EP1228130A2 - Verbesserte pct formulierungen enthaltend halogenierte imide, natriumantimonate, und verstärkungfasern - Google Patents

Verbesserte pct formulierungen enthaltend halogenierte imide, natriumantimonate, und verstärkungfasern

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Publication number
EP1228130A2
EP1228130A2 EP00992197A EP00992197A EP1228130A2 EP 1228130 A2 EP1228130 A2 EP 1228130A2 EP 00992197 A EP00992197 A EP 00992197A EP 00992197 A EP00992197 A EP 00992197A EP 1228130 A2 EP1228130 A2 EP 1228130A2
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European Patent Office
Prior art keywords
composition
acid
group
mole
bis
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EP00992197A
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English (en)
French (fr)
Inventor
Gerald Timothy Keep
Bruce Connard Bell
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Eastman Chemical Co
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Eastman Chemical Co
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    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3415—Five-membered rings
    • C08K5/3417—Five-membered rings condensed with carbocyclic rings
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
    • H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers

Definitions

  • This invention relates to an improvement in melt stability of a fiber reinforced, flame retardant (FR) poly(cyclohexylenedimethylene terephthalate) (PCT) formulation.
  • FR flame retardant
  • PCT poly(cyclohexylenedimethylene terephthalate)
  • HDT heat deflection temperatures
  • PCT is a high-melting polyester with a melting point of about 290°C and, consequently, is very challenging to formulate while retaining good molecular weight.
  • good dimensional stability and flammability characteristics are important.
  • United States Patent No. 4,338,243 by Hecht et al discloses the use of an antimonate to stabilize a PET/flame retardant system that also contains glass fiber, an ionic hydrocarbon salt, and a plasticizer. This system, being based on PET, could not achieve the high HDT required for soldering in high temperature electronics applications, nor is it mentioned in the patent.
  • NaSbO 3 effectiveness of NaSbO 3 in PET is shown to be equal in examples based on brominated polystyrene as well as brominated phthalimides. There is no criticality shown in the use of NaSbO 3 in combination with brominated phthalimides in a PET system.
  • United States Patent 4,313,903 by Bier discloses the use of high melting imides with PET in order to improve crystallization, and to achieve flammability targets. Such a system, based on PET, would not achieve good dimensional stability/HDT, especially given that absence of glass fiber reinforcement is recited as being preferred.
  • United States Patent 5,021,495 by Minnick broadly discloses use of a halogenated species and an antimony compound to flame retard PCT or PBT formulations that have an olefin with either acidic or epoxy functional groups to improve flame retardancy.
  • the examples cited are based on sodium antimonate and brominated polystyrene, and none of them achieve an HDT as high as 260°C.
  • Minnick's invention does not recognize the superior HDT but greater challenge of using brominated phthalimides as flame retardants.
  • United States Patent 4,837,254 by Minnick discloses the use of PCT, a halogenated flame retardant, a mixture of elemental antimony metal and Sb 2 O 3l and phenoxy. The invention is based on the synergistic effects of antimony metal and phenoxy. This patent mentions that sodium antimonate gives inadequate HDT in the cited system.
  • United States Patent 3,624,024 by Caldwell et al discloses the use of Sb 2 O 3 as flame reinforced synergist in a PBT formulation including talc and various flame retardant synergist.
  • the HDT obtained with PBT is not useful for high temperature soldering applications.
  • United States Patent 4,467,062 by Hornbaker et al discloses compositions based on PET or its copolymers, a bis-imide flame retardant, and optionally an inorganic FR synergist.
  • Sb 2 O 3 is said to be preferred and no special mention of stability is made.
  • the HDT obtained with PET and its copolymers is not useful for high temperature soldering applications.
  • This invention relates to a polymer composition comprised of:
  • glycol component comprising from about 60 to 100 mole % 1 ,4-cyclohexanedimethanol
  • a preferred embodiment of this invention comprises one or more phosphorous based compounds.
  • the polymer composition of this invention has improved dimensional stability, improved melt stability, and improved flammability characteristics that are particularly useful in high temperature electronics.
  • This invention relates to an improvement in melt stability of a fiber reinforced, flame retardant (FR) poly(cyclohexylenedimethylene terephthalate) (PCT) formulation.
  • FR flame retardant
  • PCT poly(cyclohexylenedimethylene terephthalate)
  • this formulation simultaneously achieves good dimensional stability (as demonstrated by Heat Deflection Temperature above 260°C) and good melt stability (as demonstrated by molecular weight retention upon melt processing).
  • formulations must have acceptable flammability characteristics to be useful. This is typified by UL- 94 flammability testing.
  • the relative hazard or environmental load of the metallic synergist can be considered in evaluating the usefulness of the invention. It is preferred in this invention that the polyester comprise 90 mole % or more of terephthalic acid based on the mole percentages of the dicarboxylic acid component of the polyester equaling a total of 100 mole %.
  • terephthalic acid By terephthalic acid, suitable synthetic equivalents, such as dimethyl terephthalate, are included.
  • the polyester useful in this invention comprises 0 to 15 mole %, preferably 0 to 10 mole %, of dicarboxylic acids other than terephthalic acid, based on the mole percentages of the dicarboxylic acid component of the polyester equaling a total of 00 mole %.
  • the other dicarboxylic acids include, but are not limited to, aromatic dicarboxylic acids preferably having 4 to 40 carbon atoms, more preferably, 8 to 14 carbon atoms; aliphatic dicarboxylic acids having, preferably 4 to 40 carbon atoms more preferably 4 to 12 carbon atoms or cycloaliphatic dicarboxylic acids having 4 to 40 carbon atoms, more preferably, 8 to 12 carbon atoms
  • dicarboxylic acids useful in forming the copolyester useful in the invention include, but are not limited to, isophthalic acid, naphthalenedicarboxylic acid, cydohexanedicarboxylic acid, 1 ,4-cyclohexaned ⁇ acet ⁇ c acid, d ⁇ phenyl-4,4'-d ⁇ carboxyl ⁇ c acid, naphthalenedicarboxylate, succinic acid, glutaric acid, adipic acid, azelaic acid, sebacic acid, and the like
  • isophthalic acid, naphthalenedicarboxylic acid cydohexanedicarboxylic acid and naphthalenedicarboxyate are preferred, either singly or in combination
  • trans-, cis-, or cis/trans mixtures may be used Any of the naphthalenedicarboxylic acid isomers or mixtures of isomers may be used Some preferred naphthalenedicarboxylic acid isomers include 2,6-, 2,7- 1 ,4- and 1 ,5- isomers
  • the mole percentages of the glycols referred to herein equal a total of 100 mole %
  • glycol component of the copolyester of the invention contain from about 80 to 100 mole %, preferably 90 to 100 mole %, of one or more of the isomers of 1 ,4- cyclohexanedimethanol
  • the copolyesters of this invention may be based on trans-, or cis/trans mixtures of 1 ,4-cyclohexaned ⁇ methanol
  • a 30/70 cis/trans mixture of the isomers may be readily used
  • the glycol component may comprise up to 20 mole %, and more preferably, up to 10 mole %, of one or more other aliphatic or alicyclic glycols.
  • Such additional diols include cycloaliphatic diols preferably having 6 to 20 carbon atoms or aliphatic diols preferably having 2 to 20 carbon atoms.
  • diols are: ethylene glycol, diethylene glycol, triethylene glycol, propane-1 ,3-diol, butane-1 ,4-diol, pentane-1 ,5-diol, hexane-1 ,6-diol, 3-methylpentanediol-(2,4), 2-methylpentanediol-(1 ,4), 2,2,4-trimethylpentane-diol-(1 ,3), 2-ethylhexanediol-(1 ,3), 2,2- diethylpropane-diol-(1,3), hexanediol-(1 ,3), 1 ,4-di-(hydroxyethoxy)-benzene,
  • Copolyesters may be prepared from the above diols in addition to the 1 ,4-cyclohexanedimethanol.
  • the one or more glycols are selected from ethylene glycol, diethylene glycol, triethylene glycol, propanediol, butanediol, pentanediol, hexanediol, and tetramethylcyclobutanediol.
  • the copolyester contains ethylene glycol
  • Copolyesters containing substantially only 1 ,4-cyclohexanedimethanol and terephthalic acid or substantially only 1 ,4- cyclohexanedimethanol, isophthalic and terephthalic acid are preferred.
  • the polyester resins useful in the blend of this invention are well known and are commercially available.
  • copolyesters are also intended. Methods for their preparation are described, for example, in United States Patents 2,465,319 and 3,047,539.
  • the polyesters can be prepared by direct condensation of terephthalic acid or ester interchange using dimethyl terephthalate with the selected glycol.
  • Typical catalysts which may be used to make these copolyesters include titanium alkoxides, dibutyl tin dilaurate, combinations of zinc, manganese, or magnesium acetates or benzoates with antimony oxide or antimony triacetate.
  • the polyesters of the invention preferably have an inherent viscosity of 0.1 to 2.0 dL/g, more preferably 0.3 to 1.5 dUg, and even more preferably, 0.4 to 1.2 dL/g as measured at a temperature of 25°C for a 0.5 gram sample in 100 ml of a solvent consisting of 60% by weight phenol and 40% by weight tetrachloroethane. It is preferred that the copolyester useful herein have a melting point of greater than 260°C, more preferably greater than 270°C. In some embodiments, the copolyester has a melting point of 260°C to 310°C.
  • melt processing refers to any processing step commonly used in the art for polyesters or copolyesters which occurs after the polyesters or copolyesters are heated to their melting temperature or melting point. This includes, but is not limited to, injection molding, calendering, extrusion and rotational molding.
  • the polymer composition of the invention undergoes less than a 50%, preferably 25%, and more preferably 15% loss in number average molecular weight as determined by gel permeation chromatography when melt processed at 25°C above the crystalline melting temperature (Tm) for 10 minutes.
  • the second component of the composition is a halogenated organic compound containing at least one imide group and having a melting point greater than 240°C
  • imide-group containing compounds include N,N'-arylenediphthal ⁇ m ⁇ des wherein the arylene group includes phenylene, diphenylene, naphthylene and sulfone bridged bisphenyls, tetrabrominated phthalimides, N, N'b ⁇ s(d ⁇ bromocyclohexane dicarboxyimides) with various bridging groups, and N,N'- alkylenebis(tetrahalophthalimides).
  • Preferred imide group containing compounds are those corresponding to the following formula:
  • n and m may be 1 or 0, X may be halogen, particularly chlorine or bromine, or hydrogen, and
  • R is a Ci to C ⁇ alkyl group, a single bond, a phenylene group, a toluene group, a cyclohexylene group, a bis phenyl methane group, a bis cyclohexylmethane group, or a naphthylene group.
  • N,N'-alkylenebis(tetrahalophthaiimides) suitable in the present invention and a process for their production are described in U.S. Pat. No. 4,087,441 , incorporated herein by reference.
  • the preferred N,N'- alkylenebis(tetrahalophthalimides) are represented by the formula:
  • R represents a C-
  • Hal which may be the same or different, represents a halogen atom, preferably Br or Cl, and most preferably Br.
  • N,N'- alkylenebis(tetrahalophthalimide) is particularly preferred.
  • N,N'-ethylenebis(tetrabromophthalimide) (R is an ethyl group and Hal is a Br atom).
  • imide group containing compounds include 1 ,4,5,6- tetrabromo-2,3-phthaloimide; N methylol-tetrabromophthalimide; N,N-bis- (1 ,4,5,6-tetrabromo-2,3-phthaloimide); N,N'-p-phenylene-diphthalimide; N,N'-di-phthalimidodiphenyl; bis-(N phenyl-phthalimido)sulphone; N,N'-p- phenylene-di-tetrachlorophthalimide; 4,4'-di-tetrachlorophthalimidodiphenyl; N-(tetrachlorophthalimido)-tetrachlorophthalimide, N,N'-p-phenylene-di- tetrabromophthalimide; N.N'-di-tetrabromophthalimidodiphenyl; N- (tetrabrom
  • Preferred imides have a melting point above 240°C, preferably above 300°C, including bis-imides made from aromatic or aliphatic diamines, including ethylene diamine, or hydrazine, and tetrabromophthallic anhydride or acid are preferred.
  • the most preferred flame retardant is the imide from reacting tetrabromo phthallic acid (anhydride) with ethylene diamine. This is sold commercially as Saytex BT-93 and BT-93W. This flame retardant has a high bromine content. It is thermally stable to processing temperatures characteristic of PCT, and does not soften below the PCT melting point.
  • This class of phthalimides has an advantage over other high temperature bromine sources like decabromodiphenyl in that they are not singled out as having the same environmental concerns (dioxins/furans).
  • the sum of all flame retardants used in this invention is 5-30%, preferably 10-20%, by weight of the total composition.
  • One or more flame retardants may be used within the context of this invention.
  • Brominated phthalimides are high melting materials, in contrast to other brominated flame retardants, and provide superior HDT.
  • PCT and BPI are especially challenging from a melt stability standpoint.
  • the polymer composition of this invention achieves good dimensional stability and good melt stability due, at least in part, to use of the flame retardant synergist.
  • Antimony compounds are preferred.
  • Sodium antimonate is more preferred.
  • Even more preferred is NaSbO 3 that is substantially free of Sb +3 or less than 1 mole % of Sb +3 based on the total mole percentages of antimony in the sodium antimonate.
  • Sodium antimonate is normally described in the art as being a sodium-neutralized version of Sb 2 O 3 but the importance of Sb +3 level and the desire to reduce rather than increase the amount of synergist suggest this different mechanism, reducing catalytic activity of the Sb species
  • the ratio of flame retardant halogenated imide(s), preferably, brominated phthalimide(s), to flame retardant synergist (sodium antimonate) is optimized at a much higher weight ratio (5:1 to 10:1 , preferably 8:1 ) than is commonly practiced in the art (3:1 to 4:1 ).
  • melt stability of the composition of the invention can be further improved by addition of a phosphorous-based compound.
  • the phosphorous-based compounds include, but are not limited to, one or more phosphites or phosphonites wherein at least one of the P-O bonds is attached to an aryl radical. Such compounds may be represented by the formulas
  • R ⁇ , R 2 and R 3 is an aryl radical of 6 to 30 carbon atoms and any other(s) of R-i, R 2 and R 3 are H or alkyl of 1 to 30 carbon atoms, or R 4 0
  • R , R 5 and R ⁇ is an aryl radical of 6 to 30 carbon atoms. Phosphites are preferred within the context of this invention.
  • symmetrical triaryl esters of phosphorous acid which may be used are triphenyl phosphite; tris(nonylphenyl) phosphite; and tris(2,4-di-t- butylphenyl) phosphite (Irgafos 168).
  • the most preferred symmetrical ester of phosphorous acid is bis(2,4-di-t-butylphenyl) pentaerythritol diphosphite
  • phosphorous-based compounds which may be used include, but are not limited to, Ultranox® 633 phosphite, (General Electric Chemicals), lrgafos®168 phosphite (Ciba-Geigy Corporation), Ethanox® 398 phosphonite (Ethyl Corporation) and Sandostab® P-EPQ phosphonite (Sandoz Chemicals).
  • the phosphorous compounds may be functioning by inhibiting the metal catalyst system present in the PCT. While much is known about use of phosphorous compounds in stabilizing polyester systems, it is not generally recognized as a way to stabilize flame retardants.
  • Such additives are generally present at 0 1 to about 40 weight %, preferably 0 1 to about 20 weight %, based on the total weight of the copolyester composition
  • branching agents 0 1 to 5 0 weight %, preferably less than 2 0 weight %, of one or more branching agents is included within the context of this invention, including but not limited to, trimellitic acid, trimellitic anhydride, pyromellitic anhydride, multifunctional epoxy compounds and multi-functional phenoxy compounds, and the like If the branching agent is a phenoxy compound, 2 0 to 5 0 weight % is preferred
  • reinforcing agents useful in the invention mica, clay, talc, wollastonite, and calcium carbonate
  • reinforcing fibers are carbon fibers and glass fibers
  • a particularly preferred reinforcing fiber is glass fiber It is preferable that the glass fibers be present in the polyester composition at from 0 1 to 45%o, preferably 10 to 40%, by weight based on the total weight of said polyester composition
  • Glass fibers suitable for use in the polyester compositions of the invention may be in the form of glass filaments, threads, fibers, or whiskers, etc , and may vary in length from about 1/8 inch to about 2 inches Chopped glass strands having a length of about 1/8 inch to about 1/4 inch are preferred Such glass fibers are well known in the art Of course the size of these glass fibers may be greatly diminished depending on the blending means employed, even to lengths of 300 to 700 microns or lower. It is preferred that the glass fibers are coated with polyurethane.
  • the polyester compositions of the invention may be reinforced with a mixture of glass and other reinforcing agents as described above, such as mica or talc, and/or with other additives.
  • the components of the copolyester composition of the invention may be blended and/or mixed by any suitable technology known in the art. Compounding temperatures must be at least the melting point of the polyester.
  • the polyester can be mixed dry in any suitable blender or tumbler with the other components and the mixture melt- extruded. The extrudate can be chopped. If desired the reinforcing material can be omitted initially and added after the first melt extrusion, and the resulting mixture can then be melt extruded.
  • the copolyester of this invention may be melt processed and extruded, injection molded or compression molded into a variety of shapes and forms including fibers, molded parts, bottles, pellets, containers, sheeting, film and the like.
  • the molded or shaped articles are formed through either injection molding or extrusion molding.
  • the product is especially suitable as an injection molding material for produdng molded articles.
  • shaped articles are extruded sheets or injection molded articles.
  • the shaped articles may include electronic components, which include, but are not limited to, sheet for circuit boards, connectors, circuit breaker housing, computer components, sockets, and switches. Unless otherwise specified, all parts, percentages, ratios, etc., are by weight. Weight of reinforcing glass fibers is based on total composition weight.
  • V0 means that a flame will self-extinguish within 10 seconds after each ignition without dripping molten polymer.
  • a rating of "V2” means that a flame will self-extinguish within 30 seconds after each ignition and may have flaming drips which ignite dry absorbent surgical cotton; Flame Retardant 1 - (FR1 ) - N,N'- ethylenebis(tetrabromophthalimide) which is reaction product of ethylene diamine and tetrabromophthalic anhydride; flame retardant of the invention;
  • HDT - heat deflection temperature as determined according to ASTM Method D648 at 264 psi loading
  • Inherent viscosity or "IN.” - refers to inherent viscosity expressed in dL/g measured as described herein;
  • melt stability was determined on these blends by drying a small sample of the compounded pellets. Adequate drying can be obtained by drying in a vacuum oven overnight at 80°C, or by drying for 4 hours at 125°C in a hot air circulating oven. The dried pellets were then loaded into a Tinius Olsen melt indexer or capillary rheometer and held for 10 minutes at 305°C melt temperature, then analyzed by gel permeation chromatography. The melt stability of these blends was shown by the retention of number average molecular weight (Mn) and weight average molecular weight (Mw) after 10 minutes at 305°C.
  • Mn number average molecular weight
  • Mw weight average molecular weight
  • Good melt stability is characterized by a loss of less than about 15% of the original Mn and Mw, after exposure for 10 minutes, the original molecular weights being defined as that at zero time. Blends with less than this degree of melt stability may still be useful, but are correspondingly inferior;
  • PCT poly(cyclohexyienedimethylene terephthalate); PCTA - poly(cyclohexylenedimethylene terephthalate modified with 5 mole% isophthalic acid;
  • Plasticizer A (PL A) - epoxided soybean oil; Plasticizer B - (PL B) - triethyleneglycol-di-2-ethylhexanoate; Plasticizer C - (PL C) - polyethyleneglycol-di-2-ethylhexanoate;
  • Plasticizer D (PL D) - 1 ,4-cyclohexanedimethanol-di-2- ethylehexanoate;
  • Plasticizer E (PL E) - trioctyltrimellitate; Plasticizer F - (PL F) - dioctylterephthalate; Plasticizer G - (PL G) - diundecylphthalate;
  • Stabilizer 2 - (ST 2) - multifunctional bisphenol F epoxy;
  • Stabilizer 4 - (ST 4) tetrakis -[methylene -(3,5-di-tert-butyl-4- hydroxyhydro-cynnamate)];
  • Stabilizer 5 (ST 5) - [bis(2,4-di-t-butylphenyl)pentaerythritol diphosphite
  • the fiber reinforced PCT blends of this work were prepared by extrusion compounding using a twin screw extruder at temperatures of 305°C.
  • the resulting pellets were injection molded into tensile and flexural bars for use in mechanical and flammability property testing.
  • Melt stability was determined on these blends by drying a small sample of the compounded pellets Adequate drying can be obtained by drying in a vacuum oven overnight at 80°C, or by drying for 4 hours at 125°C in a hot air circulating oven.
  • the dried pellets were then loaded into a Tinius Olsen melt indexer or capillary rheometer and held for 10 minutes at 305°C melt temperature, then analyzed by gel permeation chromatography.
  • the melt stability of these blends was shown by the retention of number average molecular weight (Mn) and weight average molecular weight (Mw) after 10 minutes at 305°C.
  • Blends A-D in Table I are described as follows:
  • Blend A is described as follows: 49.3% PCT 30.0% GF1 13.0% FR1
  • Blend B is described as follows:
  • Blend A Same as Blend A except that FR1 is replaced by FR2
  • Blend C is described as follows:
  • Blend D is described as follows:
  • Table 1 illustrates the fact that compositions of the invention containing brominated phthalimides (FR1 ) have a higher heat deflection temperature than brominated polystyrene (FR2) but have inferior melt stability compared to the brominated polystyrene (FR2).
  • compositions used in Table 2 all consist of the following: 48.8% PCT 30.0%) Glass Fibers Type 1
  • FR1 is N,N'-ethylenebis(tetrabromophthalimide; FR2 is brominated polystyrene; FR1-2 is the difference between FR1 & FR2.
  • FR1 halogenated imides
  • FR2 brominated phthalimides
  • FR2 brominated polystyrene
  • Blends E-F in Table 3 are described as follows:
  • Blend E is described as follows: 30.0% GF2 14.0% FR2
  • Stabilizer 4 in an amount sufficient for the composition to total 100 weight%
  • Blend F is described as follows:
  • Blend E Same as Blend E except that the 14.0% FR2 is replaced by 10.5% FR3
  • FR3 behaves similarly to brominated polystyrene (FR2).
  • Blends G-l in Table 4 are described as follows Blend G is described as follows
  • PCT is PCT modified with 5 mole%> isophthalic acid
  • Blend H is described as follows:
  • Blend G Same as Blend G except that the 14.0% FR2 is replaced by 10.5% FR3;
  • Blend I is described as follows:
  • Blend G Same as Blend G except that the 14.0% FR2 is replaced by 12.0% FR1 ;
  • Table 4 illustrates the fact that compositions of the invention containing halogenated imides (FR1) (for example, brominated phthalimides) have a higher heat deflection temperature than those with brominated polystyrene (FR2) but have inferior melt stability compared to the brominated polystyrene (FR2) compositions.
  • FR1 halogenated imides
  • FR2 brominated phthalimides
  • Blends J-0 in Table 5 are described as follows Blend J is described as follows:
  • Blend K is described as follows: 20.0% FR1
  • Blend L is described as follows: 20.0% FR1
  • Blend M is described as follows: 20.0% FR2, and
  • Blend N is described as follows: 20.0% FR2 70.0% PCT
  • Blend O is described as follows: 20.0% FR2 70.0% PCT
  • Blends P-Q in Table 6 are described as follows:
  • Blend P is described as follows: 30.0% GF2 14.0% FR1 3.5% FRS1 3.8% PL L 0.5% ST3
  • PCT in an amount sufficient for the composition to total 100 weight%.
  • Blend Q is described as follows:
  • Blend P Same as Blend P except that the FR1 is increased to 16.0% and FRS1 is decreased to 2.0%
  • Table 6 shows that stability can be improved by increasing the ratio of flame retardant to synergist while maintaining desired flammability characteristics.
  • Blends R-S in Table 7 are described as follows:
  • Blend R is described as follows: 30.0% GF3 16.0% FR1 2.0% FRS2 4.0% PL L 3.0%) Phenoxy 0.5%) polyethylene wax 0.25% ST4 0.25% ST5, and
  • PCT in an amount sufficient for the composition to total 100 weight%.
  • Blend S is described as follows:
  • Blend R Same as Blend R except that ST5 is omitted.
  • Table 7 shows the benefit of using a phosphite.
  • Blends T-U in Table 8 are described as follows: Blend T is described as follows:
  • polyethylene wax 0.25% ST4 0.25% ST5 PCT in an amount sufficient for the composition to total 100 weight%.
  • Blend U is described as follows:
  • Blend T Same as Blend T except that ST5 is present in the amount of 0.75%.
  • Table 8 shows the benefit of increasing the amount of the phosphite beyond the level normally used to stabilize against degradation.

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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)
  • Compositions Of Macromolecular Compounds (AREA)
EP00992197A 1999-09-23 2000-09-05 Verbesserte pct formulierungen enthaltend halogenierte imide, natriumantimonate, und verstärkungfasern Withdrawn EP1228130A2 (de)

Applications Claiming Priority (5)

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US15572399P 1999-09-23 1999-09-23
US155723P 1999-09-23
US45055599A 1999-11-30 1999-11-30
US450555 1999-11-30
PCT/US2000/024376 WO2001025325A2 (en) 1999-09-23 2000-09-05 Improved pct formulations containing halogenated imides, sodium antimonate, and reinforcing fibers

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EP1228130A2 true EP1228130A2 (de) 2002-08-07

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WO (1) WO2001025325A2 (de)

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JP2003511504A (ja) 2003-03-25
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BR0014132A (pt) 2002-05-21
CN1374980A (zh) 2002-10-16

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