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WO2001021699A1 - Article thermoplastique ayant l'apparence de paillettes metalliques - Google Patents

Article thermoplastique ayant l'apparence de paillettes metalliques

Info

Publication number
WO2001021699A1
WO2001021699A1 PCT/US2000/025792 US0025792W WO0121699A1 WO 2001021699 A1 WO2001021699 A1 WO 2001021699A1 US 0025792 W US0025792 W US 0025792W WO 0121699 A1 WO0121699 A1 WO 0121699A1
Authority
WO
WIPO (PCT)
Prior art keywords
transparent
polymer matrix
platelets
polycarbonate
article according
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.)
Ceased
Application number
PCT/US2000/025792
Other languages
English (en)
Inventor
David Rosendale
John G. Skabardonis
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.)
General Electric Co
Original Assignee
General Electric Co
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 General Electric Co filed Critical General Electric Co
Publication of WO2001021699A1 publication Critical patent/WO2001021699A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B44—DECORATIVE ARTS
    • B44F—SPECIAL DESIGNS OR PICTURES
    • B44F9/00—Designs imitating natural patterns
    • B44F9/10—Designs imitating natural patterns of metallic or oxidised metallic surfaces
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H2209/00—Layers
    • H01H2209/002—Materials
    • H01H2209/0021—Materials with metallic appearance, e.g. polymers with dispersed particles to produce a metallic appearance

Definitions

  • This application relates to a transparent article having a metallic flake appearance. Specifically, this application relates to an article that comprises a pigment having a metallic flake appearance dispersed within a transparent thermoplastic matrix.
  • thermoplastics become increasingly important in the marketplace, producers have sought to differentiate their products by making them more visually exciting to the customer.
  • One desirable look for thermoplastics is the metal flake appearance. This appearance can be described as the look one could imagine if small pieces of metal were dispersed in molten glass, and the glass was subsequently cooled. The flakes have a metallic glint, but one perceives clear spaces between the metallic flakes such that portions of the article are completely transparent.
  • thermoplastic article having a metal flake appearance.
  • Metal flakes most typically aluminum flake
  • aluminum flake is hazardous because it can cause dust explosions. If aluminum flake does burn in a tire, it burns at a very high temperature, which makes the fire very difficult to extinguish.
  • Mica has also been dispersed in thermoplastics in an attempt to create a metallic flake appearance. Mica can provide a metallic flake appearance, especially when coated with a layer of an inorganic pigment such as titanium dioxide.
  • mica has several drawbacks. Specifically, incorporating mica in a transparent thermoplastic tends to decrease the transparency of the thermoplastic, producing a "milky" appearance. Mica also degrades the physical properties of the thermoplastic matrix. Finally, it is difficult to prepare materials containing mica platelets because excessive shear conditions may cause breakage of the platelets, which can ruin desired appearance.
  • the articles according to the present invention have a desirable metallic flake appearance, yet they avoid the above-identified problems with previous compositions having this same appearance.
  • the transparent articles disclosed herein have a metallic flake appearance. These articles are formed by dispersing an amount of metal oxide-coated glass platelets in a transparent thermoplastic matrix. The amount and size of platelets must be sufficient to create the metallic flake appearance, but not so high that the article appears opaque and metallic. The matrix must be transparent because the platelets have minimal affect on the appearance of opaque materials.
  • the method for making a transparent article disclosed herein comprises melt extruding a transparent polymer matrix together with an amount of metal oxide-coated glass platelets effective to provide a metallic flake appearance. It is important in this process to avoid excess shear because such treatment can cause physical damage to the platelets, which results in a chemical interaction that causes the transparent matrix to yellow.
  • article designates any and all items made from a thermoplastic, including thermoplastic compositions prior to molding
  • pellets e.g., pellets
  • articles designates pellets
  • the pellets may themselves have a rough surface, and therefore may not look transparent, but will be capable of forming transparent articles upon processing. Such pellets should still be considered to be transparent, as defined below.
  • transparent means a transparent, natural or translucent article having a light transmittance above 50%.
  • the transmittance is measured according to ASTM procedure D1003, using a BYK Gardner Hazeguard Plus instrument. The machine operates by measuring the intensity difference between the projected light and the transmitted light using a photodetector.
  • a transparent article according to this definition may have reduced transmission, due to the inclusion of some other ingredients (e.g., dyes) but will still have light transmittance above 50%.
  • the term "natural” refers to an article having a light transmittance above 80%. Such materials may actually contain small amounts of dyes designed to offset any other color which mav be an undesirable artifact of the manufacturing process (e.g., yellowing), or to provide a specific color in combination with the metallic look.
  • the finished articles according to the invention have adequate transparency to produce the metallic flake appearance.
  • the transparent thermoplastic matrix described above may be any transparent thermoplastic material that is compatible with metal oxide-coated glass platelets.
  • Suitable transparent thermoplastic materials include, but are not limited to polycarbonates, copolyester carbonates, polymethyl methacrylate, polyetherimides, transparent polyimides, halo olefin polymers, transparent polyamides (nylons), polyesters, transparent polycarbonate- polyester blends, polysulfones, polyether and polyphenyl sulfones, transparent acrylonitrile butadiene styrene, styrene acrylonitrile (SAN), polystyrene, cellulosics, miscible transparent polystyrene-polyphenylene oxide (PS-PPO) blends, acrylics, polycarbonate-polvsiloxanes, polyetherimide-polysiloxanes, polyarylates, polyethvlene
  • More preferred transparent thermoplastic matrix materials are polyetherimides, polymethyl methacrylate, polycarbonate (homopolymer or copolymers), copolvester carbonates, polyethylene terephthalate (PET), styrene acrylonitrile, polystyrene, transparent acrylonitrile butadiene styrene and cellulosics.
  • An even more preferred matrix material is a clear aromatic polycarbonate homopolymer based primarily on the bisphenol-A monomer.
  • a most preferred embodiment of the invention is a copolyester carbonate made by reacting a dicarboxylic acid (e.g., dodecanedioic acid) with bisphenol-A monomer.
  • Metal oxide-coated glass platelets are preferably made by first stretching a molten C glass into thin sheets, beads or glass tubes followed by crushing this glass into flakes.
  • C glass is a form of glass that is resistant to corrosion by acid and moisture due to its zinc oxide content.
  • these glass flakes are coated by dispersing them in water at a concentration of 10 to 20%.
  • an appropriate iron or titanium source is added while maintaining the pH at an appropriate level (e.g., by adding a base) to cause precipitation of hydrous titanium dioxide or hydrous iron oxide on the glass flake.
  • an acid is typically added, the flakes are washed and subsequently calcined.
  • Suitable metal oxide-coated glass platelets and methods for making them are described in U.S. Patent No. 5,753,371, which is hereby incorporated by reference.
  • platelet loadings of 0.005 to 5 percent by weight of the transparent polymer matrix. It is more preferred to use platelet loadings of 0.01 to 2 percent by weight. If the loading is too low, the metallic flake appearance will not be observable. If the loading is too high, the entire article will seem metallic, will not be transparent, and will have degraded physical properties (e.g., poor impact performance).
  • the average particle size of the glass platelets is typically from 30 to 200 microns.
  • the transparent matrix may optionally further contain an optical brightening agent, a dye or dyes (which may be fluorescent), a light diffuser, stabilizers and/ or antioxidants, pigments, antistatic agents, mold release agents and ultraviolet light (“UV”) stabilizers. None of these additives should exceed an amount which will cause the matrix to become opaque.
  • an optical brightening agent a dye or dyes (which may be fluorescent), a light diffuser, stabilizers and/ or antioxidants, pigments, antistatic agents, mold release agents and ultraviolet light (“UV”) stabilizers. None of these additives should exceed an amount which will cause the matrix to become opaque.
  • Suitable optical brightening agents include, but are not limited to, aromatic stilbene derivatives, aromatic benzoxazole derivatives, or aromatic stilbene benzoxazole derivatives.
  • any type of dye may be added which is compatible with the matrix and does not cause the matrix to become opaque.
  • fluorescent dyestuffs include Permanent Pink R (Color Index Pigment Red 181, from Clanant Corporation), Hostasol Red 5B (Color Index #73300, CAS # 522-75-8, from Clanant Corporation) and Macrolex Fluorescent Yellow 10GN (Color Index Solvent Yellow 160 1, from Bayer Corporation)
  • Suitable light diffusers include, but are not limited to, polytetraflu ⁇ ioethvlene, zinc oxide, and polymethylmethacrylate
  • TechpoK mer MBX-se ⁇ es crosslinked polymethylmethacrylate microspheres which are available in various diameters from Nagase America (e g , 5 -50 micron avg diameter), may be added to the matrix
  • stabilizers and antioxidants include phosphites (e , aromatic phosphite thermal stabilizers), metal salts of phosphoric and phosphorous acid, hindered phenol antioxidants, epoxides, aromatic lactone radical engers, and combinations thereof
  • any other type of pigment that is well known for inclusion in thermoplastic materials can also be added to the transparent polymer matrix, provided the amount of pigment added is sufficiently low to preserve transparency and metallic flake appearance of the ai tide
  • Suitable pigments include titanium dioxide, zinc sulfide, carbon black, cobalt chromate, cobalt titanate, cadmium sulfides, iron oxide, sodium aluminum sulfosihcate, sodium sulfosihcate, chrome antimony titanium rutile, nickel antimony titanium rutile, and zinc oxide
  • Suitable antistatic agents include, but are not limited to, phosphonium salts, poly alky lene glycols, sulfonium salts and alkyl and aryl ammonium salts
  • Suitable mold release agents include, but are not limited to, pentaerythritol tetracarboxylate, glycerol monocarboxylate, glycerol triscarboxylate, polyolefins, alkyl waxes and amides.
  • Suitable UV stabilizers include, but are not limited to, substituted benzotriazoles, or triazines, or tetraalkylpiperidines.
  • the UV stabilizers may be mixed into the thermoplastic matrix, or they can be included only in a "hardcoat" transparent protective layer which is applied over the viewing surface, or stabilizers can be included both in the matrix and the hardcoat.
  • the matrix may further comprise other resins and additives such as heat resisting agents, anti-weathering agents, lubricants, plasticizers, flame retardants, and flow-improving agents. Again, the transparency and the metallic flake appearance of the matrix are limiting factors in adding any of these materials. These additives may be introduced in a mixing or molding process.
  • the components may be mixed by any known methods. Typically, there are two distinct mixing steps: a premixing step and a melt mixing step.
  • the premixing step the dry ingredients are mixed together. This premixing step is typically performed using a tumbler mixer or a ribbon blender. However, if desired, the premix may be manufactured using a high shear mixer such as a Henschel mixer or similar high intensity device.
  • the premixing step must be followed by a melt mixing step where the premix is melted and mixed again as a melt. Alternatively, it is possible to skip the premixing step, and simply add the raw materials directly into the feed section of a melt mixing device via separate feed systems.
  • the ingredients are typically melt kneaded in a single screw or twin screw extruder, a Banbury mixer, a two roll mill, or similar device. It is preferred to skip the premixing step and introduce the platelets into the molten polymeric matrix downstream in an extruder after the point where the polymer melts. This process works better than feeding the platelets at room temperature into the mouth of the extruder. Feeding at room temperature is problematic because mixing the solid polymer matrix with the platelets and subsequently melting the polymer in an extruder subjects the platelets to high shearing forces, which tends to cause breakage of the platelets. It is undesirable to break apart the platelets because they may become too small to achieve the desired metallic flake appearance. Moreover, the broken platelets may undergo a chemical reaction with the matrix, which causes yellowing of the matrix. Feeding into the melt is also preferred ' because it helps eliminate dust problems associated with adding dry platelets to the mouth of the extruder.
  • the preferred method described above can be used to form "concentrate" pellets comprising platelets dispersed in the matrix wherein at a higher concentration than the finished pellets. These "concentrate” pellets are then fed into the feed section of a single or twin screw extruder together with additional matrix material (pellets or flake) to form finished pellets having a diluted concentration of the platelets.
  • the concentrate pellets can be added to the extruder at a position down stream from the feed section.
  • the concentrate method eliminates the potential of contaminating nearby processes with raw glass flake.
  • the additional matrix material fed together with the concentrate pellets may be different from the matrix material in the concentrate pellets.
  • the additional matrix material must be miscible with the matrix material used for the concentrate pellets such that the final pellets will be transparent.
  • Finished articles according to present invention may then be manufactured by molding the melt mixed material into various shapes using an injection molding machine or other known apparatus.
  • a film can be formed on a substrate for example, by insert molding, in-mold decorating, laminating, co-injection or co-extrusion.
  • a film can be extruded onto sheet or another film, which can then be thermoformed, vacuum-formed, or shaped in some manner. All other known methods for creating multi-layer, or any other articles are also suitable.
  • a formulation consisting of 5 kg of a copolyester carbonate having a Melt Flow index of 11 (300C, 1.2kg, ASTM D1238) was prepared by reacting dodecanedioic acid with bisphenol A and phosgene, as described in US Patent Number 5,025,081, which is incorporated by reference herein.
  • the 5 kg of resin powder, 13.5 g of mold release agent (pentaerythritol tetrastearate), and 3 g of tris (2,4-di-t-butylphenyl) phosphite were added to a container.
  • the container was sealed and mixed by shaking it in a paint shaker.
  • the blended mixture was then compounded on a 2.5 inch single screw extruder and cut into pellets. After 4 hours drying at 220 °F, the pellets were molded into various test specimens
  • a formulation consisting of 5 kg of a polycarbonate having a Melt flow index of 14 was prepared by reacting bisphenol A with phosgene using the interfacial method.
  • the resin, 13.5 g of mold release agent (pentaerythritol tetrastearate), and 3g of thermal stabilizer (tris (2,4-di-t-butylphenyl) phosphite) were mixed together with 20g of Ti0 2 coated glass flake material, and pellets were prepared as described in Example 1.
  • a formulation was prepared as described in Example 2, with the exception that only 5 g of Ti0 2 coated glass flake was added.
  • a formulation was prepared as described in Example 1, with the exception that only 5 g of Ti0 2 coated glass flake was added.
  • Example 1 A formulation was prepared as described in Example 1 with the exception that 20 g of pearlescent mica material, known commercially as Magnapearl 4000 sold by Engelhard Corporation, was added in place of the glass flake. Table I, below, shows a comparison of the properties observed upon measuring samples prepared in Examples 1-4 and in this comparative example.
  • Example 1 shows that mica imparts a different look to the article and adversely affects impact strength.
  • the deterioration in impact strength is a function of the loading of the Ti0 2 coated glass flake.
  • the materials having a copolyester carbonate matrix perform are much more tolerant of high loadings of glass flake than polycarbonate homopolymers.
  • Ti0 2 coated glass flake material was pulverized with a mortar and pestle and added to the ingredients in the manner ot Example 1.
  • the molded material made using the pulverized material was more yellow than that of Example 1.
  • YI yellowness index
  • ASTM D19205 the yellowness index of the material with crushed flake showed a YI measurement 0.6 greater than the uncrushed flake.
  • the flakes in the polymer matrix had a duller appearance.
  • Ti0 2 coated glass flake material was added, along with 100 g of titanium dioxide in the manner of Example 1 in order to produce an opaque white material. The presence of the flakes in the molded material was barely discernable visually.
  • the bisphenol A (BPA) polycarbonate powder was prepared by the interfacial process, the Irgafos 168 is a phosphite stabilizer having the following chemical formula: tris-2,4 di-t-butylphenylphosphite.
  • the EP 97079 white glass flake (“Firemist Pearl”) is commercially available from Englehard.
  • Magna pearl 4000 is a mica flake material which is also available from Englehard.
  • Example 2 had a value of 7.3, whereas Example 9 had a notched izod value of 3.9. Because of the inclusion of carbon black, both of these formulations were opaque, and did not have a metallic flake appearance.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Les articles transparents de cette invention possèdent de petites particules disséminées, pourvues d'un point brillant métallique. Pour obtenir cette apparence, on disperse dans une matrice thermoplastique des paillettes de verre revêtues d'oxyde métallique. Il est souhaite de procéder par étapes pour éviter de casser les paillettes de verre au cours du processus de préparation de ces matériaux.
PCT/US2000/025792 1999-09-23 2000-09-20 Article thermoplastique ayant l'apparence de paillettes metalliques Ceased WO2001021699A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US09/401,233 1999-09-23
US09/401,233 USH1975H1 (en) 1999-09-23 1999-09-23 Thermoplastic article having a metallic flake appearance

Publications (1)

Publication Number Publication Date
WO2001021699A1 true WO2001021699A1 (fr) 2001-03-29

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US (1) USH1975H1 (fr)
WO (1) WO2001021699A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7691926B2 (en) 2002-12-17 2010-04-06 Solvay Advanced Polymers, L.L.C. 4,4′-biphenol polysulfone compositions, process to prepare them, and articles made thereof
US8961834B2 (en) 2011-03-23 2015-02-24 Sabic Global Technologies B.V. Carbon nanotube masterbatch, preparation thereof, and use in forming electrically conductive thermoplastic composition
WO2023128485A1 (fr) * 2021-12-29 2023-07-06 롯데케미칼 주식회사 Composition de résine thermoplastique et article moulé fabriqué à partir de celle-ci
DE102014227006B4 (de) 2014-03-14 2023-08-17 Hyundai Motor Company Polycarbonatharz-Zusammensetzung und Fahrzeug-Innenmaterial

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DE10002164A1 (de) * 2000-01-20 2001-07-26 Mitsubishi Polyester Film Gmbh Weiße, UV-stabilisierte, thermoformbare Folie aus einem kristallisierbaren Thermoplast, Verfahren zu ihrer Herstellung und ihre Verwendung
CN100556687C (zh) * 2002-09-12 2009-11-04 日本板硝子株式会社 覆发光膜产品
US7312257B2 (en) * 2003-01-23 2007-12-25 General Electric Company Polymer encapsulation of high aspect ratio materials and methods of making same
US7488764B2 (en) * 2003-01-23 2009-02-10 Sabic Innovative Plastics Ip B.V. Polymer encapsulation of high aspect ratio materials and methods of making same
US7205342B2 (en) * 2003-10-10 2007-04-17 General Electric Company Poly(arylene ether) composition and method of molding
US7649032B2 (en) * 2004-05-21 2010-01-19 Sabic Innovative Plastics Ip B.V. Highly ductile polycarbonate composition having a metallic-flake appearance
CN111533988B (zh) * 2019-12-23 2022-03-29 会通新材料股份有限公司 一种良外观短程控向金属银质感聚丙烯复合材料及其制备方法

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US4551491A (en) * 1983-07-29 1985-11-05 Inmont Corporation Pearlescent automotive paint compositions
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US5364926A (en) * 1992-02-27 1994-11-15 Ge Plastics, Japan, Ltd. (Gep) Preparing method of polycarbonate resin compounds for the optical use
US5753371A (en) * 1996-06-03 1998-05-19 The Mearl Corporation Pearlescent glass pigment
WO1998056850A1 (fr) * 1997-06-13 1998-12-17 M.A. Hannacolor Compositions concentrees pour donner un aspect translucide par effet optique a des polymeres thermoplastiques transparents
JPH11107160A (ja) * 1997-09-30 1999-04-20 Sekisui Chem Co Ltd 透明導電性繊維、透明性電磁波遮蔽材及びこれらの製造方法

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Publication number Priority date Publication date Assignee Title
US4551491A (en) * 1983-07-29 1985-11-05 Inmont Corporation Pearlescent automotive paint compositions
US4906676A (en) * 1984-09-13 1990-03-06 Mitsubishi Rayon Co., Ltd. Resin composition containing fine silica particles therein
US5364926A (en) * 1992-02-27 1994-11-15 Ge Plastics, Japan, Ltd. (Gep) Preparing method of polycarbonate resin compounds for the optical use
US5753371A (en) * 1996-06-03 1998-05-19 The Mearl Corporation Pearlescent glass pigment
WO1998056850A1 (fr) * 1997-06-13 1998-12-17 M.A. Hannacolor Compositions concentrees pour donner un aspect translucide par effet optique a des polymeres thermoplastiques transparents
JPH11107160A (ja) * 1997-09-30 1999-04-20 Sekisui Chem Co Ltd 透明導電性繊維、透明性電磁波遮蔽材及びこれらの製造方法

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7691926B2 (en) 2002-12-17 2010-04-06 Solvay Advanced Polymers, L.L.C. 4,4′-biphenol polysulfone compositions, process to prepare them, and articles made thereof
US8048945B2 (en) 2002-12-17 2011-11-01 Solvay Advanced Polymers, L.L.C. 4,4′-biphenol polysulfone compositions, process to prepare them, and articles made thereof
US8961834B2 (en) 2011-03-23 2015-02-24 Sabic Global Technologies B.V. Carbon nanotube masterbatch, preparation thereof, and use in forming electrically conductive thermoplastic composition
DE102014227006B4 (de) 2014-03-14 2023-08-17 Hyundai Motor Company Polycarbonatharz-Zusammensetzung und Fahrzeug-Innenmaterial
WO2023128485A1 (fr) * 2021-12-29 2023-07-06 롯데케미칼 주식회사 Composition de résine thermoplastique et article moulé fabriqué à partir de celle-ci

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