Classifications

• • 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
  • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
  • C08K5/0066—Flame-proofing or flame-retarding additives
• • 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
  • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
  • C08J5/18—Manufacture of films or sheets
• • 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
  • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
  • C08K5/3477—Six-membered rings
  • C08K5/3492—Triazines
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates

Definitions

• the present invention relates to a composition
• a composition comprising polycarbonate and from 0.0001% by weight to 0.5% by weight of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-l, 3,5-triazine (CAS No. 204583-39-1) and 0.01% to 30.00% by weight of a flame retardant additive.
• Flame-resistant plastic molding compounds are used for a variety of applications. Typical applications of such plastics are the electrical engineering and electronics, where they u.a. be used for the production of carriers of live parts or in the form of television and monitor housings. But even in the interior trim of rail vehicles or aircraft, flame retardant plastics have found their place. In addition to good flame retardancy, the plastics used must also show other positive properties at a high level. These include, among other mechanical properties, such as a high impact strength and a sufficient long-term stability to thermal stress or against possible damage from exposure to light. In this case, such a combination of properties is not always easy to achieve. Although in plastics with the help of flame retardants usually the desired flame retardancy can be easily adjusted. Often, however, relatively large amounts are required for this, which rapidly leads to a drastic deterioration of other properties such as e.g. the mechanics leads.
• EP 1 308 084 discloses polymer compositions which, in addition to a specific combination of UV absorbers, may additionally contain unspecified flame retardants.
• EP 1 762 591 describes compositions comprising polycarbonate and defined UV
• Polyalkylene (meth) acrylate and compounds of the type of 2,4-bis (4-phenylphenyl) -6- (2-hydroxyphenyl) -1, 3,5-triazines and a second, polycarbonate-containing layer In US 6,255,483 and in GB 2317174 biphenyl-substituted triazine compounds are described. Mixtures with other additives are mentioned in general terms. However, a specific teaching for providing compositions with improved flame retardance properties is not disclosed in the document.
• An object of the present invention is to provide compositions containing polycarbonate which have improved flame retardancy.
• compositions containing polycarbonate with a synergistic combination of a flame retardant and small amounts of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-1,3,5-triazine improves the flameproofing properties of the composition to a surprisingly high degree.
• the present invention thus relates to a composition
• a composition comprising polycarbonate and from 0.0001% by weight to 0.5% by weight of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-l, 3,5-triazine (CAS No. 204583-39-1) and 0.005% to 30.00% by weight of a flame retardant additive.
• 0.005% by weight to 30.00% by weight of a flame retardant additive is not limited to a single flame retardant additive, but also includes mixtures of flame retardant additives.
• compositions can be used advantageously in various applications. These include, for example, applications in the electrical / electronics sector, such as lamp housings, electrical circuit breakers, power strips or television or monitor housings.
• the compositions according to the invention can be used in the form of panels for architectural or industrial glazings, as linings of rail vehicle and aircraft interiors, to which respectively increased flame retardance requirements are placed.
• the present invention also relates to processes for preparing a composition according to the invention, characterized in that polycarbonate and 0.0001% by weight to 0.5% by weight of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4, 6-di (4-phenyl) phenyl-l, 3,5-triazine (CAS No. 204583- 39-1) and 0.01% by weight to 30.00% by weight of a flame retardant additive are combined and mixed, optionally in Solvent, optionally homogenizing and the solvent is removed.
• Polycarbonates for the compositions according to the invention are homopolycarbonates, copolycarbonates and thermoplastic polyestercarbonates.
• the polycarbonates and copolycarbonates according to the invention generally have average molecular weights (weight average) of from 2,000 to 200,000, preferably from 3,000 to 150,000, in particular from 5,000 to 100,000, very particularly preferably from 8,000 to 80,000, in particular from 12,000 to
• they furthermore preferably have average molecular weights M w of from 16,000 to 40,000 g / mol.
• the preparation is preferably carried out by the phase boundary process or the melt transesterification process and will first be described by way of example in the phase boundary process.
• Preferred starting compounds are bisphenols of the general formula HO-Z-OH, wherein Z is a divalent organic radical having from 6 to 30 carbon atoms and containing one or more aromatic groups.
• Z is a divalent organic radical having from 6 to 30 carbon atoms and containing one or more aromatic groups.
• Examples of such compounds are bisphenols which belong to the group of dihydroxydiphenyls, bis (hydroxyphenyl) alkanes, indanebisphenols,
• Particularly preferred bisphenols belonging to the aforementioned linking groups are bisphenol-A, tetraalkylbisphenol-A, 4,4- (meta-phenylenediisopropyl) diphenol (bisphenol M), 4,4- (para-phenylenediisopropyl) diphenol, N-phenyl- Isatin bisphenol, 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane (BP-TMC), bisphenols of the 2-hydrocarbyl-3,3-bis (4-hydroxyaryl) phthalimidines type, in particular 2-phenyl-3,3-bis (4-hydroxyphenyl) phthalimidine, and optionally mixtures thereof.
• homopolycarbonates based on bisphenol-A and copolycarbonates based on the monomers bisphenol A and 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane are particularly preferred.
• the bisphenol compounds to be used according to the invention are reacted with carbonic acid compounds, in particular phosgene or, during the melt transesterification process, diphenyl carbonate or dimethyl carbonate.
• Polyestercarbonates are obtained by reacting the abovementioned bisphenols, at least one aromatic dicarboxylic acid and optionally carbonic acid equivalents.
• Suitable aromatic dicarboxylic acids are, for example, phthalic acid, terephthalic acid, isophthalic acid, 3,3'- or 4,4'-diphenyldicarboxylic acid and benzophenone dicarboxylic acids.
• a portion, up to 80 mole%, preferably from 20 to 50 mole%, of the carbonate groups in the polycarbonates may be replaced by aromatic dicarboxylic acid ester groups.
• Inert organic solvents used in the interfacial process include, for example, dichloromethane, the various dichloroethanes and chloropropane compounds, tetrachloromethane, trichloromethane, chlorobenzene, and chlorotoluene. Preference is given to using chlorobenzene or dichloromethane or mixtures of dichloromethane and chlorobenzene.
• the interfacial reaction can be catalyzed by catalysts such as tertiary amines, in particular
• N-alkylpiperidines or onium salts are accelerated. Tributylamine, triethylamine and N-ethylpiperidine are preferably used. In the case of the melt transesterification process, the catalysts mentioned in DE-A 42 38 123 are used.
• the polycarbonates can be branched deliberately and controlled by the use of small amounts of branching.
• Some suitable branching agents are: isatin biscresol, phloroglucinol, 4,6-dimethyl-2,4,6-tri- (4-hydroxyphenyl) -hepten-2; 4,6-dimethyl-2,4,6-tri- (4-hydroxyphenyl) heptane;
• the optionally used 0.05 to 2 mol%, based on diphenols, of branching agents or mixtures of the branching agents can be used together with the diphenols but can also be added at a later stage of the synthesis.
• Chain terminators can be used.
• the chain terminators used are preferably phenols such as phenol, alkylphenols such as cresol and 4-tert-butylphenol, chlorophenol, bromophenol, cumylphenol or mixtures thereof in amounts of 1-20 mol%, preferably 2-10 mol%, per mol bisphenol. Preference is given to phenol, 4-tert-butylphenol or cumylphenol.
• Chain terminators and branching agents may be added separately or together with the bisphenol to the syntheses.
• the inventively preferred polycarbonate is bisphenol A homopolycarbonate.
• the polycarbonates according to the invention can also be prepared by the melt transesterification process.
• the melt transesterification process is described, for example, in the Encyclopedia of Polymer Science, Vol. 10 (1969), Chemistry and Physics of Polycarbonates, Polymer
• the aromatic dihydroxy compounds already described in the phase boundary process are transesterified in the melt with carbonic acid diesters with the aid of suitable catalysts and optionally further additives
• Carbonic acid diesters according to the invention are those of the formula (1) and (2)
• the proportion of carbonic acid ester is 100 to 130 mol%, preferably 103 to 120 mol%, particularly preferably 103 to 109 mol%, based on the dihydroxy compound.
• onium salts As catalysts in the context of the invention, basic catalysts such as, for example, alkali metal and alkaline earth metal hydroxides and oxides but also ammonium or phosphonium salts, referred to below as onium salts, are used in the melt transesterification process as described in the cited literature. Onium salts, particularly preferably phosphonium salts, are preferably used here. Phosphonium salts in the context of the invention are those of the formula (3)
• R 1 '4 the same or different Ci-Cjo-alkyl, C 6 -C 0 aryls, C 7 -C 0 aralkyls or C 5 -C 6 - Cycloalkyls can be, preferably methyl or C 6 -C 14 aryls, particularly preferably methyl or phenyl, and
• X may be an anion such as hydroxide, sulfate, hydrogensulfate, bicarbonate, carbonate, a halide, preferably chloride, or an alkoxide of the formula OR where RC 6 -
• the catalysts are preferably "3 mol, particularly preferably based on one mole of bisphenol, in amounts of from 10", are used in quantities of 10 -8 to 10 7 to 10 "4 mol.
• catalysts can be used alone or optionally in addition to the onium salt to increase the rate of polymerization.
• These include salts of alkali metals and alkaline earth metals, such as hydroxides, alkoxides and aryloxides of lithium, sodium and potassium, preferably sodium hydroxide, alkoxide or aryloxide salts. Most preferred are sodium hydroxide and sodium phenolate.
• the amounts of cocatalyst can range from 1 to 200 ppb, preferably from 5 to 150 ppb, and most preferably from 10 to 125 ppb, each calculated as sodium.
• the transesterification reaction of the aromatic dihydroxy compound and the carbonic diester in the melt is preferably carried out in two stages.
• the melting of the aromatic dihydroxy compound and the carbonic diester at temperatures of 80 to 250 0 C, preferably 100 to 230 0 C, particularly preferably 120 to 190 0 C under normal pressure in 0 to 5 hours, preferably 0.25 to 3 hours instead.
• the catalyst is prepared by applying a vacuum (up to 2 mm Hg) and increasing the temperature (up to 260 0 C) by distilling off the monophenol, the oligocarbonate of the aromatic dihydroxy compound and the carbonic acid diester. In this case, the majority of vapors from the process accrue.
• the oligocarbonate thus prepared has an average molecular weight M w (determined by measuring the relative solution viscosity in dichloromethane or in mixtures of equal amounts by weight of phenol / o-dichlorobenzene calibrated by light scattering) in the range from 2000 g / mol to 18 000 g / mol, preferably from 4 000 g / mol to 15,000 g / mol. - o -
• the polycarbonate prepared in the second stage, in the polycondensation by further increasing the temperature to 250 to 320 0 C, preferably 270 to 295 ° C, and at a pressure of ⁇ 2 mm Hg, the polycarbonate prepared. The remainder of the vapors are removed from the process.
• the catalysts can also be used together in combination (two or more).
• alkali / alkaline earth metal catalysts When using alkali / alkaline earth metal catalysts, it may be advantageous to add the alkali / alkaline earth metal catalysts at a later time (eg, after the oligocarbonate synthesis in the second stage polycondensation).
• the reaction of the aromatic dihydroxy compound and the carbonic acid diester to the polycarbonate can be carried out batchwise or preferably continuously, for example in stirred vessels, thin-film evaporators, falling film evaporators, stirred tank cascades, extruders, kneaders, simple disk reactors and high-viscous disk reactors.
• branched poly- or copolycarbonates can be prepared by using polyfunctional compounds.
• the polycarbonates and copolycarbonates according to the invention may also contain other aromatic polycarbonates and / or other plastics such as aromatic polyester carbonates, aromatic polyesters such as polybutylene terephthalate or polyethylene terephthalate, polyamides, polyimides, polyesteramides, polyacrylates and polymethacrylates such as, for example, polyalkyl (meth) acrylates and in particular polymethyl methacrylate, polyacetals, Polyurethanes, polyolefins, halogenated
• Polymers polysulfones, polyethersulfones, polyether ketones, polysiloxanes, polybenzimidazoles, urea-formaldehyde resins, melamine-formaldehyde resins, phenol-formaldehyde resins, alkyd resins, epoxy resins, polystyrenes, copolymers of styrene or of alpha-methylstyrene with dienes or acrylic derivatives, graft polymers based on acrylonitrile / butadiene / styrene or acrylate rubber-based graft copolymers (see, for example, those described in EP-A 640 655)
• Graft polymers or silicone rubbers are admixed in a known manner, for example by compounding.
• the polycarbonates according to the invention and optionally further plastics contained can also be added in the conventional amounts of the usual additives for these thermoplastics such as fillers, UV stabilizers, thermal stabilizers, antistatic agents and pigments; if necessary, the demolding behavior, the flow behavior, and / or the flame retardancy can be improved by the addition of external mold release agents, flow agents, and / or flame retardants (z. Alkyl and aryl phosphites, phosphates, phosphanes, low molecular weight carboxylic acid esters, halogen compounds, salts, chalk, quartz powder, glass and carbon fibers, pigments and combinations thereof). Such compounds are z. In WO 99/55772, pages 15-25, EP 1 308 084 and in the corresponding chapters of the "Plastics Additives Handbook", ed. Hans Zweifel, 5 * Edition 2000, Hanser Publishers, Kunststoff.
• Suitable flame retardants in the context of the present invention include Alkali sans. Alkaline earth salts of aliphatic or aromatic sulfonic acid sulfonamide and sulfonimide derivatives, e.g. Potassium perfluorobutanesulfonate, potassium diphenyl sulfone sulfonate, N- (p-tolylsulfonyl) -p-toluenesulfimide potassium salt, N- (N'-benzylaminocarbonyl) sulfanylimide potassium salt.
• Alkali Alkaline earth salts of aliphatic or aromatic sulfonic acid sulfonamide and sulfonimide derivatives, e.g. Potassium perfluorobutanesulfonate, potassium diphenyl sulfone sulfonate, N- (p-tolylsulfonyl) -p-toluenesulfimi
• Salts which may optionally be used in the molding compositions according to the invention are, for example: sodium or potassium perfluorobutanesulfate, sodium or potassium perfluoromethane sulfonate, sodium or potassium perfluorooctane sulfate, sodium or potassium 2,5-dichlorobenzenesulfate, sodium or potassium 2,4 , 5-trichlorobenzene sulfate, sodium or potassium methylphosphonate, sodium or potassium (2-phenyl-ethylene) -phosphonate, sodium or potassium pentachlorobenzoate,
• organic flame retardant salts are used in amounts of from 0.01% by weight to 1.0% by weight, preferably from 0.01% by weight to 0.8% by weight, particularly preferably from 0.01% by weight to 0.6% by weight. % in each case based on the Gesarntzusarnmen GmbH used in the molding compositions.
• flame retardants are e.g. phosphorus-containing flame retardants selected from the groups of mono- and oligomeric phosphoric and phosphonic acid esters, phosphonateamines, phosphonates, phosphinates, phosphites, hypophosphites, phosphine oxides and phosphazenes, whereby mixtures of several components selected from one or more of these groups can be used as flame retardants Question.
• phosphorus-containing flame retardants selected from the groups of mono- and oligomeric phosphoric and phosphonic acid esters, phosphonateamines, phosphonates, phosphinates, phosphites, hypophosphites, phosphine oxides and phosphazenes, whereby mixtures of several components selected from one or more of these groups can be used as flame retardants Question.
• Other preferably halogen-free phosphorus compounds which are not specifically mentioned here can also be used alone or in any combination with other preferably halogen-free phosphorus
• phosphonatamines into consideration.
• the preparation of phosphonatamines is described, for example, in US Pat. No. 5,844,028.
• Phosphazenes and their preparation are described for example in EP-A 728 811, DE-A 1 961668 and WO 97/40092.
• siloxanes, phosphorylated organosiloxanes, silicones or siloxysilanes as flame retardants, as described in more detail, for example, in EP 1 342 753, in DE 10257079A and in EP 1 188 792.
• phenyltris-trimethylsiloxysilane (CAS No. 2116-84-9) was used.
• R! to R ⁇ O are independently hydrogen, a linear or branched alkyl group up to 6 C-atoms n an average of 0.5 to 50 and
• B is in each case C 1 -C 4 -alkyl, preferably methyl, or halogen, preferably chlorine or bromine
• q are each independently 0, 1 or 2
• R 1 and R 22 are individually selectable for each Y, independently of one another hydrogen or C 1 -C 6 -alkyl, preferably hydrogen, methyl or ethyl,
• n is an integer from 4 to 7, preferably 4 or 5, with the proviso that on at least one atom Y R.21 and R ⁇ 2 are simultaneously alkyl,
• the degree of oligomerization n results as an average value from the preparation of the listed phosphorus-containing compounds.
• the degree of oligomerization is usually at n ⁇ 10.
• n 1 between 60% and 100%, preferably between 70 and 100%, particularly preferably between 79% and 100%.
• the above compounds may also contain small amounts of triphenyl phosphate.
• the amounts of this substance are usually less than 5 wt .-%, wherein compounds are preferred in the present context, whose Triphenylphosphatgehalt in the range of 0 to 5%, preferably from 0 to 4%, particularly preferably from 0 to 2.5% based on the compound of the formula (4) is located.
• the phosphorus compounds of the formula (4) are used in amounts of 1% by weight to 30% by weight, preferably 2% by weight to 20% by weight, particularly preferably 2% by weight to 15% by weight, based in each case on the total composition.
• the phosphorus compounds mentioned are known (cf., for example, EP-A 363 608, EP-A 640 655) or can be prepared by known methods in an analogous manner (eg Ullmann's Encyclopedia of Industrial Chemistry, Vol. 18, pp. 301 et seq. Houben-Weyl, Methods of Organic Chemistry, Vol. 12/1, p 43; Beilstein, Vol. 6, p. 177).
• Bisphenol A diphosphate is particularly preferred in the context of the present invention.
• Bisphe- nol A diphosphate is including as Reofos ® BAPP (Chemtura, Indianapolis, USA), NcendX ® P-30 (Albemarle, Baton Rouge, Louisiana, USA), Fyrolflex ® BDP (Akzo Nobel, Arriheim,
• CR 741 ® (Daihachi, Osaka, Japan) are commercially available.
• More organophosphate which may be used within the scope of the present invention also are triphenyl phosphate, which among other things as Reofos ® TPP (from Chemtura), Fyrolflex ® TPP (Akzo Nobel) or Disflamoll ® TP (Lanxess) is offered and resorcinol diphosphate.
• Resorcinol diphosphate can be purchased as Reofos RDP (Chemtura) or Fyrolflex ® RDP (Akzo Nobel).
• PTFE polytetrafluoroethylene
• the latter is commercially available in various product qualities. These include additives such as Hostaflon TF2021 ® or PTFE blends as Metablen ® A-3800 (40% PTFE CAS 9002-84- 0 and about 60% methyl methacrylate / butyl acrylate copolymer CAS 25852-37-3 from Misubishi-
• Blendex B449 ® about 50% PTFE and about 50% SAN [from 80% styrene and 20% acrylonitrile] from Chemtura).
• PTFE is used in amounts of 0.05% by weight to 5% by weight, preferably 0.1% by weight to 1.0% by weight, more preferably 0.1% by weight to 0.5% by weight, based in each case on Total composition used.
• halogen-containing compounds include brominated compounds such as brominated oligocarbonates (e.g.
• DSB Dead Sea Bromine
• brominated oligo- or polystyrenes eg Pyro-Chek ® 68PB from Ferro Corporation, PDBS 80 and Fire Master ® PBS-64HW from Chemtura.
• brominated oligocarbonates based on bisphenol A in particular tetrabromobisphenol A oligocarbonat.
• bromine-containing compounds are used in amounts of 0.1% by weight to 30% by weight, preferably 0.1% by weight to 20% by weight, more preferably 0.1% by weight to 10% by weight and most preferably 0.1 Gew% to 5.0% by weight in each case based on the total composition used.
• chlorine-containing flame retardants such as Tetrachlorphthalirnide can be used.
• tetrachlorophthalamides according to the invention of the formula (7) are: N-methyltetrachlorophthalimide, N-ethyltetrachlorophthalimide, N-propyltetrachlorophthalimide, N-isopropyltetrachlorophthalimide, N-butyltetrachlorophthalimide, N-isobutene t-tetrachlorophthalimide, N-phenyltetrachlorophthalimide, N- (4-chlorophenyl) tetrachlorophthalimide, N- (3,5-dichlorophenyl) tetrachlorophthalimide, N- (2,4,6-trichlorophenyl) -tetrachlorophthalimide, N-naphthyltetrachlorophthalimide.
• Tetrachlo ⁇ hthalimideim Examples of the invention according to formula (7) are: N, N, N
• NN 1 propylene-tetrachlorophthalimide N, N'-butylene-di-tetrachlorophthalimide N, N'-p-phenylene-di-tetrachlorophthalimide, 4,4'-di-tetrachlorophthalimido-diphenyl, N- (tetrachlorophthalimido) -tetrachlorophthalimide.
• N-methyl and N-phenyl tetrachlorophthalimide Particularly suitable for the purposes of the invention are N-methyl and N-phenyl tetrachlorophthalimide, N, N'-ethylene-di-tetrachl ⁇ hthalimid and N- (Tetrachlo ⁇ hthalimido) - tetrachlorophthalimide.
• the abovementioned chlorine-containing compounds are used in amounts of 0.1% by weight to 30% by weight, preferably 0.1% by weight to 20% by weight, more preferably 0.1% by weight to 10% by weight and most preferably 0 , 1% by weight to 5.0% by weight, based in each case on the total composition.
• the bromine- or chlorine-containing flame retardants can also be used in combination with
• Antimony trioxide are used.
• the flame retardants mentioned can be used alone or in a mixture, but always together with 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-l, 3,5-triazine (CAS No. 204583-39-1).
• 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-1,3,5-triazine (CAS No. 204583-39-1 ) in amounts of 0.0001 according to the invention
• % By weight to 0.5% by weight, preferably 0.0001% by weight to 0.3% by weight, particularly preferably 0.001% by weight to 0.25% by weight, based in each case on the total composition.
• the present invention is not limited to said flame retardants, but other flame retardant additives, such as. in J. Troitzsch, "International Plastics Flammability Handbook", Hanser Verlag, Kunststoff 1990 described.
• composition comprising polycarbonate and 0.0001% to 0.5% by weight of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-1 , 3,5-triazine (CAS No. 204583-39-1) and 0.01% by weight to 30.00% by weight of a flame retardant additive is carried out by customary incorporation methods and can be prepared, for example, by mixing solutions of the flame retardant additive and the 2 - [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-1,3,5- _
• triazine with a solution of polycarbonate in suitable solvents such as dichloromethane, haloalkanes, haloaromatics, chlorobenzene and xylenes done.
• suitable solvents such as dichloromethane, haloalkanes, haloaromatics, chlorobenzene and xylenes.
• the substance mixtures are then preferably homogenized in a known manner by extrusion.
• the solution mixtures are preferably worked up in a known manner by evaporation of the solvent and subsequent extrusion of the mixture, for example compounded.
• composition can be mixed in conventional mixing devices such as screw extruders (for example twin-screw extruder, ZSK), kneaders, Brabender or Banbury mills and then extruded. After extrusion, the extrudate can be cooled and comminuted. It is also possible to premix individual components and then to add the remaining starting materials individually and / or likewise mixed.
• compositions according to the invention can be worked up in a known manner and processed to give any shaped bodies, for example by extrusion, injection molding or extrusion blow molding.
• Coextruded polycarbonate solid plates can, for. B. with the help of the following machines and Appa- rates are manufactured:
• Coextruded polycarbonate web plates can, for. B. using the following machines and apparatus:
• the coexadapter feedblock system
• a coextruder for applying the cover layer with a screw of length 25 D and a diameter of 30 mm
• the polycarbonate granules of the base material are fed to the hopper of the main extruder, the coextrusion material of the coextruder.
• the melting and conveying of the respective material takes place. Both material melts are combined in the coexadapter and form a composite after leaving the die and cooling.
• the other facilities are used for transporting, cutting and depositing the extruded sheets.
• Sheets without a coextrusion layer are prepared accordingly either by not operating the coextruder or by filling it with the same polymer composition as the main extruder.
• the flame retardancy of plastics can be determined, for example, by the method UL94V (see a) Underwriters Laboratories Inc. Standard of Safety, "Test for Flammability of Plastic Materials for Parts in Devices and Appliances", S 14 ff, Northbrook 1998; J. Troitzsch, "International Plastics Flammability Handbook", p. 346 ff., Hanser Verlag, Kunststoff 1990). In this case, afterburning times and dripping behavior of ASTM standard test specimens are evaluated.
• the UL94V-1 rating requires that the individual afterburn times be no longer than 30 seconds and that the sum of the afterburn times of 10 flashings of 5 samples be no greater than 250 seconds. The total afterglow time must not exceed 250 seconds.
• Classification UL94V-2 shall be considered to result in a burning dripping if the other criteria of UL94V-1 classification are met.
• test specimens can also be assessed by determining the oxygen index (LOI according to ASTM D 2863-77).
• LOI oxygen index
• Another test of the flame retardancy consists of the glow wire test according to DIN IEC 695-2-1. This is carried out on 10 test specimens (for example on plates of geometry 60 x 60 x 2 mm or 1 mm) with the aid of a glowing wire at temperatures between 550 and 960 0 C the maximum
• the glow wire ignition test according to IEC 60695-1-13, the main focus is on the ignition behavior of the test specimen.
• the sample must not ignite during the test procedure, with ignition being defined as a flame phenomenon for more than 5 seconds. A burning dripping of the sample is not permitted.
• the impact resistance can be determined according to DIN EN ISO 180, EN ISO 20180, ASTM D256, DIN EN ISO 179, DIN EN 20179, DESf 53453 or corresponding standards.
• the determination of the IZOD notched impact strength can be carried out, for example, in accordance with ISO 180/1 A, ISO 180/1 AR or according to ISO 180 / 1B on specimens of geometry 80 * 10 * 4 mm 3 or according to ISO 180 / 4A on specimens of geometry 63 , 5 * 12,7 * 3,2 mm 3 .
• the measurement of Charpy impact strength is carried out, for example, in accordance with ISO 179 / leA, ISO 179 / leB or ISO 179 / leC or ISO 179 / lfA, ISO 179 / lfB or ISO 179 / lC on test specimens of geometry 80 * 10 * 4 mm 3 or 63.5 * 12.7 * 3.2 mm 3 .
• the impact toughness of notched and uncut specimens can be determined in accordance with DIN EN ISO 8256, DIN EN 28256, DIN 53448 or corresponding standards.
• B. bending elastic modulus, bending stress at conventional deflection (3.5% bending stress), bending strength, flexural strength at flexural strength, bending stress at break or bending elongation at break provides a bending test according to DIN EN ISO 178, DIN EN 20178, DIN 53452/53457, DIN EN 63, ASTM D790 or equivalent standards.
• the Vicat softening temperature (VST) can be determined according to DIN ISO 306, ASTM D 1525, or equivalent standards.
• the weathering of samples can be carried out by various methods. These include the Xenon WOM method according to ASTM G6, ASTM G151, ASTM Gl 55, DIN EN ISO 4892-2, SAE J 1885 or VDA 75202, the LSL-WOM method according to DIN EN ISO 4892-3, the Xenotest ® High Energy according to DIN EN ISO 4892-2 or DIN EN 50014, the spray test according to ASTM Bl 17, DIN 50021, DIN EN ISO 7253, DIN EN 9227 or ISO 11503 and the QUV test according to ISO 4892-3 or ASTM Gl 54 and ASTM G53.
• melt index (MFR, MVR) is carried out according to ISO 1133 or according to ASTM D1238 MVR.
• melt viscosity is measured in accordance with ISO 11443 or DIN 54811.
• Solution viscosities can be determined, for example, according to the standards ISO 1628-1 / -4 or DIN 51562-3.
• the determination of the degree of gloss can be carried out with a reflectometer on plates of the geometry 60 * 40 * 2 mm 3 , whereby not only thicknesses of 2 mm but also those of 3 mm, 3.2 mm and 4 mm are considered.
• the DIN 67530, ISO 2813, ASTM D523 or corresponding standards are used.
• Turbidity and transmission determinations are carried out in accordance with DIN 5036, ASTM D1003, ASTM E179 or ISO 13468.
• the yellowness index YI is calculated according to ASTM E313.
• Reflection measurements can be carried out according to DIN 5036 or ASTM E179.
• the ISO 105-A02 can be used to determine the gray scale.
• the device for compounding consists of:
• a co-rotating twin-screw mixer (ZSK 53 from Werner & Pfleiderer) with a screw diameter of 53 mm
• Makrolon ® 2808 550115 is commercially available from Bayer MaterialScience AG.
• Makrolon ® 2808 550115 is EU / FDA quality and does not contain UV absorber.
• the melt volume-flow rate (MVR) according to ISO 1133 is 9.5 CM7 (10 min) at 300 0 C and 1.2 kg load.
• Makrolon ® 3108 550115 is commercially available from Bayer MaterialScience AG.
• Makrolon ® 3108 550115 is EU / FDA quality and does not contain UV absorber.
• the melt volume-flow rate (MVR) according to ISO 1133 is 6.0 CM7 (10 min) at 300 0 C and 1.2 kg tung Belas-.
• the procedure is such that weight 75. Wt.% Of a powder mixture of Makrolon ® 3108 550115 powder containing the substances mentioned in the examples, is metered in , the bisphenol-a diphosphate is prepared by adding 20.% of a compound previously prepared from 85 wt.% Makrolon ® 3108 550115, and 15 wt.% of bisphenol-a diphosphate (NcendX ® P-30 from Albemarle) added.
• the device for compounding the bisphenol A diphosphate compound consists of:
• a co-rotating twin-screw mixer (Evolum 32 High Torque from Clextral) with a screw diameter of 32 mm
• Makrolon ® 3108 550115 • 0.10% by weight of 2- [2-hydroxy-4- (2-ethylhexyl) oxy] phenyl-4,6-di (4-phenyl) phenyl-1,3,5-triazine
• Blendex B449 ® from Chemtura a PTFE / SAN blend, weight ratio 50:50
• the compounds of Examples 1 to 12 are then processed into test specimens of geometry 63.5 * 12.7 * 3.2 mm 3 . This is done with an Arburg Allrounder 270S-500-60 with a screw diameter of 18 mm.
• the compounds of Examples 10, 13 and 14 are then processed into test specimens of geometry 63.5 * 12.7 * 1.0 mm 3 . This is done with an Arburg Allrounder 270S-500-60 with a screw diameter of 18 mm.

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