• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention is a flame-retardant high-impact polystyrene resin composition having excellent cost / performance showing excellent flame retardancy even with a small amount of flame retardant by applying an environmentally friendly non-halogen flame retardant and a novel flame retardant synergist to a high impact polystyrene resin It is about.
    公开号:KR19980031510A
    申请号:KR1019960051067
    申请日:1996-10-31
    公开日:1998-07-25
    发明作者:김석준；유승일
    申请人:성재갑；주식회사 엘지화학；
    IPC主号:
    专利说明:

    Flame retardant high impact polystyrene resin composition
    The present invention relates to a flame-retardant high-impact polystyrene resin composition, and more particularly to a high-impact polystyrene (HIPS) composition containing a phosphate ester, phosphorus, hydrated metal oxide and / or nitrogen-based flame retardant as a flame retardant The present invention relates to a novel non-halogen-based flame retardant high impact polystyrene resin composition having excellent physical properties by applying a flame retardant synergist to it, and greatly improving economic efficiency and flame retardancy.
    Recently, high impact polystyrene resins have been widely applied to housings of electric, automobiles, home appliances, and office equipment. In particular, the housing of a TV and various monitors can be said to be a main use. However, high-impact polystyrene has a disadvantage of poor flame retardancy because its limited oxygen index (18.2) is well burned in air.
    Conventional flame retardant techniques for improving the disadvantages of such high-impact polystyrene resins include halogen-based flame retardants, antimony oxide synergists, phosphorus-based flame retardants, inorganic metal hydrates, and / or expanded graphite alone or in combination of two or more thereof. Was. However, halogen-based flame retardants containing bromine or chlorine generate hydrogen halides during processing to corrode the processing equipment and provide causes for mold corrosion, resin decomposition, coloring and the like. Resin compositions containing halogen-based flame retardants have poor photochromic resistance (or weather resistance), which is a limitation in using housing parts of home appliances, office equipment, and computers. In addition, even when a fire occurs, a large amount of halogenated compounds may be generated, which may increase lives and property damage. Of these, halogenated dioxins and furans from fire and incineration, which are recently controversial, may harm the lives of residents. In Germany and the Netherlands, polybrominated biphenyls, deca, and octa are used as halogen flame retardants. , And penta, etc., have been legally restricted.
    Therefore, a flame retardant technology using non-halogen flame retardants instead of halogen flame retardants is currently being developed worldwide.
    Many non-halogen flame retardant high impact polystyrene (HIPS) or polystyrene resin compositions have been introduced in patents and literature. In Japan, US Pat. No. 3,663,654, which uses red as a flame retardant for poly (phenylene oxide) / PS (Polystyrene) blends, is used as a flame retardant in Japan with thermoplastics and functional inorganic fillers (or hydrated metal oxides). Patent (JP) No. 50-148447; U.S. Patent No. 3,974,235 with halogen flame retardants and phosphorus or phosphorus-nitrogen compounds applied to EPDM modified PS and PPO blends; and U.S. Patent with piperazine acid polyphosphate and synergists applied to thermoplastics (USP) 4,599,375 and the like. In recent years, literatures using red, magnesium hydroxide and nitrogen compounds in styrene resins, nylons and PBTs (Gerd Blinne, Plastverarbeiter, 44 (12), 78 (1993)) have been reported. Domestic patents include Korean Patent Publication (KR) 96-5077, styrene-acrylonitrile copolymer and polyurethane, which apply triphenyl isocyanurate, phosphorus-containing compound and low melting point glaze to high impact polystyrene. Korean Patent Publication (KR) 96-5079, which applies ammonium polyphosphate and a low melting glaze as a flame retardant to a blend of (Polyurethane), is known.
    In addition, as in the present invention, there are many patents and literature reports on the synergist or the flame retardant assistant. The flame retardant synergy of antimony oxides (antimony trioxide, antimony pentoxide, etc.) in halogen flame retardants is well known. The flame retardant synergistic effect on non-halogen flame retardant is that the retardant synergistic effect of metal oxides (MgO, TiO 2 , ZnO, etc.) is significantly increased when using flame retardant in glass fiber reinforced polyethylene terephthalate (poly (ethylene terephthalate)). (US Pat. No. 3,847,861), and PBT has an excellent flame retardant effect asbestos (asbestos or asbestos, 3MgO.2SiO 2 .2H 2 O) when used as an enemy (German Patents Deutsches Patentamt 2,249,910 and 2,346,056). Is known.
    However, in the prior art, there has been a problem in that the reduction in physical properties due to the use of a large amount of flame retardant is large and the manufacturing cost is high due to the large amount of expensive flame retardant. Therefore, there has been a demand for the development of new flame retardant synergists more efficient and economical.
    It is an object of the present invention to apply a non-halogen-based flame retardant that is economical and environmentally friendly without halogen, and also to apply a new flame retardant synergist to show better flame retardancy even with a small amount of flame retardant and cost / performance. It is to provide a novel high-impact polystyrene resin composition significantly improved.
    As a result of our efforts to achieve the above object, the present inventors have used talc, which is commonly used as a filler in high-impact polystyrene compositions containing phosphate esters, red, hydrated metal oxides, and / or nitrogen-based flame retardants. By applying 2SiO 2 · 2H 2 O) as a novel flame retardant synergist, it was found that a new non-halogen flame retardant high impact polystyrene resin composition having reduced use amount of flame retardant and excellent economical properties and flame retardancy can be obtained. This invention was completed.
    The present invention
    (A) 30 to 90% by weight of high impact polystyrene resin;
    (B) 5 to 75% by weight of a non-halogen-based composite flame retardant comprising at least one component selected from the group consisting of phosphate esters, red, nitrogen-based flame retardants, and hydrated metal oxides;
    (C) 0.5 to 40 weight percent talc;
    (D) 0.01 to 3% by weight of teflon resin
    It provides a flame retardant high-impact polystyrene resin composition and a flame-retardant product prepared therefrom comprising.
    As the method for preparing high impact polystyrene as the component (A), there are known methods of blending rubber into polystyrene resin and graft polymerization of styrene into rubber (Petr Svec and co-researcher, Styrene-). Based Plastics and Their Modification, Ellis Horwood Series in Polymer Science and Technology, pp. 131-145). Mainly used are butadiene rubber or styrene-butadiene, styrene-isoprene, ethylene-propylene-diene monomer or EPDM rubber and copolymers containing styrene In the case of increasing the styrene content, the compatibility is good, the impact strength increases, and the rubber with a styrene content of 20 to 30% is preferred. The content of rubber, particle size, distribution and degree of crosslinking have a great influence on the physical properties. Usually rubber content of 5-30% is preferred in terms of impact strength and other properties. In addition, polystyrene-block-polybutadiene-block-polystyrene (SBS triblock copolymer) is used to improve impact strength. In addition, methacrylate-butadiene-stadiene (MBS), all-acrylic core-shell rubber and ethylene- Propylene rubber, styrene-isoprene-styrene (SIS), ethylene-vinyl acetate (EVA), ethylene-ethyl acrylate (EEA), ethylene-vinyl alcohol (EVOH) copolymer, PBT elastomer, PET elastomer, and / or nylon A system elastic body or the like is used. In addition to the above-mentioned resins, all the rubbers that increase the impact can be used. In addition to the impact modifier, graft copolymers or block copolymer compatibilizers and oligomers or polymer type reactive compatibilizers or dispersants having maleic anhydride, oxazoline and / or epoxy groups in the end groups or side chains may be added when the rubber is modified. Can be. In addition, polyphenylene oxide or modified polyphenylene oxide, polybutylene terephthalate, polyacetal, polycarbonate, or the like may be blended for the purpose of toughening or improving the appearance. It can also be used in combination with other inexpensive resins for the purpose of increasing the amount. Graft polymerization, a chemical preparation method, is usually prepared by dissolving polybutadiene rubber in a styrene monomer and then polymerizing it by various methods such as bulk or suspension polymerization. In this case, the polybutadiene used may have a degree of polymerization, crosslinking degree, cis content, etc. suitable for the final required physical properties, and two or more polybutadienes having different physical properties may be used. In general, phase inversion occurs during the polymerization, so that polybutadiene particles containing polystyrene particles have a morphology dispersed in a polystyrene matrix. In addition to the styrene monomer, methyl styrene, α-ethyl styrene, isopropyl styrene, t-butyl styrene or halogenated styrene monomer may be used to improve heat resistance and have special physical properties, and styrene or the monomer and maleic anhydride, maleimide, and vinyl cyan monomer ( For example, two or more types of acrylonitrile), acrylate or methacrylate monomers (for example, butyl acrylate, methyl methacrylate, etc.) may be used as a copolymerization method.
    The component (A) may be used in an amount of 30 to 90% by weight of the total resin composition, more preferably 40 to 80% by weight.
    Aliphatic and / or aromatic phosphate esters are used as phosphate esters as one of the components of the composite non-halogen-based flame retardant (B), and chemically similar pyrophosphate, phosphonate, and phosphine oxide ( phosphine oxide and phosphite compounds may also be used. As the phosphate ester compound, triphenyl phosphate (TPP), trixylenyl phosphate (TXP), tricresyl phosphate (TCP) and trinaphthyl phosphate having three identical aromatic groups as monomers are preferred, and tris (isopropyl phenyl) Phosphate, tris (o-phenyl phenyl) phosphate, or tris (p-phenyl phenyl) phosphate may be used and have two or more aromatic groups. Resorcinyl diphenyl phosphate, hydroquinonyl diphenyl phosphate, phenyl diresor Cynyl phosphate, cresyl diphenyl phosphate, xylenyl diphenyl phosphate, phenyl di (isopropylphenyl) phosphate, phenyl dinonylphenyl phosphate, o-phenylphenyl dicresyl phosphate and the like can be used. Polyphosphates that are more than dimers are advantageous in terms of heat resistance and include poly (aryl-arylene phosphate), poly (alkyl-arylene phosphate), or poly (aryl-cyclicalkylene phosphate). Specific examples include resorcinol bis (diphenyl phosphate), hydroquinone bis (diphenyl phosphate), pentaerythritol bis (diphenyl phosphate) and the like. Used as a mixture of various reaction products such as tetramers. All phosphorus-based flame retardants other than those mentioned above in the present invention may be used, and one or two or more thereof may be used in combination. In detail, the polyphosphate ester is a compound represented by the following Chemical Formula 1 and produced by reacting phosphorus oxychloride with divalent aromatic alcohol (or phenol) or aliphatic ring dihydric alcohol with aromatic monovalent phenol.
    [Formula 1]
    Wherein R 1 , R 2 is an alkyl group, an aryl group, an alkylaryl group or a cyclicalkylaryl group, A is a residue of an aromatic dihydric phenol or an alicyclic dihydric alcohol compound and n is an integer between 1 and 20 and commercial The mixture as a product shows the average value of the whole. Aromatic dihydric phenols include hydroquinone, resorcinol, bisphenol-A, bisphenol-S, bisphenol-F, dihydroxy stilbene, dihydroxy azobenzene, dihydroxy methionine groups, and aromatic monohydric phenols. May be phenol, cresol, xylenol, isopropyl phenol, o-phenylphenol or naphthol. Aromatic dihydric phenols, aliphatic ring dihydric alcohols and aromatic monohydric phenols are not limited to the above-mentioned chemicals. Recently, polyphosphate ester compounds in solid form have been developed and commercialized, which can also be used.
    Phosphoric acid ester which is one of the components of the above (B) can be used in an amount of 0 to 15% by weight based on the total resin composition.
    As one of the components of the composite non-halogen-based flame retardant (B), the powder may be used directly, or may be used by blending with a hydrated metal oxide, or a master batch mixed in a thermoplastic resin at a high concentration, and may be dispersed in a resin. In order to suppress the generation of phosphine gas and coating the enemy in a variety of ways is used more safely. Typical coating methods include titanium oxide and synthetic resin, aluminum hydroxide or magnesium hydroxide and synthetic resin, thermosetting resins (melamine or amino resins, urea resins, phenolic resins, alkyd resins, unsaturated polyester resins and / or epoxy resins) alone and Coating with a single layer or multiple layers with a Zn or Ni compound, a thermosetting resin, or the like is known (see Japanese Patent Nos. 61-11132 and 62-21704). In addition, sodium carbonate or the like may be used to suppress phosphine generation, and as the phosphine gas trapping agent, MoS 2 , PbO 2 , AgNO 3 , activated carbon, paraffin oil, or silicone oil may be used. The smaller the mean particle size of the droplet is, the more advantageous it is, and usually within 30 m is appropriate, preferably 20 m or less, and more preferably 5 m or less.
    One of the components of the component (B) may be used in an amount of 0 to 15% by weight, preferably 2 to 10% by weight, most preferably 3 to 8% by weight of the total resin composition.
    The nitrogen-based flame retardant which is one of the components of the composite non-halogen-based flame retardant (B) includes a nitrogen-containing flame retardant or a nitrogen-phosphorus-containing flame retardant. Nitrogen-containing flame retardants include melamine, melamine cyanurate, and triphenylisocyanurate, which have a triazine structure. Melamine phosphate, melamine pyro Phosphate (melamine pyrophosphate), ammonium polyphosphate (ammonium polyphosphate), alkyl amine phosphate (alkyl amine phosphate), piperazine acid polyphosphate (piperazine acid polyphosphate) and the like can be used alone or in combination. In addition, one or two or more of various nitrogen-based flame retardants and / or intumescent additives (eg, polyhydric compounds such as dipentaerythritol, starch, dextrin, inorganic acid, etc.) Can be used.
    As for the nitrogen-based flame retardant content which is one of the components of said (B), 0-30 weight% of the whole resin composition, Preferably 3-20 weight% is used.
    The hydrated metal oxide, which is one of the components of the composite non-halogen-based flame retardant (B), may be used in blend with the powder as an inorganic flame retardant or may be added as a component of the master batch or directly to the mixture. As the hydroxide metal oxide, magnesium hydroxide (Mg (OH) 2 ) is suitable, and aluminum hydroxide (Al (OH) 3 ) which has recently increased the dehydration temperature to 250 ° C. or more may be used. A variety of silanes, titanates, zirconates, zirco aluminates and / or organosilicon compounds are used to treat various coupling agents on the surface of the metal oxides by increasing the adhesion between the metal hydroxides and the resins and improving their physical properties. organosilicone chemicals), stearic acid and the like are suitable. In addition, in the case of the hydrous metal oxide which is not surface-treated, a coupling agent may be directly mixed with the composition.
    The hydrated metal oxide, which is one of the constituents of (B), may be used in 0 to 20% by weight of the total resin composition.
    The talc, which is the component (C), is also called talc as an essential component, and the theoretical composition formula is hydrated magnesium silicate having 3MgO.4SiO 2 .H 2 O or 31.7% MgO, 63.5% SiO 2 and 4.8% H 2 O. Talc is an inorganic material commonly used as a reinforcing filler for plastics, and when applied to polypropylene composite resins, talc greatly increases stiffness, creep resistance, and the like. Commercial talc has some impurities and slightly different base composition depending on the origin of the ore. In some cases, soapstone, asbestos, diatomite, pyrophyllite, perlite, etc., which are classified in the same group as talc, may also be used. Talc with reduced impurities may be used for special purposes, such as washing, drying, firing or semi-baking. The talc is mainly used when the average particle size is 100 μm or less, preferably 3 μm or less. Regardless of the shape of the talc particles, those having a plate-like shape are usually used. Factors affecting the resin properties include talc particle size, particle size distribution and surface treatment. Talc is advantageous as long as it is surface treated to suit the application resin. Various coupling agents are used as surface treatments to increase the adhesion to the resin to improve the overall physical properties, such as silane, titanate, zirconate, zirco aluminate, organosilicon compound, stearic acid and the like. It is also possible to use talc without surface treatment, in which case a coupling agent may be added separately.
    The talc of the component (C) is used in an amount of 0.5 to 40% by weight, preferably 1 to 20% by weight, more preferably 2 to 12% by weight of the total resin composition.
    The teflon of the component (D) is added as an antidropping agent, and those having various properties such as its molecular weight and copolymer composition are suitable for the resin.
    Teflon is used in an amount of 0.01 to 3.0% by weight, preferably 0.05 to 1% by weight, most preferably 0.08 to 0.4% by weight of the total resin composition.
    In addition, the flame retardant resin composition may further contain various inorganic and / or organic fillers such as fiber, plate and / or particle form in order to increase the mechanical properties, heat resistance and numerical stability of the composition. Examples of fillers that may be used include carbon fibers, glass fibers, aramid fibers, mineral fibers, potassium titanate whiskers, silicon carbide fibers, boron carbide fibers, aramid pulp, glass flakes, mica, kaolin Clay, barium sulfate (BaSO 4 ), calcium carbonate, molybdenum disulfide, carbon black, conductive carbon black, metal oxide, wollastonite, asbestos, feldspar, nephelline, and the like. As is known in the patents and literature, some have a synergistic effect or no effect or antagonism.
    The filler is used in an amount of 5 to 60 parts by weight, preferably 10 to 40 parts by weight based on 100 parts by weight of the flame retardant resin composition containing the components (A) to (D).
    In addition, the flame-retardant resin composition of the present invention is a halogen-based flame retardant, silicone flame retardant, lubricant, antioxidant, light stabilizer, mold release agent, pigment, antistatic agent, conductive imparting agent or EMI shielding agent, magnetic imparting agent, antibacterial agent, within the range that physical properties are not impaired It may contain additives such as anti-microbial agents, processing aids, metal deactivators, depressants, and the like.
    The flame-retardant resin composition of the present invention is first mixed with the additive in a mixer according to a conventional method, twin-screw extruder, single-screw extruder, roll-mills, kneader or Various types of products can be manufactured by melt-kneading and injecting one of various processing machines such as a banbury mixer.
    The following examples illustrate and describe the present invention in detail and do not limit the present invention. The content of each component is expressed in weight percent unless otherwise specified. In the following examples the physical properties of the injection molded specimens were measured in the following manner.
    Tensile Strength and Elongation: ASTM D638
    Heat Deflection Temperature: ASTM D648 (with a load of 18.6 kgf / cm 2 )
    Flame retardant: UL (Underwriter's Laboratory) 94 bar vertical combustion test method
    Impact Strength: ASTM D256 (1/8 inch thick, room temperature, Izod notched)
    Examples 1-6
    High-impact polystyrene (HIPS) is LG Chemical's HIPS 66SI grade and Hishgard CPA-15 (85% of phosphorus) from Nippon Chemical Co., Ltd. TPP), Magnesium Hydroxide were used by Kyowa Chemical Co., Ltd., Nitrogen-containing flame retardant, domestic melamine, and Ni-phosphorus-containing flame retardant, Albright Wilson's melamine phosphate. The talc was made in Japan having a particle average size of 3 ㎛ or less. Glass fibers were chopped strand products having a length of 3 mm from Owens Corning Fiberglass. Teflon used a product of DuPont, USA.
    The contents of each component shown in Table 1 and additives such as stabilizers and lubricants (1.7% by weight) were mixed well with a super mixer, melt-kneaded in a twin extruder to form pellets, and then dried and injected. After molding and sufficiently stabilized at room temperature, various physical properties were measured.
    Comparative Examples 1 to 3
    All contents are the same except for replacing the talc of Examples 1, 2, and 5 with kaolin clay (trade name, Translink, USA) in order.
    The results of the measurement of the physical properties are shown in Table 1, and it can be clearly seen that the flame retardant synergistic effect of talc is superior to kaolin clay. In addition, the use of a relatively small amount of flame retardant is slightly superior mechanical properties and excellent performance in terms of economy or price.
    TABLE 1
    As can be seen from the regular examples it can be clearly seen the flame retardant synergistic effect of talc and is superior to the kaolin clay. In addition, the use of a relatively small amount of flame retardant is slightly superior mechanical properties and excellent performance in terms of economy or price.
    权利要求:
    Claims (16)
    [1" claim-type="Currently amended] (A) 30 to 90% by weight of high impact polystyrene resin;
    (B) 5 to 75% by weight of a non-halogen-based composite flame retardant comprising at least one component selected from the group consisting of phosphate esters, red, nitrogen-based flame retardants, and hydrated metal oxides;
    (C) 0.5 to 40 weight percent talc;
    (D) Flame retardant high impact polystyrene resin composition comprising 0.01 to 3% by weight of teflon resin.
    [2" claim-type="Currently amended] The resin composition according to claim 1, wherein component (A) is used at 40 to 80% by weight based on the total resin composition.
    [3" claim-type="Currently amended] The resin composition according to claim 1, wherein the phosphate ester of component (B) is triphenyl phosphate.
    [4" claim-type="Currently amended] The resin composition according to claim 1, wherein the phosphate ester of component (B) is used at 0 to 15% by weight based on the total resin composition.
    [5" claim-type="Currently amended] The resin composition according to claim 1, wherein the product of component (B) is used at 0 to 15% by weight based on the total resin composition.
    [6" claim-type="Currently amended] A resin composition according to claim 5, wherein the product of component (B) is used in an amount of 2 to 10% by weight based on the total resin composition.
    [7" claim-type="Currently amended] The resin composition according to claim 6, wherein the product of component (B) is used at 3 to 8% by weight based on the total resin composition.
    [8" claim-type="Currently amended] 2. The nitrogen-based flame retardant of component (B) is selected from the group consisting of melamine, melamine cyanurate, melamine phosphate, melamine pyrophosphate, ammonium polyphosphate, alkylamine phosphate, melamine resin, or urea resin. Resin composition characterized by the above-mentioned.
    [9" claim-type="Currently amended] The resin composition according to claim 1, wherein the nitrogen-based flame retardant of component (B) is used at 0 to 30% by weight based on the total resin composition.
    [10" claim-type="Currently amended] The resin composition according to claim 9, wherein the nitrogen-based flame retardant of component (B) is used at 3 to 20% by weight based on the total resin composition.
    [11" claim-type="Currently amended] The resin composition according to claim 1, wherein the hydrated metal oxide of component (B) is used at 0 to 20% by weight based on the total resin composition.
    [12" claim-type="Currently amended] The resin composition according to claim 1, wherein component (C) is used at 1 to 20% by weight based on the total resin composition.
    [13" claim-type="Currently amended] The resin composition according to claim 13, wherein component (C) is used at 2 to 12% by weight based on the total resin composition.
    [14" claim-type="Currently amended] The resin composition according to claim 1, wherein the resin composition further contains 5 to 60 parts by weight of a filler with respect to 100 parts by weight of the total resin composition.
    [15" claim-type="Currently amended] The resin composition according to claim 14, wherein the filler is conductive carbon black, glass fiber, carbon fiber, kaolin or mica.
    [16" claim-type="Currently amended] A flame retardant product made from the resin composition as claimed in claim 1.
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    同族专利:
    公开号 | 公开日
    KR100200033B1|1999-06-15|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    法律状态:
    1996-10-31|Application filed by 성재갑, 주식회사 엘지화학
    1996-10-31|Priority to KR1019960051067A
    1998-07-25|Publication of KR19980031510A
    1999-06-15|Application granted
    1999-06-15|Publication of KR100200033B1
    优先权:
    申请号 | 申请日 | 专利标题
    KR1019960051067A|KR100200033B1|1996-10-31|1996-10-31|Flame retardant high impact polystyrene resin composition|
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