits about a 380°C endotherm.
  • the disclosure is directed to an article comprising a first layer, an expanded PTFE (ePTFE) having a thermal conductivity of less than or equal to 25 mW/m K at atmospheric conditions; and a second layer, wherein said ePTFE is sandwiched between said first and said second layers.
  • ePTFE expanded PTFE
  • the ePTFE is hydrophobic.
  • at least one of said first and said second layer may be impermeable to gases.
  • at least one of said first and said second layer may be impermeable to liquids.
  • the ePTFE comprises thermally insulative particles selected from silica aerogel and fumed silica.
  • FIG. 1 is a scanning electron micrograph of the surface of a thermally insulative material comprising an ePTFE material including 20% aerogel loading taken at 5000x magnification;
  • FIG. 2 is a scanning electron micrograph of the surface of a thermally insulative material comprising an ePTFE material including 40% aerogel loading taken at 5000x magnification;
  • FIG. 3 is a scanning electron micrograph of the surface of a thermally insulative material comprising an ePTFE material including fumed silica taken at 5000x
  • FIG. 4 is scanning electron micrograph of the surface of a thermally insulative material comprising an ePTFE material including 60% aerogel loading taken at 5000x magnification.
  • the insulative material of the present disclosure includes thermally insulative particles, such as aerogels and the like, and a polymer matrix.
  • the polymer matrix can be, for example, a fluoropolymer, a polytetrafluoroethylene (PTFE), an ultrahigh molecular weight polyethylene (UHMWPE), a polyolefin, a polyurethane or a combination thereof.
  • PTFE polytetrafluoroethylene
  • UHMWPE ultrahigh molecular weight polyethylene
  • the polymer matrix is a fluoropolymer matrix
  • UHMWPE ultrahigh molecular weight polyethylene
  • the thermally insulative material may be formed into articles (e.g., ePTFE membranes, composites, etc.) that are hydrophobic, highly breathable, possess high strength, and which may be used in non-static, or dynamic flexing, applications. Articles produced from the thermally insulative materials are flexible, stretchable, and bendable. Also, the thermally insulative material has little to no shedding or dusting of fine particles.
  • Aerogel particles having a particle density of less than about 100 kg/m 3 and a thermal conductivity of less than or equal to about 15 mW/m K at atmospheric conditions (about 298.5 K and 101.3 kPa) may be used in the insulative material. It is to be understood that the term "aerogel(s)" and “aerogel particles” are used interchangeably herein.
  • Aerogels are thermal insulators which significantly reduce convection and conductive heat transfer.
  • Silica aerogel particles are particularly good conductive insulators. Aerogel particles are solid, rigid, and dry materials, and may be commercially obtained in a powdered form. For example, a silica aerogel formed by a relatively low cost process is described by Smith et al. in U.S. Pat. No. 6,172,120. The size of the aerogel particles can be reduced to a desired dimension or grade by jet-milling or other size reduction techniques.
  • Aerogel particles for use in the insulative material may have a size from about 1 ⁇ m to about 1 mm, from about 1 ⁇ m to about 500 ⁇ m, from about 1 ⁇ m to about 250 ⁇ m, from about 1 ⁇ m to about 200 ⁇ m, from about 1 ⁇ m to about 150 ⁇ m, from about 1 ⁇ m to about 100 ⁇ m, form about 1 ⁇ m to about 75 ⁇ m, from about 1 to about 50 ⁇ m, from about 1 ⁇ m to about 25 ⁇ m, from about 1 ⁇ m to about 10 ⁇ m, or from about 1 ⁇ m to about 5 ⁇ m.
  • the aerogel particles have a size from about 2 ⁇ m to about 24 ⁇ m.
  • aerogels having smaller particle sizes for example, an average particle size of less than or equal to about 200 nm, or even 100 nm, may be used in the insulative material.
  • the density of the aerogel particle may be less than 100 kg/m 3 , less than 75 kg/m 3 , less than 50 kg/m 3 , less than 25 kg/m 3 or less than 10 kg/m 3 .
  • the aerogel particles have a bulk density from about 30 kg/m 3 to about 50 kg/m 3 .
  • Aerogels suitable for use in the insulative material include both inorganic aerogels, organic aerogels, and mixtures thereof.
  • suitable inorganic aerogels include those formed from an inorganic oxide of silicon, aluminum, titanium, zirconium, hafnium, yttrium, and vanadium.
  • Suitable organic aerogels for use in the insulative material include, but are not limited to, aerogels be prepared from carbon, polyacrylates, polystyrene, polyacrylonitriles, polyurethanes, polyimides, polyfurfural alcohol, phenol furfuryl alcohol, melamine formaldehydes, resorcinal formaldehydes, cresol, formaldehyde, polycyanurates, polyacrylamides, epoxides, agar, and agarose.
  • the insulative material contains an inorganic aerogel such as a silica.
  • Another example of a thermally insulative particle suitable for the present disclosure is fumed silica.
  • the aerogels used in the insulative material may be hydrophilic or hydrophobic.
  • the aerogels are hydrophobic to partially hydrophobic and have a thermal conductivity of less than about 15 mW/m K. It is to be appreciated that particle size reduction techniques, such as milling, may affect some of the external surface groups of hydrophobic aerogel particles, which results in partial surface hydrophilicity (hydrophobic properties are retained within the aerogel particle). Partially hydrophobic aerogels may exhibit enhanced bonding to other compounds and may be utilized in applications where bonding is desired.
  • the thermally insulative material of the present disclosure further comprises a polymer matrix or an expanded polymer matrix, wherein the polymer matrix is a fluoropolymer, a polytetrafluoroethylene, an expanded polytetrafluoroethylene, an ultrahigh molecular weight polyethylene (UHMWPE), an expanded ultrahigh molecular weight polyethylene, a polyolefin, an expanded polyolefin, a polyurethane or a combination thereof.
  • UHMWPE ultrahigh molecular weight polyethylene
  • an ultrahigh molecular weight means a polymer having a number average mo!ecuiar weight in the range of from 3,000,000 to 10.000,000 g/moi.
  • the polymer matrix can be produced from polytetrafluoroethyiene (PTFE) particles.
  • PTFE particles have a size smaller than the aerogel particles.
  • PTFE particles having a size similar to the aerogel particles may be used.
  • the PTFE is present as primary particles that have a size of about 50 nm or greater or PTFE aggregates having a size of about 600 ⁇ or less in a dispersion.
  • the PTFE dispersion is an aqueous colloidal dispersion of high molecular weight PTFE particles formed by emulsion polymerization.
  • the PTFE dispersion may have a SSG of about 2.2 or less.
  • the thermally insulative material is formed by preparing a mixture of aerogel and PTFE particles, such as, for example, by forming a mixture of an aqueous dispersion of aerogel particles and a PTFE dispersion.
  • the aerogel/PTFE particle mixture may include, by weight, less than about 90% aerogel particles, less than about 85% aerogel particles, less than about 80% aerogel particles, less than about 75% aerogel particles, less than about 70% aerogel particles, less than about 65% aerogel particles, less than about 60% aerogel particles, less than about 55% aerogel particles, or less than about 50% aerogel particles.
  • the aerogel particles are present in the mixture in an amount less than 40%, less than or equal to 35%, less than or equal to 30%, less than or equal to 25%, less than or equal to 20%, less than or equal to 15%, or less than or equal to 10%.
  • the aerogel particles may be present in the mixture an amount from about 10% to 40%. In exemplary embodiments, the aerogel particles may be present in an amount less than 40%.
  • the aerogel/PTFE particle mixture may contain, by weight, greater than about 10% PTFE particles, greater than about 15% PTFE particles, greater than about 20% PTFE particles, greater than about 25% PTFE particles, greater than about 30% PTFE particles, greater than about 35% PTFE particles, greater than about 40% PTFE particles, greater than about 45% PTFE particles, or greater than about 50% PTFE particles.
  • the PTFE particles are present in the mixture in an amount greater than or equal to 60%, greater than or equal to 65%, greater than or equa! to 70%, greater than or equal to 75%, or greater than or equal to 80%.
  • the PTFE particles may be present in an amount from about 60% to 90%. in exemplary embodiments, the PTFE particles may be present in the aerogel/PTFE particle mixture in an amount greater than 60%.
  • Properties such as thermal conductivity, dusting, formability and strength may be tailored in part by varying the ratio of the weight percentage of aerogel to PTFE in the mixture.
  • thermally insulative material of the present disclosure may optionally comprise additional components.
  • Optional components may be added to the
  • aerogel/PTFE binder mixture such as finely dispersed opacifiers to reduce radiative heat transfer and improve thermal performance, and include, for example, carbon black, titanium dioxide, iron oxides, silicon carbide, molybdenum silicide, manganese oxide, polydialkylsiloxanes wherein the alkyl groups contain 1 to 4 carbon atoms, flame retardant materials or a combination thereof.
  • polymers, dies, plasticizers, thickeners, various synthetic and natural fibers are optionally added, for example, to increase mechanical strength and to achieve properties such as color and thermal stability, elasticity and the like.
  • Optional components are preferably added at less than about 10% of the aerogel PTFE mixture.
  • the thermally insulative material additionally include expandable microspheres such as Expancel, expandable microspheres. It is envisioned that other materials, expandable spheres, or foaming agents may be used to expand the thermally insulative material into a foamed material.
  • the thermally insulative material containing expandable microspheres is co-coagulated and formed into a tape as described below. The tape may then be heated to a temperature sufficient to expand the microspheres, causing the tape to expand into a foamed insulating material. The amount of expandable microspheres and the processing temperature can affect the thickness of the final product.
  • a tape containing about 10 percent by weight of expandable microspheres and having a thickness of about 1 millimeter can be expanded to give a thermally insulative material having a thickness of up to about 8 millimeters or more.
  • a thermally insulative material having a thickness of up to about 8 millimeters or more.
  • heating and expansion may result in a foamed thermally insulative material that is 4 mm thick.
  • the foamed thermally insulative material is pliable and compressible with substantially full recovery.
  • the foamed thermally insulative material has a low density, for example, a density of less than 0.5 g/cm 3 , or less than 0.4 g cm 3 , or less than 0.3 g/cm 3 or less than 0.2 g/cm 3 or less than 0.1 g/cm 3 .
  • the thermally insulative material comprises a polymer matrix, aerogel particles and expanded microspheres.
  • the thermally insulative material may consist essentially of, or may consist of a polymer matrix, aerogel particles and expanded microspheres.
  • the expandable microspheres can be present in an amount in the range of from about 0.5% to 15% by weight, based on the total weight of the aerogel particles, the PTFE particles and the expandable microspheres.
  • the expandable microspheres can be present at greater than about 0.5% by weight and up to 14, 13, 12, 11 , 10, 9, 8, 7, 6, 5, 4, 3, 2 or 1 % by weight.
  • the expandable microspheres are present in the range of from about 5 to 14% or 6% to 13%, wherein all percentages by weight are based on the total amount of the polymer matrix, the aerogel particles and the
  • the mixture of aerogel and PTFE particles in a carrier liquid may be co-coagulated, such as by coagulating the mixture by agitation or by the addition of coagulating agents.
  • the co- coagulated mixture contains a substantially uniform blend of aerogel particles and PTFE particles.
  • the co-coagulated mixture may be at least partially dried (e.g., in an oven) and compressed into a preform.
  • the preform may then be extruded into a tape, calendered to a desired thickness, and expanded (uniaxiaily or biaxially) into a thermally insulative expanded PTFE (ePTFE) material.
  • ePTFE thermally insulative expanded PTFE
  • a mixture of aerogel particles, the polymer matrix, for example, PTFE particles and expandable microspheres in the carrier liquid can be co-coagulated, by agitation or by the addition of coagulating agents.
  • the co-coagulated mixture contains a substantially uniform blend of aerogel particles, polymer matrix particles and expandable microspheres.
  • This mixture can be at least partially dried, for example, in an oven and compressed into a preform.
  • the preform may then be extruded into a tape, calendered to a desired thickness and expanded (uniaxiaily or biaxially) into the thermally insulative material.
  • the process of uniaxiaily or biaxially expanding the tape is typically preformed at elevated temperatures, for example, above the temperature at which the expandable microspheres expand.
  • the expansion of the expandable microspheres can result in the formation of the expanded microsphere wherein less than complete expansion of the expandable microspheres, full expansion of the expandable microspheres, rupture of the expandable microspheres or a combination thereof.
  • the resulting material is thermally insulative with a thermal conductivity (k) of less than or equal to 40, 39, 38, 37, 36, 35, 34, 33, 32, 31 , 30, 29, 28, 27, 26, 25, 24, 23, 22 or 21 mW/m-K, less than or equal to 20 mW/m-K, or less than or equal to 15 mW/m-K, all at atmospheric conditions, that is, 298 K and 101.3 kPa.
  • the ePTFE has a node and fibril structure as can be seen in FIGS. 1-4. Also, the ePTFE demonstrates high tensile strength in the length and transverse directions.
  • the ePTFE has high breathability, with an MVTR of at least 5,000 g/m 2 /24 hours, at least 10,000 g/m 2 /24 hours, at least 20,000 g/m 2 /24 hours, or at least 30,000 g m 2 /24 hours or greater.
  • breathable is meant to describe an article with a breathability of at least 5,000 g/m /24 hours.
  • a thermally insulative material comprising an expanded polymer matrix, aerogel particles and expanded microspheres wherein the aerogel particles are present in an amount of 30% by weight or greater, the expanded polymer matrix in an amount of greater than or equal to 20% by weight and the expandable microspheres in an amount of 0.5% to 15% by weight can produce a thermally insulative material that when tested according to a 3-second exposure to a vertical flame test (described below), exhibits no melting, no dripping and/or no bumthrough.
  • the fiammability test method is described below and is based on Federal Standard 191 A Method 5903.
  • the thermally insulative material that is flame resistant comprises an expanded polytetrafluoroethylene matrix, aerogel particles and expanded microspheres, wherein the thermally insulative material is free from any an added flame retardant material.
  • flame resistant means that the thermally insulative material when tested according to the fiammability test method below, resists melting, dripping, bumthrough or a combination thereof.
  • the thermally insulative material can optionally be laminated or adhered or otherwise bonded to one or more additional layers to form an article.
  • the thermally insulative material is typically in the form of a sheet or a film having a first side and a second side, wherein the thickness is less than the width and/or length directions.
  • One or more layers can be adhered to the first side, to the second side or to both the first and the second side of the thermally insulative material.
  • the one or more additional layers can be a polymer layer, a woven layer, a knit layer, a nonwoven layer or a combination thereof.
  • the polymer layer can be a nonporous layer, a microporous layer, a breathable layer or a combination thereof.
  • the one or more layers may be a fluoropolymer, a PTFE, a polyolefin, an expanded fluoropolymer, an
  • the one or more layers can be adhered to the thermally insulative material using an adhesive, welding, calendering, coating or a combination thereof.
  • the thermally insulative material can have an expanded
  • the article can comprise multiple layers, for example, the thermally insulative material can have a layer of expanded PTFE bonded to one or both sides, resulting in a composite material having a 2-layer or a 3-iayer structure.
  • One or more additional textile layers for example, a woven, a knit, a non-woven or a combination thereof, may be adhered to the composite material.
  • textile layers can be adhered using an adhesive material.
  • the adhesive may be applied to the thermally insulative material, to the textile or to both in a continuous or a discontinuous manner, as is known in the art.
  • the adhesive may optionally comprise a flame resistant material.
  • the one or more textile layers can be a woven, a knit, a nonwoven or a combination thereof.
  • the woven, knit or nonwoven textiles can be flame resistant woven, flame resistant knit or flame resistant nonwoven textiles.
  • Suitable textile layers are well known in the art and can include elastic and non-elastic textiles, for example, LYCRA®, polyurethane, polyester, polyamide, acrylic, cotton, wool, silk, linen, rayon, flax, jute; flame resistant textiles, for example, NOMEX® aramid (available from Du Pont, Wilmington, DE), aramids, flame resistant cotton,
  • polybenzim idazole poly p-phenyiene-2,6 ⁇ bezobisoxazole, flame resistant rayon, modacrylics, modacrylic blend, polyamine, carbon, fiberglass or a combination thereof.
  • the thermally insulative ePTFE material is used as insulation in a footwear article.
  • the ePTFE material may be used in any portion of the footwear article, including the upper portion, heel portion, toe portion, or sole (bottom) portion.
  • the foamed thermally insulative material may be used as insulation in a footwear article.
  • the foamed thermally insulative material may be utilized in the upper portion, heel portion, toe portion, and/or sole (bottom) portion.
  • an insulated footwear article includes at least one thermally insulative ePTFE material in the upper portion of the footwear article and a foamed thermally insulative material in the sole (bottom) portion of the footwear article.
  • footwear article is meant to include shoes and boots.
  • formable, moldable, low dusting materials with low thermal conductivity are considered to be within the purview of the disclosure. These materials are sufficiently moldable to be formed into flexible three-dimensional structures or shapes having curves in one or more directions. Further, the materials optionally form stretchable structures with minimal dusting upon stretching. T ey may be wrapped around a tube or pipe for insulation.
  • thermally insulative materials described herein may be used in numerous applications, including insulating materials and composites made therefrom for use in apparel, such as glove and footwear insulation inserts, garments, and inserts for garments, pipe insulation, cryogenic insulation, electronic devices, cookware, home appliances, storage containers and packaging of food and pharmaceuticals, immersion suits, as well as dual function insulation, such as acoustic insulation, electrical insulation, thermal insulation, and the like.
  • the MVTR for each sample fabric was determined in accordance with the general teachings of ISO 15496 except that the sample water vapor transmission (VWP) was converted into MVTR moisture vapor transmission rate (MVTR) based on the apparatus water vapor transmission (VWPapp) and using the following conversion.
  • the specimens were conditioned at 73.4 ⁇ 0.4° F and 50 ⁇ 2% relative humidity (rH) for 2 hrs prior to testing and the bath water was a constant 73.4° F ⁇ 0.4° F.
  • the larger dimension of the sample was oriented in the machine, or "down web,” direction.
  • the larger dimension of the sample was oriented perpendicular to the machine direction, also known as the "cross web” direction.
  • the thickness of the samples was then measured using a Mitutoyo 547-400 Absolute snap gauge. The samples were then tested individually on the tensile tester. Three different sections of each sample were measured. The average of the three maximum load (i.e., the peak force) measurements was used.
  • Sample thickness was measured with the integrated thickness measurement of the thermal conductivity instrument. (Laser Comp Model Fox 314 Laser Comp Saugus, MA). The results of a single measurement was recorded.
  • Thermal Conductivity Measurement (Under Compression) Thermal conductivity of samples of the present disclosure was measured using a custom-made heat flow meter thermal conductivity tester following the general teachings of ASTM C518 plus the addition of compression at atmospheric conditions (about 298 K and 101.3 kPa).
  • the tester consisted of a heated aluminum plate with a heat flow sensor (Model FR-025-TH 4033, Concept Engineering, Old Saybrook, CT) and a temperature sensor (thermistor) imbedded in its surface, and a second aluminum plate maintained at room temperature, also with a temperature sensor imbedded in its surface.
  • the temperature of the heated plate was maintained at 303.15 K while the temperature of the "cold" plate was kept at 298.15 K.
  • the diameter of the plates was about 10 cm.
  • the sample was compressed by applying weights to a pivoting arm connected to the lower plate.
  • the thickness of the samples under compression was measured by a digital encoder which was calibrated with metal shims which were measured using a digital micrometer (model ID-F125E, Mitutoyo Corp., Japan).
  • the heat flow measurement was normally obtained within about two to five minutes after the sample was placed in the tester upon reaching a steady state.
  • Thermal conductivity was also measured without compressing the sample.
  • the samples were measured with a Laser Comp Model Fox 314 thermal conductivity analyzer. (Laser Comp Saugus, MA). The results of a single measurement was recorded.
  • Water entry pressure provides a test method for water intrusion through membranes and/or fabrics.
  • a test sample is clamped between a pair of testing plates taking care not to cause damage.
  • the lower plate has the ability to pressurize a section of the sample with water.
  • a piece of paper towel is placed on top of the sample between the plate on the non-pressurized side as an indicator of evidence for water entry.
  • the sample is then pressurized in small increments until the first visible sign of water through the paper towel indicates breakthrough pressure or entry pressure. The pressure was recorded as the water entry pressure. The results of a single test sample is clamped between a pair of testing plates taking care not to cause damage.
  • the lower plate has the ability to pressurize a section of the sample with water.
  • a piece of paper towel is placed on top of the sample between the plate on the non-pressurized side as an indicator of evidence for water entry.
  • the sample is then pressurized in small increments until the first visible sign of water through the paper towel indicates breakthrough pressure or entry pressure.
  • Samples of the thermally insulative material having a size of about 75 millimeter (mm) by 200mm were conditioned at 21 °C and 50% ⁇ 2% relative humidity for 2 hours prior to testing.
  • the conditioned samples were placed in sealed sample bags after conditioning until they were removed for testing.
  • aforementioned burner and sample holder were located inside of the flame cabinet.
  • the sample was placed horizontally on the sample holder and held in place using medium size binder clips.
  • the laboratory hood airflow was set to low.
  • the burner was positioned away from the sample holder in the flame cabinet.
  • the needle valve was closed and the supply valve opened.
  • the needle valve was opened and the burner lit.
  • the flame height was adjusted to 75mm.
  • the burner was allowed to bum for 1 minute and flame height readjusted, if necessary.
  • the burner was then moved under the specimen, placing the flame as close to the center of the sample as possible, and a timer started for 3 seconds.
  • the burner was moved out from under the specimen, if the sample does not burn or goes out immediately upon removal of the flame, the timer was stopped. If the sample burns, the timer was allowed to continue until the flame extinguished. In order to determine the afterflame time, 3 seconds was subtracted from the timer measured time and the result recorded. Any melting, dripping, or hole formation was also recorded. Hole formation either through ablation or burning is known as burn through and was also recorded. Melting, Dripping or burn-through constituted the test sample to fail the test.
  • PTFE 601 commercially available from E. I. DuPont de Nemours, Inc., Wilmington, DE
  • Aerogel Enova Aerogel MT 1200, Cabot, Boston, MA
  • the PTFE and Aerogel were co-coagulated in the following manner. 91 grams of Hexanol (PN H13303- L, Sigma-Aldrich, St Louis, MO) was added to 14.4 Kg of water and mixed for 1 minute in a Silverson Model EX60 mixer (Silverson
  • the wet tape was calendered to a thickness of 2.2 mm and dried in a forced air oven set to 150°C for 4 minutes and then at 250°C for an additional 4 minutes.
  • the dried, calendered tape was then biaxially expanded simultaneously in both directions in the following manner: expansion ratio of 8:1 , in the length direction and 18:1 in the transverse direction at a rate of 500%/sec at 260°C.
  • the resulting thermally insulating ePTFE membrane had the following properties: tensile strength in the length and transverse directions: 1.54 MPa and 1.53 MPa, respectively ; thickness: 0.36 mm; thermal conductivity without compression: 21 mW/m- K; thermal conductivity at 5 psi compression: 8.9 mW/m-K; MVTR (MDM): 32508 g/m 2 /24 hours: Gurley Number: 0.7 sec; ATEQ airflow: 6.2 1/hr-cm 2 at 4.5 mBar pressure drop; and Water Entry Pressure (WEP): 29 psi.
  • SEM scanning electron micrograph
  • a thermally insulating ePTFE membrane was made as follows. A dispersion form of PTFE 601 (commercially available from E. I. DuPont de Nemours, Inc., Wilmington, DE) and Aerogel (Enova Aerogel MT 1200, Cabot, Boston, MA) were obtained. The PTFE and Aerogel were co-coagulated in the following manner. 136 grams of Hexanol was added to 15.1 Kg of water and mixed for 1 minute with an impeller speed of 1500 rpm. The speed was slowed to 500 rpm and 363 grams of silica aerogel was slowly added. Mixing continued until the aerogel was fully wet-out (approximately 6-10 minutes).
  • the wet tape was calendered to a thickness of 2.2 mm and dried in a forced air oven set to 150°C for 4 minutes and then 250°C for an additional 4 minutes.
  • the dried, calendered tape was then biaxially expanded in both directions simultaneously in the following manner: expansion ratio of 3:1 , in the longitudinal direction and 6:1 in the transverse direction at a rate of 500%/sec at 250°C.
  • the resulting thermally insulating ePTFE membrane had the following properties: tensile strength in the length and transverse directions, respectively: 0.59 MPa and 0.7 MPa, respectively; thickness: 0.86 mm; thermal conductivity without compression: 21 mW/m-K; thermal conductivity at 5 psi compression: 10 mW/m-K; MVTR (MDM): 9798 g/m 2 /24 hours; Gurley Number: 1.4 sec; ATEQ airflow: 2.71/hr-cm 2 at 4.5 mBar pressure drop; and Water Entry Pressure (WEP): 34 psi.
  • SEM magnification scanning electron micrograph
  • PTFE 601 commercially available from E. I. DuPont de Nemours, Inc., Wilmington, DE
  • fumed silica Aerosil R812, Evonik Industries AG, Hanau Germany
  • the PTFE and fumed silica were co-coagulated in the following manner. 280 grams of Hexanol were added to 23 Kg of water and mixed for 1 minute at an impeller rate of 1500 rpm. The impeller rate was decreased to 500 rpm and 750 grams of fumed silica was slowly added. Mixing continued for 15 minutes. 4.4 Kg of PTFE dispersion was then added and the mixer speed was increased to 1500 rpm for 3.33 minutes.
  • the resulting coagulum was dewatered using a Reemay sheet and then dried for 24 hours at 165°C in a hot air oven. [0077] The resulting dry coagulum was then blended with 95 wt % ISOPAR K and 5% lauric acid (PN L556, Sigma Aldrich, St Louis, MO) at 1.1 kg/kg and subsequently compressed into a cylindrical perform. The preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.4 mm thick.
  • the wet tape was calendered to a thickness of 2 mm and dried in a forced air oven set to 250°C.
  • the resulting thermally insulating ePTFE membrane had the following properties: tensile strength in the length and transverse directions: 0.35 MPa; and 0.19 MPa, respectively; thickness: 0.86 mm; thermal conductivity without compression: 23 mW/m- K; and thermal conductivity at 5 psi compression: 16 mW/m-K.
  • SEM scanning electron micrograph
  • a dispersion form of PTFE 601 (commercially available from E.I. DuPont de Nemours, Inc., Wilmington, DE) and Aerogel (Enova Aerogel MT 1200, Cabot, Boston, MA) were obtained.
  • the resulting coagulum was dewatered through a Reemay sheet (item#2014-686, Reemay, Old Hickory TN) and then dried for 24 hours at 165°C in a forced air oven. [0082] The resulting dry coagulum was then blended with ISOPAR K (1.5 kg/kg) and subsequently compressed into a cylindrical preform. The preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.7 mm thick.
  • the wet tape was calendered to a thickness of 2.2 mm and dried in a forced air oven set to 150°C for 4 minutes and then 250°C for an additional 4 minutes.
  • the dried, calendered tape was then biaxially expanded simultaneously in both directions in the following manner: expansion ratio of 4:1 , in the length direction and 6:1 in the transverse direction at a rate of 500%/sec at 250°C.
  • the resulting thermally insulating ePTFE membrane had the following properties: tensile strength in the length and transverse directions: 0.7 MPa and 0.27 MPa, respectively; thickness: 1.1 mm; thermal conductivity without compression: 22 mW/m K; thermal conductivity at 5 psi compression: 12.2 mW/m K; Gurley Number: 0.7 sec;
  • a comparative thermally insulative material was produced using PVOH as the polymer matrix.
  • 50 grams (g) of unexpended Expancel 951 DU 120 manufactured by Akzo Nobel, NV, Amsterdam, Netherlands was combined with 50g of ENOVA® MT1200 aerogel particles manufactured by Cabot Corporation, Boston, Massachusetts in a 4 liter plastic tub.
  • the PVOH and water admixture was then poured into the plastic tub containing the aerogel and Expancel particles.
  • the tub was sealed and mixed by tumbling until it reached the consistency of stiff whipped cream.
  • a PTFE release material was then placed on a table and dusted lightly with ENOVA® MT1200 aerogel particles to prevent sticking and a golf ball sized aliquot of the aerogel/Expancel/PVOH mixture was placed on the release material and rolled into a disc approximately 3mm thick and 150mm in diameter using a 90mm diameter cardboard tube wrapped with PTFE release material. This disk forming process was repeated on a second sample and the resulting discs along with the release material were placed in a 150°C oven for approximately 30 minutes (min), initiating Expancel expansion, then moved to a 100°C oven and allowed to completely dry overnight The resulting material had a thickness of 6.58 mm.
  • a thermally insulative material was made as follows. A dispersion of PTFE 601 (commercially available from E. I. DuPont de Nemours, Inc., Wilmington, Delaware) and Aerogel (ENOVA® MT 1200 aerogel, Cabot, Boston, Massachusetts) were co- coagulated in the following manner. 308g of hexanol was added to 23.9 kilograms (kg) of water and mixed for 1 minute with an impeller speed of 1500 rpm. The speed was slowed to 500 rpm and 817g of the ENOVA® aerogel particles were slowly added. The mixing was continued until the aerogel particles were fully wet-out (approximately 6-10 minutes).
  • the resulting dry coagulum was then blended with ISOPAR K at a ratio of 1.04kg/kg and subsequently compressed into a cylindrical perform.
  • the preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.7 mm thick.
  • the wet tape was calendered to a thickness of 0.78mm and dried in a forced air oven set to a temperature of 150°C for 4 minutes and then 190°C for an additional 4 minutes.
  • the final drying step caused the Expancel to expand. This enlargement caused the dried, calendered tape to biaxially expanded in both directions simultaneously.
  • the thermally insulative material had a thickness of 2.25mm, a thermal conductivity without compression of XX mW/mK; an MVTR of 3086 g/m 2 /24 hours.
  • the resulting dry coagulum was then blended with ISOPAR K at a ratio of 1.04kg/kg and subsequently compressed into a cylindrical perform.
  • the preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.7 mm thick.
  • the wet tape was calendered to a thickness of 0.78 mm and dried in a forced air oven set to 150°C for 4 minutes and then 190°C for an additional 4 minutes.
  • the final drying step caused the Expancel to expand. This enlargement caused the dried, calendered tape to biaxially expanded in both directions simultaneously.
  • the thermally insulative material had a thickness of 1.25mm, a thermal conductivity without compression of XX mW/mK; an MVTR of 4475 g/m 2 /24 hours.
  • the resulting dry coagulum was then blended with ISOPAR K at a ratio of 1.04kg/kg and subsequently compressed into a cylindrical perform.
  • the preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.7 mm thick.
  • the wet tape was calendered to a thickness of 0.78 mm and dried in a forced air oven set to 150°C for 4 minutes and then 190°C for an additional 4 minutes.
  • the final drying step caused the Expancel to expand. This enlargement caused the dried, calendered tape to biaxially expanded in both directions simultaneously.
  • the thermally insulative material had the following properties; thickness: 3.37 mm; thermal conductivity without compression: xx mW/m-K; MVTR (MDM): 3271 g m 2 24 hours.
  • the resulting dry coagulum was then blended with ISOPAR K at a ratio of 1.04kg/kg and subsequently compressed into a cylindrical perform.
  • the preform was then extruded through a barrel to provide a wet tape 15.2 cm wide and 3.7 mm thick.
  • the wet tape was calendered to a thickness of 0.78 mm and dried in a forced air oven set to 150°C for 4 minutes and then 190°C for an additional 4 minutes.
  • the final drying step caused the expancel to expand. This enlargement caused the dried, calendered tape to biaxially expanded in both directions simultaneously.
  • the resulting thermally insulative material had the following properties; thickness: 1.1 mm; thermal conductivity without compression: xx mW/m-K; MVTR (MDM): 1990 g/m 2 /24 hours.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Thermal Insulation (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne des matériaux et des articles thermiquement isolants. Selon un mode de réalisation, un matériau thermiquement isolant comprend une matrice polymère, des particules d'aérogel et des microsphères expansées, les particules d'aérogel étant présentes en une quantité supérieure ou égale à 30 % en poids, la matrice polymère étant présente en une quantité supérieure ou égale à 20 % en poids et les microsphères expansées étant présentes en une quantité de 0,5 % à 15 % en poids, les pourcentages étant basés sur le poids total de la matrice polymère, des particules d'aérogel et des microsphères expansées, et la conductivité thermique du matériau thermiquement isolant étant inférieure à 40 mW/m K à des conditions atmosphériques.
EP18718277.9A 2017-03-29 2018-03-27 Articles en polytétrafluoroéthylène expansé thermiquement isolants Withdrawn EP3601422A1 (fr)

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US15/472,819 US20170203552A1 (en) 2013-12-19 2017-03-29 Thermally Insulative Expanded Polytetrafluoroethylene Articles
PCT/US2018/024417 WO2018183225A1 (fr) 2017-03-29 2018-03-27 Articles en polytétrafluoroéthylène expansé thermiquement isolants

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WO2020117932A1 (fr) * 2018-12-05 2020-06-11 W. L Gore & Associates, Inc, Gant
RU2709129C1 (ru) * 2019-08-15 2019-12-16 Общество с ограниченной ответственностью "Научно-исследовательский центр "Современные полимерные материалы" Порошковый форполимер термокомпрессионного синтактического пенопласта
JP6782478B1 (ja) * 2020-03-10 2020-11-11 株式会社コゼットクリエーション エアロゲル含有高通気性積層シート
CN112617330A (zh) * 2020-12-17 2021-04-09 恒劢安全防护用品（南通）有限公司 一种红外隐形手套的制备方法
WO2022261579A1 (fr) * 2021-06-11 2022-12-15 W. L. Gore & Associates, Inc. Composites isolants à haute température et articles associés
CN113402766B (zh) * 2021-06-22 2023-01-10 成都希瑞方晓科技有限公司 一种膨体聚四氟乙烯材料及其制备方法
JP2023090369A (ja) * 2021-12-17 2023-06-29 アクア株式会社 断熱材及びそれを用いた冷蔵庫、冷凍冷蔵庫、または冷凍庫

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EP0799343B1 (fr) 1994-12-21 2000-03-22 Cabot Corporation Materiau composite non-tisse-aerogel contenant des fibres a deux composants, son procede de fabrication et son utilisation
US6172120B1 (en) 1997-04-09 2001-01-09 Cabot Corporation Process for producing low density gel compositions
CN1306993C (zh) 2000-12-22 2007-03-28 思攀气凝胶公司 带有纤维胎的气凝胶复合材料
ATE365071T1 (de) * 2002-05-15 2007-07-15 Cabot Corp Zusammensetzung auf basis von aerogel, hohlen partikeln und binder, hergestelltes dämmmaterial und herstellungsverfahren
US7118801B2 (en) 2003-11-10 2006-10-10 Gore Enterprise Holdings, Inc. Aerogel/PTFE composite insulating material
CN105753388A (zh) * 2009-04-27 2016-07-13 卡博特公司 气凝胶组合物及其制造和使用方法
US20130344279A1 (en) * 2012-06-26 2013-12-26 Cabot Corporation Flexible insulating structures and methods of making and using same
CA2934539A1 (fr) * 2013-12-19 2015-06-25 W.L. Gore & Associates, Inc. Articles en polytetrafluoroethylene expanse thermiquement isolants

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