EP2041211A1 - Mousses de polymère contenant du nano-graphite multifonctionnel stratifié - Google Patents

Mousses de polymère contenant du nano-graphite multifonctionnel stratifié

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Publication number
EP2041211A1
EP2041211A1 EP06800020A EP06800020A EP2041211A1 EP 2041211 A1 EP2041211 A1 EP 2041211A1 EP 06800020 A EP06800020 A EP 06800020A EP 06800020 A EP06800020 A EP 06800020A EP 2041211 A1 EP2041211 A1 EP 2041211A1
Authority
EP
European Patent Office
Prior art keywords
graphite
polymer
nano
foam
hfc
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Withdrawn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
EP06800020A
Other languages
German (de)
English (en)
Inventor
Roland R. Loh
Mark E. Polasky
Joseph P. Rynd
Kurt W. Koelling
Bharat Patel
Manoj K. Choudhary
Yadollah Dellaviz
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.)
Owens Corning Intellectual Capital LLC
Original Assignee
Owens Corning Intellectual Capital LLC
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
Application filed by Owens Corning Intellectual Capital LLC filed Critical Owens Corning Intellectual Capital LLC
Publication of EP2041211A1 publication Critical patent/EP2041211A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/143—Halogen containing compounds
    • C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
    • 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
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
    • C08J2201/03—Extrusion of the foamable blend

Definitions

  • the present invention relates to rigid foamed polymeric boards containing nano- graphite. More particularly, it relates to rigid foamed polymeric board wherein nano-graphite is added to provide benefits as a process aid, an R-value enhancer, UV radiation stability enhancer, a dimensional stability enhancer, a mechanical strength enhancer, and as a fire retardant.
  • nano-graphite also is added to control the cell morphology, to reduce foam surface static, and to function as internal lubricant in the foaming process.
  • IAAs infrared attenuating agents
  • carbon black powdered amorphous carbon, graphite, and titanium dioxide have been used as fillers in polymeric foam boards to minimize material thermal coductivity which, in turn, will maximize insulating capability (increase R-value) for a given thickness.
  • R value is defined as the commercial unit used to measure the effectiveness of thermal insulation.
  • a thermal insulator is a material, manufactured in sheets, that resists conducting heat energy. Its thermal conductance is measured, in traditional units, in Btu's of energy conducted times inches of thickness per hour of time per square foot of area per Fahrenheit degree of temperature difference between the two sides of the material.
  • the R value of the insulator is defined to be 1 divided by the thermal conductance per inch.
  • R is an abbreviation for the complex unit combination hr-ft 2 -°F/Btu. In SI units, an R value of 1 equals 0.17611 square meter Kelvin per watt (m 2 -K/W).
  • the heat transfer through an insulating material can occur through solid conductivity, gas conductivity, radiation, and convection.
  • UV stability particularly for such as exterior wall insulation finishing system (EIFS), and highway and railway underground applications where prolonged exposure of sun light of the surface of the polymer foam boards are usually occurred in job-sites.
  • EIFS exterior wall insulation finishing system
  • Regular low density foams have very thin cell wall thickness in the range of 0.2 to 6 microns. Particularly, in order to enhance the insulation R-value, a target cell wall thickness of less than about 1 micron is needed.
  • the present invention relates to foam insulating products and the processes for making such products, such as extruded polystyrene foam, containing nano- graphite as a process additive to improve the physical properties, such as thermal insulation and compressive strength.
  • nano-graphite acts as a nucleating agent and lubricant as well as its slipping action makes the flow of the melted polymer in the extruder easier, and provides a smooth surface to the foam board. Further, the nano-graphite reduces the amount of static present during the foaming process due to the increased electric conductivity of the skin of the nano- graphite polymer foam boards.
  • Nano-graphite in a foam product also acts as a UV stabilizer and as a gas barrier in the final product.
  • Figure 1 is a graphical illustration depicting the density v. compressive modulus of polystyrene foam and polystyrene foams containing nano-graphite.
  • Figure 2 is a graphical illustration comparing the rheology of pure polystyrene foam v. polystyrene foam containing nanographite.
  • Figure 3 is a scanning electronic microscope (SEM) image of the foam cells of the present invention.
  • Figure 4 is a scanning electronic microscope (SEM) image of the foam cell walls and struts.
  • Figure 5 is a graphical illustration comparing a polystyrene foam board to the nano-graphite/polystyrene board of the present invention when both boards are exposed to UV radiation.
  • the above objects have been achieved through the development of a polymer foam which contains nano-graphite to control cell morphology and act as a gas diffusion barrier.
  • the foam exhibits improved thermal insulation (R-values) acting as an infrared attenuating agent and a cell nucleating agent.
  • the nano-graphite in the foam serves as an internal lubricant during processing of the foam and permits the release of surface static during processing of the foam.
  • Foams containing nano-graphite, of the present invention also have increased dimensional stability. Aesthetically, the foam of the present invention has a shiny surface and is silver in color.
  • the present invention particularly relates to the production of a rigid, closed cell, polymer foam board prepared by extruding process with nano-graphite, at least one blowing agent and other additives.
  • the rigid foamed plastic materials may be any such materials suitable to make polymer foams, which include polyolefins, polyvinylchloride, polycarbonates, polyetherimides, polyamides, polyesters, polyvinylidene chloride, polymethylmethacrylate, polyurethanes, polyurea, phenol-formaldehyde, polyisocyanurates, phenoiics, copolymers and terpolymers of the foregoing, thermoplastic polymer blends, rubber modified polymers, and the like.
  • Suitable polyolefins include polyethylene and polypropylene, and ethylene copolymers.
  • a preferred thermoplastic polymer comprises an alkenyl aromatic polymer material.
  • Suitable alkenyl aromatic polymer materials include alkenyl aromatic homopolymers and copolymers of alkenyl aromatic compounds and copolymerizable ethylenically unsaturated comonomers.
  • the alkenyl aromatic polymer material may further include minor proportions of non-alkenyl aromatic polymers.
  • the alkenyl aromatic polymer material may be comprised solely of one or more alkenyl aromatic homopolymers, one or more alkenyl aromatic copolymers, a blend of one or more of each of alkenyl aromatic homopolymers and copolymers, or blends of any of the foregoing with a non-alkenyl aromatic polymer.
  • Suitable alkenyl aromatic polymers include those derived from alkenyl aromatic compounds such as styrene, alphamethylstyrene, ethylstyrene, vinyl benzene, vinyl toluene, chlorostyrene, and bromostyrene.
  • a preferred alkenyl aromatic polymer is polystyrene.
  • Minor amounts of monoethylenically unsaturated compounds such as C 2 - 6 alkyl acids and esters, ionomeric derivatives, and C 4-6 dienes may be copolymerized with alkenyl aromatic compounds.
  • copoiymerizable compounds examples include acrylic acid, methacrylic acid, ethacrylic acid, maleic acid, itaconic acid, acrylonitrile, maleic anhydride, methyl acrylate, ethyl acrylate, isobutyl acrylate, n-butyl acrylate, methyl methacrylate, vinyl acetate and butadiene
  • Preferred structures comprise substantially (i.e., greater than about 95 percent) and most preferably entirely of polystyrene.
  • the present invention relates to a process for preparing a foam product involving the steps of forming a foamable mixture of (1 ) polymers having weight -average molecular weights from about 30,000 to about 500,000.
  • the polystyrene has weight-average molecular weight about 250,000, and (2) nano-graphite, (3) at least one blowing agent, (4) other process additives, such as a nucleation agent, flame retardant chemicals, foaming the mixture in a region of atmosphere or reduced pressure to form the foam product.
  • the nano-graphite used in this invention is a nano-graphite which has at least in one dimension, most likely the thickness of the particle, less than about 100 nanometers by X-ray diffraction.
  • the foam comprises nanosheets of exfoliated graphite dispersed in the polymeric matrix.
  • Exfoliated graphite is graphite that has been intercalated preferably by an oxidation process, where the atoms or molecules have been inserted into the inter-planar spacing between the layered planes of carbons, and expanded.
  • the intercalated graphite is expanded or exfoliated preferably by brief exposure to high heat to expand the thickness of the graphite.
  • the expanded or exfoliated graphite is then mixed with monomers and polymerized in situ to form a polymer with a network of nanosheets of the exfoliated graphite dispersed therein.
  • the exfoliated graphite advantageously retains its nanostructure during the polymerization process.
  • the expanded or exfoliated graphite is compressed together into flexible thin sheets.
  • the nano-graphite in the foam comprises a plurality of nanosheets typically in layers.
  • the nanosheets having a thickness of between about 10 to several hundred nanometers, with majority in the range from about 10 to about 100 nanometers.
  • Detailed explanation of graphite exfoliation may be found in Graphite Intercalation Compounds I: Structure and Dynamics, H. Zabel; S.A. Solin (1990) and Carbon and Graphite Handbook, CL. Mantell (1968) which are herein incorporated by reference.
  • Nano-graphite is then added into the extruder preferably greater than 0% to about 10%, more preferably about 0.5 to about 3% by weight based on the weight of the polymer along with polystyrene, a blowing agent, and optionally other additives.
  • an extruded polystyrene polymer foam is prepared by twin-screw extruders (low shear) with flat die and plate shaper.
  • twin-screw extruders low shear
  • a single screw tandem extruder high shear
  • the nano-graphite compound is added into the extruder via multi-feeders, along with polystyrene, a blowing agent, and/or other additives.
  • the plasticized resin mixture, containing nano-graphite, polymer, and optionally, other additives are heated to the melt mixing temperature and thoroughly mixed.
  • the melt mixing temperature must be sufficient to plastify or melt the polymer. Therefore, the melt mixing temperature is at or above the glass transition temperature or melting point of the polymer.
  • the melt mix temperature is from about 200 to about 250°C, most preferably about 220 to about 240°C depending on the amount of nano-graphite.
  • a blowing agent is then incorporated to form a foamable gel.
  • the foamable gel is then cooled to a die melt temperature.
  • the die melt temperature is typically cooler than the melt mix temperature, in the preferred embodiment, from about 100°C to about 130°C, and most preferably from about 120 0 C.
  • the die pressure must be sufficient to prevent prefoaming of the foamable gel, which contains the blowing agent. Prefoaming involves the undesirable premature foaming of the foamable gel before extrusion into a region of reduced pressure. Accordingly, the die pressure varies depending upon the identity and amount of blowing agent in the foamable gel. Preferably, in the preferred embodiment, the pressure is from about 50 to about 80 bars, most preferably about 60 bars.
  • the expansion ratio, foam thickness per die gap is in the range of about 20 to about 70, typically about 60.
  • Fig. 2 illustrates a comparison of viscosity (eta* in Pa-sec) between grade 1600 polystyrene from NOVA Chemical, PA and the same polystyrene with 1 wt% of nano-graphite additive at regular die shear rate range (around 100 rad/sec frequency).
  • regular die temperature operation range - from 115 to 125 0 C, the viscosity of the polystyrene with nano-graphite is higher, but is manageable within the operation temperature window.
  • blowing agents useful in the practice of this invention include inorganic agents, organic blowing agents and chemical blowing agents.
  • Suitable inorganic blowing agents include carbon dioxide, nitrogen, argon, water, air, nitrogen, and helium.
  • Organic blowing agents include aliphatic hydrocarbons having 1-9 carbon atoms, aliphatic alcohols having 1-3 carbon atoms, and fully and partially halogenated aliphatic hydrocarbons having 1-4 carbon atoms.
  • Aliphatic hydrocarbons include methane, ethane, propane, n- butane, isobutane, n-pentane, isopentane, and neopentane.
  • Aliphatic alcohols include methanol, ethanol, n-propanol, and isopropanol.
  • Fully and partially halogenated aliphatic hydrocarbons include fluorocarbons, chlorocarbons, chloroftuorocarbons and cyclopentane.
  • fluorocarbons include methyl fluoride, perfluoromethane, ethyl fluoride (HFC-161 ), ethyl fluoride, 1 ,1- difluoroethane (HFC-152a), 1 ,1 ,1-trifluoroethane (HFC-143a), 1 ,1 ,1 ,2-tetrafluoro- ethane (HFC-134a), 1 ,1 ,2,2-tetrafluoroethane (HFC-134), pentafluoroethane (HFC-125), difluoromethane (HFC-32), perfluoroethane, 2,2-difluoropropane (HFC-272fb), 1 ,1 ,1-trifluoropropane (HFC-263fb), perfluoropropane, 1 ,1 ,1 ,3,3- pentafluorobutane (HFC-365mfc), 1 ,1
  • Partially halogenated chlorocarbons and chlorofluorocarbons for use in this invention include methyl chloride, methylene chloride, ethyl chloride, 1 ,1 ,1-trichloroethane, 1 ,1-dichloro-1- fluoroethane(HCFC-141 b), 1 -chloro-1 , 1 -difluoroethane (HCFC-142b), 1 ,2- difluoroethane (HFC-142), chlorodifluoromethane (HCFC-22), 1 ,1-dichloro-2,2,2- trifluoroethane (HCFC-123) and 1 -chloro-1 ,2,2,2-tetrafluoroethane (HCFC-124), and the like.
  • Fully halogenated chlorofluorocarbons include trichloromonofluoromethane (CFC-11), dichlorodifluoromethane (CFC-12), trichlorotrifluoroethane (CFC-113), 1 ,1,1-trifluoroethane, pentafluoroethane, dichlorotetrafluoroethane (CFC-114), chioroheptafiuoropropane, and dichlorohexafluoropropane.
  • CFC-11 trichloromonofluoromethane
  • CFC-12 dichlorodifluoromethane
  • CFC-113 trichlorotrifluoroethane
  • 1 ,1,1-trifluoroethane pentafluoroethane
  • dichlorotetrafluoroethane CFC-114
  • chioroheptafiuoropropane dichlorohexafluoroprop
  • Chemical blowing agents include azodicarbonamide, azodiisobutyro-nitrile, benzenesulfonhydrazide, 4,4-oxybenzene sulfonyl- semicarbazide, p-toluene sulfonyl semi-carbazide, barium azodicarboxylate, and N,N'-dimethyl-N,N'-dinitrosoterephthalamide and trihydrazino triazine.
  • a mixture of blowing agents may be used with the present invention such as a mixture including 1 ,1 ,2,2-tetrafluoroethane (HFC-134a) with around same amount of 1 ,1-difluoroethane (HFC-152a).
  • HFC-134a 1 ,1 ,2,2-tetrafluoroethane
  • HFC-152a 1 ,1 ,2,2-tetrafluoroethane
  • About 50% of the 134a blowing agent and about 50% of the 152b blowing agent may be present in the composition. Both components based on the weight of the polymer. However, for low density, thick products, the amount of 152a may be increased up to about 60% or more based on the weight of the polymer.
  • the present invention it is preferable to use about 6 to about 14%, preferably about 1 1 %, cyclopentane by weight based on the weight of the polymer. It is preferred to add about 0 to about 4% ethanol, about 3 to about 6%, preferably about 3.5% carbon dioxide. All percentages are based on the weight of the polymer.
  • Optional additives may be incorporated in the extruded foam product and include additional infrared attenuating agents, plasticizers, flame retardant chemicals, pigments, elastomers, extrusion aids, antioxidants, fillers, antistatic agents, UV absorbers, citric acids, nucleating agents, surfactants, processing aids, etc. These optional additives may be included in any amount to obtain desired characteristics of the foamable gel or resultant extruded foam products.
  • optional additives are added to the resin mixture but may be added in alternative ways to the extruded foam manufacture process.
  • the product produced by the above-described process is a rigid, foam insulation board which is about 1/8 to about 12 inches thick, typically about 1 to about 4 inches thick.
  • the density of the foam board is typically about 1.2 to about 5 pcf, typically about 1.4 to about 3 pcf.
  • the resulting board is silver in color with a shiny surface.
  • the nanographite in the foam controls cell morphology.
  • the nano-scale graphite acts as a nucleating agent in the foaming process
  • Fig. 3 is an SEM image of the foam including 1% nano-graphite in polystyrene foam.
  • Fig. 4 is an SEM image of the cell walls and struts of the foam product.
  • the polystyrene foam contains 1% nano-graphite.
  • the thickness of the cell walls is about 0.86 microns, the strut diameter is about 3.7 microns.
  • Figure 5 illustrates the UV protect ability of polystyrene foam board with the nano- graphite of the present invention when the board is exposed to UV radiation.
  • the test method used is a QUV test, followed by color measurement.
  • Test methods and material standards for the QUV test include ISO 4982-1 Plastics, ASTM G- 151 , ASTM G-154, ASTM G53, British Standard BS 2782, Part 5, Method 540B, and SAE J2020, JIS D0205. All test methods and standards cited above are herein incorporated by reference.
  • the color measurements are made on the L*a * b scales.
  • the L scale, from 0 to 100, represents a black to white relationship.
  • the nano-graphite foam with grey color was almost no change from an extended UV exposure for more than 100 days.
  • the a and b scale, from 1 to -1 represent the different color changes: from red to green, and from yellow to blue. Slight changing of color has been observed after more than 90 days UV exposure for the nano-graphit
  • Example 1 which is not to be construed as limiting, in which all foam boards are extruded polystyrene foam boards.
  • rigid polystyrene foam boards are prepared by a twin screw LMP extruder with flat die and shaper plate; and a two single screw tandem extruder with radial die and slinky shaper.
  • a vacuum may also be applied in both of the above described pilot and manufacturing lines.
  • Table 1 shows the process conditions for samples in a twin screw extruder for making foam boards having a width of 16 inches and a thickness of one inch.
  • nano-graphite used was confirmed by X-ray diffraction to be 29.7 nm, and 51 nm after compounding with about 60 wt% of polystyrene. Carbon black was not part of mix with nano-graphite due to its poor process ability and high smoke density during fire test.
  • Table 3 compares the operating conditions between batch foaming and traditional low-density foam extrusion.
  • the polymerized nano-graphite/polystyrene compound Prior to batch foaming, the polymerized nano-graphite/polystyrene compound is heated and compressed into a solid shape.
  • the solid sheet is cut into small pieces according to the size of pressure vessel, such as 77 x 32 x 1 mm.
  • the solid sheet specimen is then placed in a mold and foamed in a high-pressure vessel at about 80 to about 160 0 C, typically about 12O 0 C and about 500 to about 4000 psi, typically about 2000 psi.
  • the solid sheet remains in the pressurized vessel for about 8 to about 50 hours, typically about 12 hours, after which the pressure in the vessel was released quickly (about 12 seconds) for foaming.
  • the nano-graphite/polystyrene foam of the batch foaming samples were evaluated to determine the amount infrared radiation transmitted through the foam.
  • infrared light is the major form of thermal radiation.
  • PS/graphite foam attenuates thermal radiation and enhances the heat solid conduction. Further, by improved graphite dispersion and concentration, these trends are expected to be more significant.

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

Abstract

La présente invention concerne des produits isolants en mousse, en particulier une mousse de polystyrène extrudée, contenant du nano-graphite en tant qu'additif de traitement pour améliorer les propriétés physiques des produits de mousse.
EP06800020A 2006-07-05 2006-07-05 Mousses de polymère contenant du nano-graphite multifonctionnel stratifié Withdrawn EP2041211A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2006/026490 WO2008005022A1 (fr) 2006-07-05 2006-07-05 Mousses de polymère contenant du nano-graphite multifonctionnel stratifié

Publications (1)

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EP2041211A1 true EP2041211A1 (fr) 2009-04-01

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Country Status (8)

Country Link
EP (1) EP2041211A1 (fr)
JP (1) JP2009542839A (fr)
CN (1) CN101479330A (fr)
AU (1) AU2006345744A1 (fr)
BR (1) BRPI0621791A2 (fr)
CA (1) CA2655727A1 (fr)
MX (1) MX2009000042A (fr)
WO (1) WO2008005022A1 (fr)

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