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WO2001088033A1 - Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions - Google Patents

Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions Download PDF

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Publication number
WO2001088033A1
WO2001088033A1 PCT/US2001/015548 US0115548W WO0188033A1 WO 2001088033 A1 WO2001088033 A1 WO 2001088033A1 US 0115548 W US0115548 W US 0115548W WO 0188033 A1 WO0188033 A1 WO 0188033A1
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WIPO (PCT)
Prior art keywords
composition
weight
compositions
epoxy resin
compound
Prior art date
Application number
PCT/US2001/015548
Other languages
English (en)
Inventor
Chin-Jui Chang
Gerald Fitzgerald
Original Assignee
Sika Corporation
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Filing date
Publication date
Application filed by Sika Corporation filed Critical Sika Corporation
Priority to CA002409750A priority Critical patent/CA2409750A1/fr
Priority to MXPA02011238A priority patent/MXPA02011238A/es
Priority to JP2001585246A priority patent/JP2004527587A/ja
Priority to EP01933339A priority patent/EP1287069A4/fr
Priority to AU2001259772A priority patent/AU2001259772A1/en
Publication of WO2001088033A1 publication Critical patent/WO2001088033A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
    • 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
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • 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
    • C08J9/06—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 chemical blowing agent
    • C08J9/10—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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102—Azo-compounds
    • C08J9/103—Azodicarbonamide
    • 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
    • C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
    • 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
    • C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins

Definitions

  • the present invention is broadly concerned with expandable sealant and baffle compositions for sealing hollow structural members of vehicles, and methods for making and using such compositions.
  • the compositions are prepared by forming an expandable mixture including a first thermoplastic resin (preferably an SBS block co- polymer) and an epoxy resin (preferably a bisphenol A-based liquid epoxy resin).
  • the compositions preferably also include a second thermoplastic resin (preferably a polystyrene) different from the first thermoplastic resin, and a compound selected from the group consisting of pigments, blowing agents, catalysts, curing agents, reinforcers, and mixtures thereof.
  • the preferred reinforcers are hydrated amorphous silica and glass microspheres.
  • the compositions of the invention are injection moldable and can be formed into freestanding, self-sustaining parts. Alternately, the compositions of the invention can be supported on lattice-type nylon supports. Upon heating of the compositions to temperatures of at least about 300°F, the compositions greatly expand to form lightweight products having high compressive strengths
  • U.S. Patent No. 5,755,486 to Wycech is directed towards a structural reinforcement member which includes a thermally expandable resin-based material.
  • the structural member is heated so as to expand the resin-based material, thus locking the reinforcement member in place.
  • the compositions disclosed in the '486 patent do not possess sufficient expansion capabilities. As a result, more of the composition is required to adequately fill and seal a particular cavity, thus resulting in added weight to the car and added expense to the automotive manufacturer.
  • composition disclosed in the '486 patent makes use of fumed silica which leads to a product having a high viscosity and therefore unsuitable for injection molding of the composition.
  • U.S. Patent Nos. 5,373,027 and 5,266,133 to Hanley et al. are respectively directed towards expansible sealant and baffle components for sealing and providing an acoustic baffle for cavities in vehicle bodies and methods of making such components.
  • the components expand upon heating, thus sealing the cavity in which they are placed.
  • the components are formed of a composition which includes an ethylene- ⁇ , ⁇ ethylenically unsaturated carboxylic acid copolymer, a blowing agent, a tackifier, and optionally an additive polymer and a cross-linking agent. While the compositions of the '027 and ' 133 patents possess sufficient expansion capabilities, they are not strong enough to make suitable reinforcement members.
  • U.S. Patent No. 5,506,025 to Otto et al. is concerned with an expandable baffle apparatus for sealing an automobile cavity.
  • the apparatus of the '025 patent includes a piece of heat expandable sealing material formed in a shape corresponding to the shape of the cross-section of the cavity to be sealed.
  • the sealing material is supported by an open lattice support element formed of material such as nylon. While the apparatus of the '025 patent is suitable as a cavity sealant and baffle apparatus, it does not provide sufficient reinforcement to the structural member forming the cavity in which the apparatus is placed.
  • the instant invention overcomes these problems by providing expandable sealant and baffle compositions comprising mixtures of thermoplastic resin(s) and an epoxy resin which are injection moldable and lightweight, and which have high compressive strengths.
  • the compositions of the invention include a first thermoplastic resin, usually selected from the group consisting of the polystyrenes, rubbers (preferably solid rubbers), and mixtures thereof. It is preferred that the first thermoplastic resin be a solid rubber or mixtures of solid rubbers.
  • Preferred solid rubbers include styrene-butadiene rubber (such as SBR 1009 ® ), nitrile-butadiene rubber (such as Nipol 1411 ® ), thermoplastic elastomers including SBS block co-polymers (such as Fina Clear 530 ® ), and mixtures thereof. (As used herein, "rubber” is intended to include all synthetic rubbers as well as elastomers.).
  • the rubber used is an SBS block co-polymer
  • the SBS block, co-polymer have a molecular weight of from about 100,000-150,000, and preferably from about 110,000-135,000.
  • the ratio of butadiene to styrene is preferably from about 32:68 to about 18:82, and more preferably from about 27:73 to about 23 :77.
  • the first thermoplastic resin is a rubber
  • the rubber is preferably present in the composition at a level from about 20-30% by weight, and more preferably from about 23-28% by weight, based upon the total weight of the composition taken as 100% by weight.
  • the polystyrene should be present in the composition at a level of from about 5-20% by weight, and preferably at aleveiof from about 10-15% by weight, based upon the total weight of the composition taken as 100% by weight. It is preferable that the polystyrene have a molecular weight of from about 150,000-320,000, and more preferably from about 200,000-270,000. Two preferred polystyrenes are sold under the trade names Fina Crystal 500 ® and Fina Crystal 535 ® .
  • the compositions further include an epoxy resin, preferably a liquid epoxy resin such as a bisphenol A-based liquid epoxy resin.
  • the epoxy resin should be present in the composition at a level of from about 30-45% by weight, and -preferably from about 35-40% by weight, based upon the total weight of the composition taken as 100% by weight.
  • a preferred solid epoxy resin is available under the ' trade name Epon 1001 F ® .
  • Two preferred liquid epoxy resins are sold under the trade names Araldite 6010 ® and
  • Epon 71 ® Epon 71 ®
  • the compositions of the inventions further include a second thermoplastic resin different from the first thermoplastic resin.
  • the second thermoplastic resin is likewise preferably selected from the group consisting of the polystyrenes, rubbers (preferably solidrubbers or thermoplastic elastomers), and mixtures thereof.
  • the first thermoplastic resin be a solid rubber and mixtures of solid rubbers while the second thermoplastic resin is preferably a polystyrene, with the individual concentrations of solid rubber and polystyrene being those described above.
  • the total weight of both the first thermoplastic resin and the second thermoplastic resin is preferably from about 25-50% by weight, and more preferably ' from about 33-43% by weight, based upon the total weight of the composition taken as 100% by weight.
  • compositions of the invention further include a third thermoplastic resin in addition to and different from the first and second thermoplastic resins.
  • the third thermoplastic resin is preferably selected from the group consisting of polystyrenes, rubbers (preferably solid rubbers or thermoplastic elastomers), and mixtures thereof.
  • the third resin shouldbe present in an amount of from about 1-10% by weight, and preferably from about 3-7% by weight, based upon the total weight of the composition taken as 100%o by weight.
  • a preferred third thermoplastic resin is a solid rubber such as nitrile-butadiene rubber (NBR).
  • NBR nitrile-butadiene rubber
  • the ratio of acrylonitrile to butadiene is preferably from about 42: 58 to about 35:65, and more preferably about 38:62.
  • compositions of the invention should also include a compound selected from the group consisting of pigments, blowing agents, catalysts, curing agents, reinforcers, and mixtures thereof. Any pigments, blowing agents, catalysts, and curing agents known in the art are suitable for use in the instant invention. Examples of some of those compounds and their preferred concentrations in the compositions of the invention are set forth in Table 1. It is preferred that the compositions be essentially free (i.e., less than about 0.1% by weight, and preferably about 0% by weight) of plasticizers, diluents, and surfactants in order to avoid the negative effects these compounds have on the compressive strengfhof the composition during heating thereof.
  • Percent by weight o the particular compound based upon the total weight of the composition taken as 100% by weight.
  • the preferred reinforcers are selected from the group consisting of hydrated amorphous silica, glass microspheres, and mixtures thereof. Glass microspheres are particularly preferred because they greatly increase the strength of the cured composition while only slightly increasing the weight thereof.
  • the compositions hereof include from about 1-10% by weight hydrated amorphous silica and from about 10-20% 0 glass microspheres. Utilizing both of these reinforcers results in a composition having a very high compressive strength- Also, hydrated amorphous silica is important for providing a composition that has high expansion capabilities as well as a viscosity (at 110 °C) of less than about 1500 P, and preferably less than about 1250 P, so that the composition can readily be injection molded.
  • compositions in accordance with the instant invention includes the following: from about 20-30%) by weight SBS block co-polymer; from about 5-20% by weight polystyrene; from about 30-45% by weight bisphenol A-based liquid epoxy resin; from about 0.5-5% by weight carbon black; from about 1 - 10% by weight hydrated amorphous silica; from about 10-20% by weight glass microspheres; from about 0.5-5% by weight blowing agent; from about 0.3-5% by weight catalysts; and from about 1-5% by weight curing agent, with all percents by weight being based upon the total weight of the composition taken as 100%o by weight.
  • Another particularly preferred embodiment of the invention includes the following: from about 20-30% by weight SBS block co-polymer; from about 5-20% by weight polystyrene; from about 0.5-5% by weight of a rubber (e.g., nitrile-butadiene rubber); from about 30-45% by weight bisphenol A-based liquid epoxy resin; from about 0.5-5% by weight of a pigment (e.g., carbon black); from about 1-10% by weight hydrated amorphous silica; from about 10-20% by weight glass microspheres; from about 0.1 -5% by weight blowing agent (e.g., azodicarbonamide); from about 0.1 -5% by weight catalysts (e.g., N,N-dimethyl phenyl urea); from about 0.1-5% by weight curing agent (e.
  • SBS block co-polymer from about 5-20% by weight polystyrene; from about 0.5-5% by weight of a rubber (e.g., nitrile-but
  • dicyandiamide e.g., dicyandiamide
  • a accelerator compound e.g., zinc oxide
  • compositions of the invention are formed by mixing the first thermoplastic resin (preferably solid rubber) with a small portion (about l/40th of the total amount) of the epoxy resin in a heated mixer until the temperature of the mixer reaches from about 240-260 °F (the temperature of the mixture within the mixer is at least about 175 °F), and the mixture is substantially homogeneous, at which time all of the second thermoplastic resin (preferably a polystyrene) is added to the mixer and mixing is continued. After the second thermoplastic resin is substantially mixed with the first thermoplastic resm/epoxy resin mixture, the remainder of the epoxy resin is slowly added to the mixer, stopping and starting the mixer as necessary, with the ingredients being thoroughly mixed to obtain a substantially homogeneous mixture. The resulting
  • premix can then be used immediately to form the final composition or, alternately, can be formed into a thick sheet (approximately 20 mm) via a two-roll mill, cut into pieces, and stored for later use.
  • the desired amount of premix is placed in a heated mixer (set at a temperature of about 250 °F) and mixing is commenced. While mixing, the desired pigments are added to the mixer and mixing is stopped once a homogeneous mixture is obtained within the mixer. While mixing is stopped, one of the desired reinforcers is added to the mixer and mixing is resumed and continued until the mixture is homogeneous. This step can be repeated, adding additional reinforcers as desired.
  • the temperature of the mixer is then set to a temperature below 160°F. When the temperature of the mixer drops below 160°F, the desired blowing agents, curing agents, and/or catalysts are added and mixing is resumed and continued only until the mixture is homogeneous.
  • the resulting mixture is then preferably extruded into strands (at an extruder temperature of 170-180°F and screw rotation speeds of about 400 rpm) and cut into pellets.
  • the desired blowing agents, curing agents, and/or catalysts can be dry blended with the cut pellets rather than being added to the mixture prior to extrusion.
  • the pellets are then injection molded into the desired shape at a temperature of about 180-200° Fusing any injection molding techniques and equipment known in the art.
  • the desired shape of the molded composition will depend upon the volume of the cavity to be sealed and baffled, as well as the configuration of that cavity thus ensuring that the composition fully expands into a sealing relationship with the structural sidewalls.
  • the molded product that is formed is a physical mixture, and no chemical reactions have occurred prior to the heating of the product within the vehicle cavity to a temperature of at least about 300 °F.
  • sealing and baffling compositions of the invention can be manufactured as formed, freestanding parts, in other embodiments the compositions can be supported on a support element comprising an open lattice formed in the same shape as of the composition, thus forming a sealant and baffle apparatus.
  • Preferred lattice support elements are formed of nylon, and particularly glass reinforced nylon.
  • Use of open lattice supports allows the composition to expand through the openings of the lattice upon heating of the composition to a temperature of at least about 300°F. This structure is superior to the structure in U.S. Patent No. 5,755486 to Wycech as the use of a lattice support element adds minimal weight to the apparatus.
  • Preferred apparatuses comprise a plurality of U-shaped expandable composition structures spaced apart from one another and in general alignment, having the lattice support element attached to the three outer surfaces of the U-shaped structure.
  • This embodiment provides for contact by the composition with a greater surface area of the cavity walls than is provided by U.S. Patent No. 5,506,025 to Otto et al., thus providing superior reinforcement of structural member forming the cavity.
  • compositions of the invention are formed into the U-shaped structure described above, or are shaped (in either free standing form or some type of lattice-supported form) to conform to the cross-sectional shape of (although slightly smaller than) the cavity in which the composition or apparatus is to be used.
  • the formed composition or apparatus is then placed within the hollow channel or cavity and heat is applied so that the composition expands as the epoxy resin is crosslinked and the expanded composition adheres to the sidewalls of the cavity resulting in a channel or cavity that is substantially blocked by the expanded composition.
  • some type of fastening device or mechanism canbe utilized to secure the composition within the channel prior to heat expansion.
  • compositions of the invention can be used in virtually any area of the automotive industry, including body shops, paint shops, and automobile manufacturing facilities.
  • a particular advantage of the compositions and apparatuses of the invention is that they can be placed within the desired channel prior to conveyance of the vehicle body through a bake oven where the temperatures are sufficiently high to expand the composition.
  • the sealants and baffle compositions of the invention are subjected to a temperature of at least about 300 °F, the percent expansion of the composition will be from about 80-220% and preferably from about 95-200% wherein the percent expansion (as used herein) is defined as:
  • the expanded compositions have a compressive strength (using a sample having a diameter of 2 inches and a length of 4 inches and a compression rate of 0.5 inches/minute) of at least about 1200 psi, preferably at least about 1400 psi, and more preferably at least about 1600 psi.
  • the compositions Prior to expansion, the compositions have a specific gravity (with reference to water) of at least about 0.90, while the specific gravity (with reference to water) of the expanded compositions is less than about 0.47, preferably less than about 0.37, and more preferably less than about 0.32.
  • the compositions of the invention have a ratio of compressive strength:specific gravity after bake of at least about 2500:1, preferably at least about 3000:1, and more preferably at least about
  • Figure 1 is a side elevation view of the preferred U-shaped sealant and baffle apparatus utilizing the open lattice support element in accordance with the invention
  • Fig. 2 is a top plan view of the apparatus of Fig. 1
  • Fig. 3 is a left end elevation view of the apparatus of Fig I; and
  • Fig. 4 is a fragmentary sectional view taken along line — 4 of Fig. 2.
  • the apparatus 10 broadly includes three expandable, U-shaped members 12, 14,
  • member 12 includes a base portion 20 and two leg portions 22, 24.
  • Members 1 , 16 are identical to member 12 in that they each include a base portion and two leg portions.
  • Leg portions 26, 28 of members 14, 16, respectively, are illustrated in Fig. 2, while base portions 30, 32 of members 14, 16, respectively, are illustrated in Fig. 3.
  • the leg portions are substantially perpendicular to their respective base portions. Stated otherwise, each of the legs of members 12, 14, 16 is essentially parallel to its counterpart leg on the respective member.
  • Members 12, 14, 16 are each formed of the heat expandable compositions of the invention and are preferably injection molded as integral members into the illustrated U-shape.
  • Support element 18 is formed of three sections, i.e., abase section and two leg sections, which are likewise configured into a U-shape.
  • Base section 34 of element 18 is illustrated in Fig.3 while leg section 36 is illustrated in Fig. 2.
  • the final leg section 38 of element 18 is shown in phantom in Fig. 1.
  • Each of sections 34, 36, 38 of support element 18 have a latticework structure and are formed of a material having a melting point higher than the temperature at which members 12, 14, 16 expand.
  • a preferred material for element 18 is nylon, and particularly glass reinforced nylon.
  • the outside planar surfaces of the base and leg portions of members 12, 14, 16 are preferably formed with depressions (indicated by double lines 40 in Figs.2 and 3).
  • depressions correspond in both size and shape with the size and shape of the latticework of element 18.
  • the depressions are preferably at least as deep as the lattice is thick, and act as a retaining mechanism so that element 18 remains attached to members 12, 14, 16.
  • the expandable composition of which members 12, 14, 16 are formed protrudes somewhat through the lattice openings of element 18 (as indicated by numeral 42 in Figs. 2-4).
  • Element 18 can be formed so that each of the sections 34, 36, 38 are integral, or alternately, each of sections 34, 36, 38 can be formed separately and connected by some fastening mechanism (such as clips or snaps) around the members 12, 14, 16 of the apparatus.
  • the apparatus 10 is positioned within the channel of a hollow member (such as within a vehicle).
  • the apparatus 10 can be positioned at any angle and orientation as determined appropriate by one having ordinary skill in the art.
  • the base portions 20, 30, 32 and base section 34 of apparatus 10 can be positioned against the lower wall of the channel, while the respective leg portions and sections of apparatus 10 would be positioned against the sidewalls of the channel.
  • the apparatus 10 could be inverted so that the base portions 20, 30, 32 and base section 34 are positioned against the upper wall of the channel.
  • the apparatus 10 is then subjected to heat (such as by passing the vehicle through a bake oven), preferably having a temperature of at least about 300 °F.
  • heat such as by passing the vehicle through a bake oven
  • the heat application will cause the composition to expand in all directions, thus protruding even further through the openings of the latticework.
  • the expanded composition will then adhere to the walls of the channel, securing apparatus 10 within the channel.
  • compositions of the invention do not require a support structure and can be used in a freestanding, self-sustaining form. Also, numerous other support elements can be used with the compositions of the invention depending upon the particular application.
  • a mixer (Moriyama Company, Japan) equipped with a ram was used to prepare a premix.
  • the temperature of the mixer was set to 210°F, and 266.67 grams of Fina Clear 530 ® (SBS block copolymer) was added to the mixer followed by the addition of about 10 grams of Araldite 6010 ® (liquid epoxy resin).
  • the ram was lowered and slow mixing was commenced when the temperature of the mixer had reached 200°F. Mixing was continued until the mixture was substantially homogeneous, and the temperature display indicated 250°F. At this point, the ram was opened and 133.33 grams of Fina Crystal 500 ® (polystyrene) was added to the mixer. Mixing was continued until the material in the mixer became substantially homogeneous.
  • the remainder of the Araldite 6010 ® (about 390 grams) was added to the mixture slowly, in small increments, with mixing carried out between each addition.
  • the resulting mixture was thoroughly mixed for about 5 minutes, and the material was then transferred to a 2-roll mill. The material was milled into sheets having a thickness of about 20 mm, and cut into pieces to be used later.
  • the temperature of the mixer was set below 160°F. When the mixer temperature cooled to below 160°F, 16 grams of Celogen AZ 765 ® (blowing agent) and 64 grams of Urisys DDA 10 ® (curing agent) was added to the mixer and mixing was resumed and continued only until the mixture was homogeneous.
  • the compound formed in Part 2 of this Example was fed into the inlet of a single screw extruder set at an extruder temperature of 175 °F.
  • the screw was rotated at a speed of about 400 rpm, and the stranded compound was cut into pellets as it emerged from the die positioned at the outlet of the extruder barrel.
  • the die used was one designed to make pellets of such a size that 90 ( ⁇ 10) of the pellets weighed 1 gram.
  • the pellets were added to the hopper (not equipped with a stirrer) of a conventional injection mold machine and molded into the desired shapes at about 190°F.
  • test specimens were aged in a 90°C oven for four hours and tested immediately upon removal from- the oven. b Several tests of the compressive strength were conducted on this sample. This number is the average of the results of all tests conducted.
  • EXAMPLE 2 A molded compound was formed following the procedures set forth in Example 1 except that the following components and concentrations were used: 133.33 grams of Fina Crystal 500 ® ; 266.67 grams of Fina Clear 530 ® ; 400 grams of Araldite 6010 ® ; 10 grams of carbon black; 4.8 grams of zinc oxide (pigment); 45 grams of HiSil 233 ® ; 155 grams of Scotchlite S60/10,000 ® ; 30 grams of Urisys DDA 10 ® ; 4 grams of Urisys U 405 ® (catalyst); and 6 grams of Celogen.AZ 130 ® (blowing agent). The catalyst was added at the same time as the blowing agent and curing agent. The final product was tested for its mechanical properties as described in Example 1 and as set forth in Table
  • Example 1 The test specimens were aged in a 90° C oven for four hours and tested immediately upon removal from the oven. b Several tests of the compressive strength were conducted on this sample. This number is the average of the results of all tests conducted.
  • EXAMPLE S A molded compound was formed following the procedures set forth in Example 1 except the following components and concentrations were used: 120 grams of Fina Crystal 500 ® ; 240 grams ofFina Clear 530 ® ; 40 grams ofNipol 1411 ® (nitrile-butadiene rubber); 400 grams of Araldite 6010 ® ; 10 grams of carbon black; 4.8 grams of zinc oxide; 45 grams of HiSil 233 ® ; 155 grams of Scotchlite S60/10,000 ® ; 30 grams of Urisys DDA 10 ® ; 4 grams of Urisys U 405 ® ; and 6 grams of Celogen AZ 130 ® . The final product was tested for its mechanical properties as set forth in Table 4.
  • test specimens were aged in a 90° C oven for four hours and tested immediately upon removal from the oven. b Several tests of the compressive strength were conducted on this sample. This number is the average of the results of all tests conducted.
  • the components and concentrations used were as follows: 133.33 grams of Fina Crystal 500 ® ; 266.67 grams of Fina Clear 530 ® ; 400 grams of Araldite 6010 ® ; 10 grams of carbon black; 4.8 grams of zinc oxide; 45 grams of Cabot TS-720 ® (fumed silica); 155 grams of Scotchlite S60/10,000 ® ; 30 grams of Urisys DDA 10 ® ; 4 grams of Urisys U 405 ® ; and 6 grams of Celogen AZ 130 ® .
  • the properties of the resulting compound are set forth in Table 7 below.
  • test specimens were aged in a 90° C oven for four hours and tested immediately upon removal from the oven. b Several tests of the compressive strength were conducted on this sample. This number is the average of the results of all tests conducted.
  • test specimens were aged in a 90° C oven for four hours and tested immediately upon removal from the oven. b Several tests of the compressive strength were conducted on this sample. This number is the average of the results of all tests conducted.
  • EXAMPLE 7 This test was carried out to determine the effect on the mechanical properties of the composition if no SBS (or any other rubber) was used. Preparation of the composition was commenced following the previously described procedures. However, the preparation was aborted during the preparation of the premix because, without the use of a rubber, the initial ingredients could not be mixed.
  • EXAMPLE 8 This test was carried out to determine how the use of SBR, in addition to SBS rubber, would affect the overall properties of the composition.
  • the procedure followed to prepare the composition was as described in the previous examples.
  • the components and concentrations used were as follows: 120.0 grams of Fina Crystal 500 ® ; 240 grams of Fina Clear 530 ® ; 40 grams of SBR 1009 ® , crumb; 400 grams of Araldite 6010 ® ; 10 grams of carbon black; 4.8 grams of zinc oxide; 45 grams of HiSil 233 ® ; 155 grams of Scotchlite S60/10,000 ® ; 30 grams of Urisys DDA 10 ® ; 4 grams of Urisys U 405 ® ; and 6 grams of Celogen AZ 130 ® .
  • the properties of the resulting compound are set forth in Table 9.

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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)
  • General Chemical & Material Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Epoxy Resins (AREA)

Abstract

L'invention concerne des compositions de scellement et d'écran acoustique expansibles et des procédés de formage et d'utilisation de ces compositions. Ces compositions comprennent une première résine thermoplastique, une résine époxyde, de préférence un seconde résine thermoplastique différente de la première résine thermoplastique et éventuellement un composé sélectionné dans le groupe constitué par les pigments, les agents d'expansion, les catalyseurs, les agents de polymérisation, les charges renforçantes et des mélanges de ces composés. On forme les compositions résultantes de manière a obtenir des éléments autonomes pouvant être expansés à chaud pour donner des produits légers haute résistance servant à sceller les éléments structurels creux des véhicules, et à atténuer sensiblement le bruit qui se propage le long de ces éléments tout en renforçant ces éléments avec une augmentation minimale de leur poids. Dans un mode de réalisation préféré, la première résine thermoplastique est un copolymère séquencé SBS, la résine époxyde est une résine époxyde liquide à base de bisphénol A, la seconde résine thermoplastique est un polystyrène et la charge renforçante est de la silice amorphe hydratée. Ces compositions permettent de former des éléments autonomes, autoportants ou des éléments en U maintenus par des supports de Nylon de type treillis.
PCT/US2001/015548 2000-05-16 2001-05-15 Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions WO2001088033A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA002409750A CA2409750A1 (fr) 2000-05-16 2001-05-15 Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions
MXPA02011238A MXPA02011238A (es) 2000-05-16 2001-05-15 Composiciones de amortiguamiento de sonido y de reforzamiento estructural y metodos para el uso de las mismas.
JP2001585246A JP2004527587A (ja) 2000-05-16 2001-05-15 防振／構造補強組成物およびその使用方法
EP01933339A EP1287069A4 (fr) 2000-05-16 2001-05-15 Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions
AU2001259772A AU2001259772A1 (en) 2000-05-16 2001-05-15 Sound deadening and structural reinforcement compositions and methods of using the same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US57275400A 2000-05-16 2000-05-16
US09/572,754 2000-05-16

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WO2001088033A1 true WO2001088033A1 (fr) 2001-11-22

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PCT/US2001/015548 WO2001088033A1 (fr) 2000-05-16 2001-05-15 Compositions d'attenuation sonore et de renfort structurel et procedes d'utilisation de ces compositions

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EP (1) EP1287069A4 (fr)
JP (1) JP2004527587A (fr)
AU (1) AU2001259772A1 (fr)
CA (1) CA2409750A1 (fr)
MX (1) MXPA02011238A (fr)
WO (1) WO2001088033A1 (fr)

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EP1493558A1 (fr) * 2003-07-04 2005-01-05 Nitto Denko Corporation Feuille de renforcement pour plaques d'acier
US6846559B2 (en) 2002-04-01 2005-01-25 L&L Products, Inc. Activatable material
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US7025409B2 (en) 2001-11-14 2006-04-11 L & L Products, Inc. Automotive rail/frame energy management system
US7041193B2 (en) 2003-05-14 2006-05-09 L & L Products, Inc. Method of adhering members and an assembly formed thereby
US7077460B2 (en) 2002-04-30 2006-07-18 L&L Products, Inc. Reinforcement system utilizing a hollow carrier
US7105112B2 (en) 2002-11-05 2006-09-12 L&L Products, Inc. Lightweight member for reinforcing, sealing or baffling
US7111899B2 (en) 2003-04-23 2006-09-26 L & L Products, Inc. Structural reinforcement member and method of use therefor
US7125461B2 (en) 2003-05-07 2006-10-24 L & L Products, Inc. Activatable material for sealing, baffling or reinforcing and method of forming same
US7144071B2 (en) 2002-05-23 2006-12-05 L&L Products, Inc. Multi segment parts
US7160491B2 (en) 2000-02-11 2007-01-09 L&L Products, Inc. Structural reinforcement system for automotive vehicles
US7169344B2 (en) 2002-04-26 2007-01-30 L&L Products, Inc. Method of reinforcing at least a portion of a structure
US7199165B2 (en) 2003-06-26 2007-04-03 L & L Products, Inc. Expandable material
US7255388B2 (en) 2003-05-08 2007-08-14 Zephyros, Inc. Reinforcing members
US7313865B2 (en) 2003-01-28 2008-01-01 Zephyros, Inc. Process of forming a baffling, sealing or reinforcement member with thermoset carrier member
US7318873B2 (en) 2002-03-29 2008-01-15 Zephyros, Inc. Structurally reinforced members
US7374219B2 (en) 2004-09-22 2008-05-20 Zephyros, Inc. Structural reinforcement member and method of use therefor
US7428774B2 (en) 2005-05-25 2008-09-30 Zephyros, Inc. Baffle for an automotive vehicle and method of use therefor
US7438782B2 (en) 2006-06-07 2008-10-21 Zephyros, Inc. Activatable material for sealing, baffling or reinforcing and method of forming same
US7473715B2 (en) 2001-05-02 2009-01-06 Zephyros, Inc. Two component (epoxy/amine) structural foam-in-place material
US7479246B2 (en) 2004-06-21 2009-01-20 Zephyros, Inc. Overmoulding
US7494179B2 (en) 2005-04-26 2009-02-24 Zephyros, Inc. Member for baffling, reinforcement or sealing
US7503620B2 (en) 2005-05-12 2009-03-17 Zephyros, Inc. Structural reinforcement member and method of use therefor
US7521093B2 (en) 2004-07-21 2009-04-21 Zephyros, Inc. Method of sealing an interface
US7597382B2 (en) 2005-06-07 2009-10-06 Zephyros, Inc. Noise reduction member and system
US7941925B2 (en) 2003-06-26 2011-05-17 Zephyros, Inc. Method of forming members for providing sealing or baffling
US8967327B2 (en) 2012-03-20 2015-03-03 Zephyros, Inc. Baffle assembly
US9010843B2 (en) 2012-06-08 2015-04-21 Zephyros, Inc. Partial-filled baffle
US9096039B2 (en) 2010-03-04 2015-08-04 Zephyros, Inc. Structural composite laminates
US9427902B2 (en) 2009-09-15 2016-08-30 Zephyros, Inc. Cavity filling
US9688050B2 (en) 2004-06-18 2017-06-27 Zephyros, Inc. Panel structure
US9713885B2 (en) 2010-12-08 2017-07-25 Zephyros, Inc. Sealing assembly
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Cited By (75)

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US7160491B2 (en) 2000-02-11 2007-01-09 L&L Products, Inc. Structural reinforcement system for automotive vehicles
US7011315B2 (en) 2000-03-14 2006-03-14 L&L Products, Inc. Expandable pre-formed plug
US6928736B2 (en) 2000-03-14 2005-08-16 L & L Products Method of reinforcing an automobile structure
US6620501B1 (en) 2000-08-07 2003-09-16 L&L Products, Inc. Paintable seal system
US6991237B2 (en) 2000-08-07 2006-01-31 L & L Products, Inc. Paintable seal system
US6777049B2 (en) 2001-03-20 2004-08-17 L&L Products, Inc. Structural foam
US6905745B2 (en) 2001-03-20 2005-06-14 L & L Products Inc. Structural foam
US7473715B2 (en) 2001-05-02 2009-01-06 Zephyros, Inc. Two component (epoxy/amine) structural foam-in-place material
US6706772B2 (en) 2001-05-02 2004-03-16 L&L Products, Inc. Two component (epoxy/amine) structural foam-in-place material
US6787579B2 (en) 2001-05-02 2004-09-07 L&L Products, Inc. Two-component (epoxy/amine) structural foam-in-place material
US6941719B2 (en) 2001-05-08 2005-09-13 L&L Products, Inc. Structural reinforcement
US6855652B2 (en) 2001-08-24 2005-02-15 L&L Products, Inc. Structurally reinforced panels
WO2003018688A1 (fr) * 2001-08-24 2003-03-06 L & L Products, Inc. Materiau peignable
US6729425B2 (en) 2001-09-05 2004-05-04 L&L Products, Inc. Adjustable reinforced structural assembly and method of use therefor
US6880657B2 (en) 2001-09-05 2005-04-19 L&L Products Inc. Adjustable reinforced structural assembly and method of use therefor
US6887914B2 (en) * 2001-09-07 2005-05-03 L&L Products, Inc. Structural hot melt material and methods
US6890021B2 (en) 2001-09-24 2005-05-10 L & L Products Structural reinforcement system having modular segmented characteristics
US7025409B2 (en) 2001-11-14 2006-04-11 L & L Products, Inc. Automotive rail/frame energy management system
US7114763B2 (en) 2001-11-14 2006-10-03 L & L Products, Inc. Automotive rail/frame energy management system
US7318873B2 (en) 2002-03-29 2008-01-15 Zephyros, Inc. Structurally reinforced members
US6846559B2 (en) 2002-04-01 2005-01-25 L&L Products, Inc. Activatable material
US6969551B2 (en) 2002-04-17 2005-11-29 L & L Products, Inc. Method and assembly for fastening and reinforcing a structural member
US7169344B2 (en) 2002-04-26 2007-01-30 L&L Products, Inc. Method of reinforcing at least a portion of a structure
US7077460B2 (en) 2002-04-30 2006-07-18 L&L Products, Inc. Reinforcement system utilizing a hollow carrier
US7296847B2 (en) 2002-04-30 2007-11-20 Zephyros, Inc. Reinforcement system utilizing a hollow carrier
US7144071B2 (en) 2002-05-23 2006-12-05 L&L Products, Inc. Multi segment parts
US6920693B2 (en) 2002-07-24 2005-07-26 L&L Products, Inc. Dynamic self-adjusting assembly for sealing, baffling or structural reinforcement
US7004536B2 (en) 2002-07-29 2006-02-28 L&L Products, Inc. Attachment system and method of forming same
US6923499B2 (en) 2002-08-06 2005-08-02 L & L Products Multiple material assembly for noise reduction
US6932421B2 (en) 2002-09-10 2005-08-23 L & L Products, Inc. Structural reinforcement member and method of use therefor
US6883858B2 (en) 2002-09-10 2005-04-26 L & L Products, Inc. Structural reinforcement member and method of use therefor
US6692347B1 (en) 2002-09-27 2004-02-17 L&L Products, Inc. Filter housing assembly for transportation vehicles
US7105112B2 (en) 2002-11-05 2006-09-12 L&L Products, Inc. Lightweight member for reinforcing, sealing or baffling
US7478478B2 (en) 2003-01-06 2009-01-20 Zephyros, Inc. Method of providing reinforcing members
US6953219B2 (en) 2003-01-06 2005-10-11 L&L Products, Inc. Reinforcing members
US7313865B2 (en) 2003-01-28 2008-01-01 Zephyros, Inc. Process of forming a baffling, sealing or reinforcement member with thermoset carrier member
US7111899B2 (en) 2003-04-23 2006-09-26 L & L Products, Inc. Structural reinforcement member and method of use therefor
US7125461B2 (en) 2003-05-07 2006-10-24 L & L Products, Inc. Activatable material for sealing, baffling or reinforcing and method of forming same
US7255388B2 (en) 2003-05-08 2007-08-14 Zephyros, Inc. Reinforcing members
US7041193B2 (en) 2003-05-14 2006-05-09 L & L Products, Inc. Method of adhering members and an assembly formed thereby
US7199165B2 (en) 2003-06-26 2007-04-03 L & L Products, Inc. Expandable material
US8931173B2 (en) 2003-06-26 2015-01-13 Zephyros, Inc. Method of forming fastenable member for sealing, baffling or reinforcing
US8671573B2 (en) 2003-06-26 2014-03-18 Zephyros, Inc. Method of forming fastenable member for sealing, baffling or reinforcing
US11390004B2 (en) 2003-06-26 2022-07-19 Zephyros, Inc. Fastenable member for sealing, baffling or reinforcing and method of forming same
US10328624B2 (en) 2003-06-26 2019-06-25 Zephyros, Inc. Method of forming fastenable member for sealing, baffling or reinforcing
US9352505B2 (en) 2003-06-26 2016-05-31 Zephyros, Inc. Method of forming fastenable member for sealing, baffling or reinforcing
US7941925B2 (en) 2003-06-26 2011-05-17 Zephyros, Inc. Method of forming members for providing sealing or baffling
EP1493558A1 (fr) * 2003-07-04 2005-01-05 Nitto Denko Corporation Feuille de renforcement pour plaques d'acier
US8017533B2 (en) 2003-07-04 2011-09-13 Nitto Denko Corporation Steel plate reinforcing sheet
EP1504890A3 (fr) * 2003-08-08 2005-05-25 Nitto Denko Corporation Feuille adhésive pour tôle d'acier
US8092906B2 (en) 2003-08-08 2012-01-10 Nitto Denko Corporation Adhesive sheet for steel plate
EP1504890A2 (fr) * 2003-08-08 2005-02-09 Nitto Denko Corporation Feuille adhésive pour tôle d'acier
US10647083B2 (en) 2004-06-18 2020-05-12 Zephyros, Inc. Panel structure
US9688050B2 (en) 2004-06-18 2017-06-27 Zephyros, Inc. Panel structure
US7479246B2 (en) 2004-06-21 2009-01-20 Zephyros, Inc. Overmoulding
US7521093B2 (en) 2004-07-21 2009-04-21 Zephyros, Inc. Method of sealing an interface
US7374219B2 (en) 2004-09-22 2008-05-20 Zephyros, Inc. Structural reinforcement member and method of use therefor
US7494179B2 (en) 2005-04-26 2009-02-24 Zephyros, Inc. Member for baffling, reinforcement or sealing
US7503620B2 (en) 2005-05-12 2009-03-17 Zephyros, Inc. Structural reinforcement member and method of use therefor
US7428774B2 (en) 2005-05-25 2008-09-30 Zephyros, Inc. Baffle for an automotive vehicle and method of use therefor
US7597382B2 (en) 2005-06-07 2009-10-06 Zephyros, Inc. Noise reduction member and system
US7438782B2 (en) 2006-06-07 2008-10-21 Zephyros, Inc. Activatable material for sealing, baffling or reinforcing and method of forming same
US11248145B2 (en) 2008-04-09 2022-02-15 Zephyros, Inc. Structural adhesives
US11667813B2 (en) 2008-04-09 2023-06-06 Zephyros, Inc. Structural adhesives
US9427902B2 (en) 2009-09-15 2016-08-30 Zephyros, Inc. Cavity filling
US9096039B2 (en) 2010-03-04 2015-08-04 Zephyros, Inc. Structural composite laminates
US9713885B2 (en) 2010-12-08 2017-07-25 Zephyros, Inc. Sealing assembly
US8967327B2 (en) 2012-03-20 2015-03-03 Zephyros, Inc. Baffle assembly
US9776368B2 (en) 2012-06-08 2017-10-03 Zephyros, Inc. Partial-filled baffle
US9010843B2 (en) 2012-06-08 2015-04-21 Zephyros, Inc. Partial-filled baffle
US10577522B2 (en) 2013-07-26 2020-03-03 Zephyros, Inc. Thermosetting adhesive films including a fibrous carrier
US10577523B2 (en) 2013-07-26 2020-03-03 Zephyros, Inc. Relating to thermosetting adhesive films
US11873428B2 (en) 2013-07-26 2024-01-16 Zephyros, Inc. Thermosetting adhesive films
US11028220B2 (en) 2014-10-10 2021-06-08 Zephyros, Inc. Relating to structural adhesives
USD938887S1 (en) 2018-06-21 2021-12-21 Zephyros, Inc. Sealing device

Also Published As

Publication number Publication date
JP2004527587A (ja) 2004-09-09
EP1287069A4 (fr) 2004-09-29
AU2001259772A1 (en) 2001-11-26
CA2409750A1 (fr) 2001-11-22
MXPA02011238A (es) 2003-04-25
EP1287069A1 (fr) 2003-03-05

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