Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
  • C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
  • C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
  • C08L71/12—Polyphenylene oxides
  • C08L71/123—Polyphenylene oxides not modified by chemical after-treatment

Definitions

• the invention relates to glass fiber reinforced poly(phenylene ether) resin compositions, and more particularly relates to flame resistant, glass fiber reinforced poly(phenylene ether) resin compositions.
• compositions containing polyphenylene ether resins that are rated V-0 under the UL94 protocol when measured at a 1.6 mm wall thickness.
• a polyphenylene ether resin (b) at least one polystyrene resin; (c) about 5% by weight to about 20% by weight of an organophosphate resin; (d) about 5% by weight to about 40% by weight of glass fibers; and (e) an amount of mica effective to render the composition V-0 when measured at a thickness of 1.6 mm; wherein all weights are based on the weight of the entire composition
• compositions of the present invention comprise polyphenylene ether resin, polystyrene resin, glass fibers, an organophosphate compound and an amount of mica effective to render the composition V-0 when measured at a thickness of 1.6 mm.
• PPE per se, are known polymers comprising a plurality of structural units of the formula:
• each Q 1 is independently halogen, primary or secondary lower alkyl (e.g., alkyl containing up to 7 carbon atoms), phenyl, haloalkyl, aminoalkyl, hydrocarbonoxy, or halohydrocarbonoxy wherein at least two carbon atoms separate the halogen and oxygen atoms; and each Q 2 is independently hydrogen, halogen, primary or secondary lower alkyl, phenyl, haloalkyl, hydrocarbonoxy or halohydrocarbonoxy as defined for Q 1 .
• each Q 1 is alkyl or phenyl, especially CM alkyl
• each Q 2 is hydrogen.
• Both homopolymer and copolymer PPE are included.
• the preferred homopolymers are those containing 2,6-dimethyl-l,4-phenylene ether units.
• Suitable copolymers include random copolymers containing, for example, such units in combination with 2,3,6-trimethyl-l,4-phenylene ether units.
• PPE containing moieties prepared by grafting vinyl monomers or polymers such as polystyrenes, as well as coupled PPE in which coupling agents such as low molecular weight polycarbonates, quinones, heterocycles and formals undergo reaction in known manner with the hydroxy groups of two PPE chains to produce a higher molecular weight polymer.
• PPE contemplated for use in the present invention include all those presently known, irrespective of variations in structural units or ancillary chemical features.
• the PPE generally have an intrinsic viscosity often between about 0.10- 0.60 dl.7g., preferably in the range of about 0.30-0.48 dl./g., all as measured in chloroform at 25°C. It is also possible to utilize a higher intrinsic viscosity PPE and a lower intrinsic viscosity PPE in combination. Determining an exact ratio, when two intrinsic viscosities are used, will depend somewhat on the exact intrinsic viscosities of the PPE used and the ultimate physical properties that are desired.
• G is hydrogen, lower alkyl or halogen
• Z is vinyl, halogen or lower alkyl
• p is from 0 to 5.
• resins include homopolymers of styrene, chlorostyrene and vinyltoluene, random copolymers of styrene with one or more monomers illustrated by acrylonitrile, butadiene, ⁇ -methylstyrene, ethylvinylbenzene, divinylbenzene and maleic anhydride, and rubber- modified polystyrenes comprising blends and grafts, wherein the rubber is a polybutadiene or a rubbery copolymer of about 98-68% styrene and about 2- 32% diene monomer.
• HIPS high impact polystyrene
• Non-elastomeric block copolymer compositions of styrene and butadiene can also be used that have linear block, radial block or tapered block copolymer architectures. They are commercially available from such companies as Fina Oil as under the trademark FINACLEAR and Phillips under the trademark K-RESINS.
• the amount of the polymer of a nonelastomeric alkenylaromatic compound i.e. polystyrene resin, is an amount effective to improve the flow and processability of the composition. Improved flow can be indicated by reduced viscosity or reduced injection pressures needed to fill a part during an injection molding process.
• the nonelastomeric alkenylaromatic compound is utilized in the range of about 2% to about 40% by weight based on the total weight of the composition. The preferred range is about 4% to about 30% by weight; based on the total weight of the composition.
• R is the same or different and is alkyl, cycloalkyl, aryl, alkyl substituted aryl, halogen substituted aryl, aryl substituted alkyl, halogen, or a combination of any of the foregoing, provided at least one R is aryl.
• Examples include phenyl bisdodecyl phosphate, phenylbisneopentyl phosphate, phenyl-bis (3,5,5'-tri-methyl-hexyl phosphate), ethyldiphenyl phosphate, 2-ethyl-hexyldi(p-tolyl) phosphate, bis-(2-ethylhexyl) p- tolylphosphate, tritolyl phosphate, bis-(2-ethylhexyl) phenyl phosphate, tri- (nonylphenyl) phosphate, di (dodecyl) p-tolyl phosphate, tricresyl phosphate, triphenyl phosphate, dibutylphenyl phosphate, 2- chloroethyldiphenyl phosphate, p-tolyl bis(2,5,5'-trimethylhexyl) phosphate, 2-ethylhexyl
• the organic phosphate can be a di- or polyfunctional compound or polymer having the formula
• R 1 , R 2 , R 3 , R 4 , R 5 , R 6 and R 7 are, independently, hydrocarbon of from C1-20, aryl, or alkyl-substituted aryl;
• X 1 , X 2 and X 3 are halogen;
• m and r are 0 or integers from 1 to 4, and
• n and p are from 1 to 30.
• the aromatic rings contain hydrogens without halogen substitution. Examples include the (tetraphenyl)bisphosphates of resorcinol, hydroquinone and bisphenol-A, respectively, or their polymeric counterparts.
• flame-retardant additives for this invention are compounds containing phosphorus -nitrogen bonds, such as phosphonitrilic chloride, phosphorus ester amides, phosphoric acid amides, phosphonic acid amides, phosphi ic acid amides, tris(aziridinyl) phosphine oxide, or tetrakis(hydroxymethyl) phosphonium chloride.
• phosphorus -nitrogen bonds such as phosphonitrilic chloride, phosphorus ester amides, phosphoric acid amides, phosphonic acid amides, phosphi ic acid amides, tris(aziridinyl) phosphine oxide, or tetrakis(hydroxymethyl) phosphonium chloride.
• Preferred phosphate flame retardants include those based upon resorcinol such as, for example, resorcinol tetraphenyl diphosphate, as well as those based upon bis-phenols such as, for example, bis-phenol A tetraphenyl diphosphate. Phosphates containing substituted phenyl groups are also preferred.
• the organophosphate is selected from the group consisting of resorcinol tetraphenyl diphosphate, bis- phenol A tetraphenyl diphosphate, and mixtures containing at least one of the foregoing.
• the flame retardant is preferably present between about 5% by weight and 20% by weight, based on the weight of the entire composition.
• the particular amount will vary, depending on the molecular weight of the organic phosphate , the amount of the flammable resin present and possibly other normally flammable ingredients which might also be included in the composition.
• the present invention contains glass fibers, which greatly increase flexural strength and modulus, as well as increasing tensile strength.
• lime-aluminum borosilicate glass that is relatively soda- free (“E" glass) is preferred.
• glass roving may be used, cut fibers are preferred.
• the length of such fibers is usually at least about 3 mm; and a preferred length is in the range of about 3 mm to about 13 mm. (These lengths are based on the material before incorporation into the composition).
• a preferred diameter for the fibers is in the range of about 0.002 mm to about 0.02 mm.
• a preferred amount of glass fiber for the present invention is in the range of about 5% by weight to about 40% by weight, based on the weight of the entire composition. Larger amounts within this range are usually employed when the end use of the composition requires a higher degree of stiffness and strength. In some preferred embodiments, the amount of glass fiber present is in the range of about 10% by weight to about 30% by weight, based upon the weight of the entire composition.
• the various forms are muscovite, phlogopite, biotite, fluorophlogopite, and synthetic mica, with phlogopite being the most preferred.
• the mica is preferably in the form of flakes having an aspect ratio of about 40-120 (length /thickness). Such mica is commercially available, for example, from Suzorite Mica Products, Inc. as grade 200-HK.
• compositions have the major components which make up the composition in an amount within the following preferred ranges:
• Polyphenylene ether resin (a) about 50 to about 70 parts;
• compositions of the present invention is normally achieved by blending the ingredients under conditions for the formation of an intimate blend. Such conditions often include mixing in single or twin screw type extruders or similar mixing devices which can apply a shear to the components. It is often advantageous to apply a vacuum to the melt through a vent port in the extruder to remove volatile impurities in the composition.
• the compositions of the present invention are useful for making molded articles such as internal frames and parts for computer printers and facsimile machines, and are useful for making various other molded articles.
• Adds a combination of additives containing a weight ratio of 1.5 polyethylene to 0.3 tridecylphosphite to 0.1 zinc oxide to 0.1 zinc sulfide
• the compositions of the table were extruded on a Werner-Pfleiderer twin-screw extruder at a temperature of about 290°C with a vacuum of 1 inch Hg applied to the melt during compounding.
• the resultant compositions were molded using a Stork injection molding machine using a temperature set of about 280°C and a mold temperature of about 80°C. All the compositions were subjected to flammability testing in accordance with Underwriters Laboratory Bulletin 94 Procedures (UL94) utilizing a test sample thickness of 1.6 mm. Specifically, the average flame out time and the maximum flame out times were measured and UL94 rating was assigned.
• UL94 Underwriters Laboratory Bulletin 94 Procedures
• the present invention encompasses a method to afford a resin composition that is rated V-0 when measured at a thickness of 1.6 mm and the resin composition made by the method.

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

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• 1998
  • 1998-09-24 US US09/159,577 patent/US6359043B1/en not_active Expired - Fee Related
• 1999
  • 1999-07-06 WO PCT/US1999/015239 patent/WO2000017272A1/en not_active Ceased
  • 1999-07-06 CN CN99811309A patent/CN1116359C/zh not_active Expired - Fee Related
  • 1999-07-06 EP EP99932281A patent/EP1124901A1/en not_active Withdrawn
  • 1999-07-06 JP JP2000574176A patent/JP2002526587A/ja active Pending

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