WO2020011058A1 - Polycarbonate composition and preparation method therefor and application thereof - Google Patents

Polycarbonate composition and preparation method therefor and application thereof Download PDF

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WO2020011058A1
WO2020011058A1 PCT/CN2019/094312 CN2019094312W WO2020011058A1 WO 2020011058 A1 WO2020011058 A1 WO 2020011058A1 CN 2019094312 W CN2019094312 W CN 2019094312W WO 2020011058 A1 WO2020011058 A1 WO 2020011058A1
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polycarbonate composition
flame retardant
composition according
parts
polycarbonate
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PCT/CN2019/094312
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French (fr)
Chinese (zh)
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李明昆
黄险波
叶南飚
岑茵
吴俊�
彭民乐
欧俊麟
丁超
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金发科技股份有限公司
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Publication of WO2020011058A1 publication Critical patent/WO2020011058A1/en

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    • 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
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
    • 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
    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
    • 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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • 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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Definitions

  • the invention relates to the technical field of engineering plastics, in particular to a polycarbonate composition and a preparation method and application thereof.
  • PC Polycarbonate
  • PC resin has comprehensive and balanced mechanical properties, dimensional stability, and heat resistance, and is particularly known for its excellent impact strength and creep resistance.
  • PC resin has a visible light transmittance of more than 90%, high thermal decomposition temperature, and excellent electrical insulation. It is widely used in many fields such as machinery, automobiles, aerospace, construction, electronics, office and household goods, especially in Polycarbonate insulation films for electrical and electronic applications are widely used.
  • Polycarbonate insulation film for electronic and electrical applications whose thickness level is less than 0.5mm, can be divided into non-flame retardant and flame retardant types.
  • the flame retardant type insulation film is the application development trend.
  • As a thin material for electronic component materials For the development and safety performance guarantee, it is necessary to have stable flame retardancy in a reduced thickness to reduce the thermal damage from electronic components. To this end, it is also necessary to ensure high heat resistance and storage resistance. At the same time, its folding performance, voltage resistance and heat resistance are also expected.
  • many polycarbonate compositions can provide a beneficial combination of the aforementioned properties, there have been no reports of very thin polycarbonate materials to achieve the desired flame retardancy performance in demanding electrical insulation applications.
  • sulfonate flame retardants can promote the cross-linking of PC to char during the combustion process of PC, thereby improving the flame retardancy of PC. Degraded performance and flame retardancy.
  • Mineral filler is a common flame retardant synergistic component, but its surface is generally alkaline, which may cause the risk of degradation of the PC matrix, and its application in PC flame retardant compositions is limited.
  • the primary object of the present invention is to provide a flame retardant and anti-drip effect that can achieve good flame retardant viscosity at a low combustion temperature, and in the case of a film with a flame retardant thickness of 0.40 mm Polycarbonate composition that still has good flame retardancy and thermal stability, as well as molding appearance.
  • Another object of the present invention is to provide a method for preparing the polycarbonate composition.
  • a polycarbonate composition including by weight parts, the following composition:
  • the viscosity average molecular weight of the polycarbonate is 18000-50000.
  • the viscosity average molecular weight is calculated by using the viscosity of a solution of dichloromethane as a solvent at a test temperature of 25 ° C.
  • the sulfonate flame retardant is selected from one or more of potassium perfluoroalkylsulfonate, potassium benzenesulfonylbenzenesulfonyl, and sodium p-toluenesulfonate, and is preferably potassium perfluorobutylsulfonate.
  • the viscosity of the synergistic flame retardant at a melting point of 140 ° C is 80 mPa ⁇ s-9000 mPa ⁇ s, and the acid value is 6-90; selected from polyolefin oxides, maleic anhydride-modified polyolefins, and acrylates. One or more of these are preferably maleic anhydride-modified polyolefins.
  • the siloxane is selected from polyaminopropylphenylsilsesquioxane, hydroxyl-terminated polyaminopropylsilsesquioxane, polymethylsilsesquioxane, polyphenylsilsesquioxane One or more of polydimethylsiloxane, polymethylphenylsiloxane, and preferably polyphenylsilsesquioxane.
  • the anti-dripping agent is selected from polytetrafluoroethylene, silicone-coated polytetrafluoroethylene, silica-coated polytetrafluoroethylene, methacrylate polymer-coated polytetrafluoroethylene, and propylene.
  • the weight added amount of the silicone is 0.56-1.53 times, preferably 0.75-1.25 times, the weight added amount of the synergistic flame retardant; the weight added amount of the anti-dripping agent is 0.07-1.67 times the amount of addition by weight, preferably 0.5-1.0 times.
  • the polycarbonate composition according to the present invention may further include 0-24 parts of a mineral filler, 0-1 parts of an antioxidant, and 0-1 parts of a lubricant; wherein the mineral filler is selected from talc Powder, titanium dioxide, mica, montmorillonite, kaolin one or more.
  • the present invention also discloses a method for preparing the polycarbonate composition, including the following steps:
  • the components are uniformly mixed in a high-mixer in proportion, added to a twin-screw extruder, melt-mixed at a temperature of 240 ° C-260 ° C, and then pelletized, cooled, and dried to obtain a polycarbonate composition.
  • the invention also discloses the application of the polycarbonate composition in an insulation film in the field of electronics and electricity.
  • the present invention has the following beneficial effects:
  • a specific content and a specific type of anti-dripping agent are added to the formulation of the polycarbonate composition, and a specific content of polycarbonate, a sulfonate flame retardant, a synergistic flame retardant, and a siloxane can be used. Achieve good flame retardancy and anti-drip effect at lower combustion melt viscosity.
  • the polycarbonate composition still has good flame retardancy and thermal stability in the case of 0.40mm film thickness, and molding appearance .
  • Combustion melt index test method Test standard ASTM D1238, 300 ° C, 1.2kg; The definition of combustion melt viscosity is: in the combustion process, the spline receives the same combustion heat, which is generated in the carbon layer. The viscosity of the melt. If the viscosity is too large, the carbon formation rate will be low and the burning time will be too long to cause the test to fail. If the viscosity is too small, it will cause the carbon layer to break down and cause the test to fail.
  • Stable flame retardance can only be achieved within the range, among which V-0 flame retardance stability is judged by the burning time and burning state of the 10 splines, where the A grade represents the burning time of t1 among the ten is less than 3s, and the burning of t2 The average time is less than 3s, the total burning time of a single root does not exceed 7s, and no dripping occurs; the B level represents the burning time of t1 in 10 roots is less than 5s, the burning time of t2 is not limited, and the total burning time of 10 splines Neither can exceed 50s, and no dripping occurs; C level means that the burning time of t1 among the 10 is less than 5s, and the time of t2 is not limited. The total burning time of the 10 splines cannot exceed 50s, and dripping does not ignite;
  • Test method for flame retardancy (0.40mm) The polycarbonate composition is prepared into a 0.40mm film, and the flame retardancy is tested.
  • the test standard is UL94;
  • Test method for notched impact strength at room temperature test standard ASTM D256;
  • Test method for tensile strength test standard ASTM D638;
  • Test method for thermal stability Use TGA initial thermal decomposition temperature to characterize: Use the temperature corresponding to the weight loss rate of 5% in the TGA curve as the initial thermal decomposition temperature; the higher the TGA initial decomposition temperature, the more thermally stable the material is. it is good;
  • Test method for appearance grade cast the material into a film with a thickness of 0.40mm-0.45mm, and measure the surface gloss at 60 ° according to the ASTM D523 standard.
  • a test result greater than 30 is defined as "level 1”
  • a test result of 30-15 is defined as level 2
  • a test result less than 15 is defined as level 3.
  • PC-1 viscosity average molecular weight is 25000
  • PC-2 viscosity average molecular weight is 45000
  • Synergistic flame retardant used in the present invention is a mixture of synergistic flame retardant used in the present invention:
  • Oxidized polyolefin has a viscosity of 8500 mPa ⁇ s and an acid value of 16 at a melting point of 140 ° C;
  • siloxane used in the present invention is a siloxane used in the present invention.
  • Anti-dripping agent used in the present invention is a compound having the following properties:
  • Anti-dripping agent-1 viscosity of 40cps, molecular weight of polytetrafluoroethylene of 500,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-2 viscosity of 15cps, molecular weight of polytetrafluoroethylene of 800,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-3 viscosity is 50cps, molecular weight of polytetrafluoroethylene is 300,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-4 viscosity is 5cps, molecular weight of polytetrafluoroethylene is 500,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-5 viscosity is 80cps, polytetrafluoroethylene has a molecular weight of 500,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-6 viscosity is 40cps, molecular weight of polytetrafluoroethylene is 100,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-7 viscosity is 40cps, molecular weight of polytetrafluoroethylene is 1,000,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-8 viscosity is 5cps, molecular weight of polytetrafluoroethylene is 1,000,000, silicone-coated polytetrafluoroethylene;
  • Anti-dripping agent-9 viscosity of 40cps, molecular weight of polytetrafluoroethylene of 500,000, polytetrafluoroethylene coated with methacrylate polymer;
  • the sulfonate flame retardant used in the present invention potassium perfluorobutyl sulfonate
  • Mineral filler used in the present invention talc, the mesh size is 3000 mesh;
  • Antioxidants used in the present invention a compound of a hindered phenolic antioxidant CHINOX 1076 and a thiol antioxidant JADEWIN AN 412S, and the compounding ratio of the two is 1: 1;
  • Lubricant used in the present invention Pentaerythritol stearate lubricant LOXIOL P861 / 3.5, Corning, Germany.
  • the components are mixed uniformly in a high-mixer, added to a twin-screw extruder, melt-mixed at a temperature of 240 ° C to 260 ° C, and then pelletized, cooled, and dried to obtain polycarbonate.
  • Ester composition Burning melt viscosity, flame retardant thickness, melting index, flame retardant grade (0.40mm), notched impact strength at room temperature, flexural strength, tensile strength, thermal stability, appearance grade, etc. of the polycarbonate composition Performance indicators were tested. The test data is shown in Table 1.

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Abstract

Disclosed by the present invention is a polycarbonate composition, comprising the following components according to parts by weight: a, polycarbonate 0.5-98.5 parts; b, a sulfonate flame retardant 0.15-0.95 parts; c, a synergistic flame retardant 0.03-0.72 parts; d, siloxane 0.04-1.1 parts; e, an anti-dripping agent 0.02-1 parts. In the present invention, a specific content and specific type of anti-dripping agent, and a specific content of polycarbonate, sulfonate flame retardant, synergistic flame retardant and siloxane are selected to be added into a polycarbonate composition formulation, and thus a good flame retardant and drip resistance effect may be attained at a lower combustion melt viscosity, while the polycarbonate composition still has good flame retardancy and thermal stability, as well as molding appearance, in case of a flame retardant film having a thickness of 0.40 mm.

Description

一种聚碳酸酯组合物及其制备方法与应用Polycarbonate composition, preparation method and application thereof 技术领域Technical field
本发明涉及工程塑料技术领域，特别涉及一种聚碳酸酯组合物及其制备方法与应用。The invention relates to the technical field of engineering plastics, in particular to a polycarbonate composition and a preparation method and application thereof.
背景技术Background technique
聚碳酸酯(PC)具有综合均衡的机械性能、尺寸稳定性及耐热性能，特别以优异的抗冲击强度和耐蠕变性著称。PC树脂的可见光透过率在90％以上，热分解温度高，具有优良的电绝缘性，广泛用于机械、汽车、航天航空、建筑、电子电气、办公及家庭用品等诸多领域，尤其是在电子电气应用的聚碳酸酯绝缘膜得到广泛应用。Polycarbonate (PC) has comprehensive and balanced mechanical properties, dimensional stability, and heat resistance, and is particularly known for its excellent impact strength and creep resistance. PC resin has a visible light transmittance of more than 90%, high thermal decomposition temperature, and excellent electrical insulation. It is widely used in many fields such as machinery, automobiles, aerospace, construction, electronics, office and household goods, especially in Polycarbonate insulation films for electrical and electronic applications are widely used.
电子电气应用的聚碳酸酯绝缘膜，其厚度水平低于0.5mm，可以分为非阻燃类和阻燃类型，阻燃类型的绝缘膜是应用发展趋势，作为电子元件材料，材料的薄壁化发展和安全性能保障，需要在减小的厚度具有稳定的阻燃性，来降低受到电子元件发出的热损害，为此还需要保证高的耐热性和耐储存性。同时还对其折叠性能，耐电压性和耐热性是有所期待的。虽然许多聚碳酸酯组合物可以提供上述性能的有益组合，但尚未有非常薄的聚碳酸酯材料来实现所期望的抗阻燃性能在要求苛刻的电气绝缘应用中的性能的相关报道。随着电子设备变成快消品&产品设计薄壁化趋势，绝缘膜增长预计约为20％每年，而且轻薄化，功能化，环保化的发展趋势势必推进无卤阻燃聚碳酸酯薄膜材料在电子电气绝缘应用中成为新起之秀。Polycarbonate insulation film for electronic and electrical applications, whose thickness level is less than 0.5mm, can be divided into non-flame retardant and flame retardant types. The flame retardant type insulation film is the application development trend. As a thin material for electronic component materials, For the development and safety performance guarantee, it is necessary to have stable flame retardancy in a reduced thickness to reduce the thermal damage from electronic components. To this end, it is also necessary to ensure high heat resistance and storage resistance. At the same time, its folding performance, voltage resistance and heat resistance are also expected. Although many polycarbonate compositions can provide a beneficial combination of the aforementioned properties, there have been no reports of very thin polycarbonate materials to achieve the desired flame retardancy performance in demanding electrical insulation applications. As electronic equipment becomes thinner in FMCG & product design, the growth of insulating film is expected to be about 20% per year, and the development trend of lightening, thinning, functionalization and environmental protection is bound to promote halogen-free flame-retardant polycarbonate film materials. Become a rising star in electronic and electrical insulation applications.
然而，磺酸盐阻燃剂在PC燃烧过程中能够促进PC交联成炭，从而提高PC的阻燃性能，但磺酸盐的饱和添加量低，过量使用时反而导致PC严重降解，致力学性能和阻燃性能劣化。为了获得更优异的阻燃效果，需要对磺酸盐阻燃剂进行复配协效，如中国专利CN201510443170。矿物填料是常见的阻燃协效组分，但其表面普遍呈碱性，有导致PC基体降解的风险，在PC阻燃组合物中的应用受到限制。However, sulfonate flame retardants can promote the cross-linking of PC to char during the combustion process of PC, thereby improving the flame retardancy of PC. Degraded performance and flame retardancy. In order to obtain more excellent flame retardant effects, it is necessary to perform synergistic effects on sulfonate flame retardants, such as Chinese patent CN201510443170. Mineral filler is a common flame retardant synergistic component, but its surface is generally alkaline, which may cause the risk of degradation of the PC matrix, and its application in PC flame retardant compositions is limited.
发明内容Summary of the invention
为了克服现有技术的缺点与不足，本发明的首要目的在于提供一种能够在较低燃烧熔体粘度下实现良好的阻燃和抗滴落效果，且在阻燃厚度为0.40mm薄膜情况下仍然具有良好的阻燃性能和热稳定性，以及成型外观性的聚碳酸酯组合物。In order to overcome the shortcomings and deficiencies of the prior art, the primary object of the present invention is to provide a flame retardant and anti-drip effect that can achieve good flame retardant viscosity at a low combustion temperature, and in the case of a film with a flame retardant thickness of 0.40 mm Polycarbonate composition that still has good flame retardancy and thermal stability, as well as molding appearance.
本发明的另一目的是提供上述聚碳酸酯组合物的制备方法。Another object of the present invention is to provide a method for preparing the polycarbonate composition.
本发明的再一目的是提供上述聚碳酸酯组合物的用途。It is still another object of the present invention to provide the use of the polycarbonate composition.
本发明是通过以下技术方案实现的：The present invention is achieved through the following technical solutions:
一种聚碳酸酯组合物，按重量份计，包括以下组成：A polycarbonate composition, including by weight parts, the following composition:
Figure PCTCN2019094312-appb-000001
Figure PCTCN2019094312-appb-000001
其中，所述聚碳酸酯的粘均分子量为18000-50000。其中，粘均分子量是通过使用二氯甲烷作为溶剂在测试温度为25℃的溶液粘度计算出来的。Wherein, the viscosity average molecular weight of the polycarbonate is 18000-50000. Among them, the viscosity average molecular weight is calculated by using the viscosity of a solution of dichloromethane as a solvent at a test temperature of 25 ° C.
其中，所述磺酸盐阻燃剂选自全氟烷基磺酸钾、苯磺酰基苯磺酰钾、对甲苯磺酸钠中的一种或几种，优选为全氟丁基磺酸钾。The sulfonate flame retardant is selected from one or more of potassium perfluoroalkylsulfonate, potassium benzenesulfonylbenzenesulfonyl, and sodium p-toluenesulfonate, and is preferably potassium perfluorobutylsulfonate. .
其中，所述协效阻燃剂在熔点为140℃下的粘度为80mPa·s-9000mPa·s，酸值为6-90；选自聚烯烃氧化物、马来酸酐改性聚烯烃、丙烯酸酯类中的一种或几种，优选为马来酸酐改性聚烯烃。Wherein, the viscosity of the synergistic flame retardant at a melting point of 140 ° C is 80 mPa · s-9000 mPa · s, and the acid value is 6-90; selected from polyolefin oxides, maleic anhydride-modified polyolefins, and acrylates. One or more of these are preferably maleic anhydride-modified polyolefins.
其中，所述硅氧烷选自聚氨丙基苯基倍半硅氧烷、端羟基聚氨丙基倍半硅氧烷、聚甲基倍半硅氧烷、聚苯基倍半硅氧烷、聚二甲基硅氧烷、聚甲基苯基硅氧烷中的一种或几种，优选为聚苯基倍半硅氧烷。Wherein, the siloxane is selected from polyaminopropylphenylsilsesquioxane, hydroxyl-terminated polyaminopropylsilsesquioxane, polymethylsilsesquioxane, polyphenylsilsesquioxane One or more of polydimethylsiloxane, polymethylphenylsiloxane, and preferably polyphenylsilsesquioxane.
其中，所述抗滴落剂选自聚四氟乙烯、硅酮包覆的聚四氟乙烯、二氧化硅包覆聚四氟乙烯、甲基丙烯酸酯聚合物包覆的聚四氟乙烯、丙烯腈包覆的聚四氟乙烯中的一种或几种；优选为硅酮包覆的聚四氟乙烯；更加优选为粘度在25℃下为15cps-50cps，且聚四氟乙烯的分子量为300000-800000的硅酮包覆的聚四氟乙烯。The anti-dripping agent is selected from polytetrafluoroethylene, silicone-coated polytetrafluoroethylene, silica-coated polytetrafluoroethylene, methacrylate polymer-coated polytetrafluoroethylene, and propylene. One or more of nitrile-coated polytetrafluoroethylene; preferably silicone-coated polytetrafluoroethylene; more preferably a viscosity of 15 cps to 50 cps at 25 ° C, and a molecular weight of PTFE of 300,000 -800000 silicone-coated polytetrafluoroethylene.
其中，所述硅氧烷的重量添加量为协效阻燃剂的重量添加量的0.56-1.53倍，优选0.75-1.25倍；所述抗滴落剂的重量添加量为协效阻燃剂的重量添加量的0.07-1.67倍，优选0.5-1.0倍。Wherein, the weight added amount of the silicone is 0.56-1.53 times, preferably 0.75-1.25 times, the weight added amount of the synergistic flame retardant; the weight added amount of the anti-dripping agent is 0.07-1.67 times the amount of addition by weight, preferably 0.5-1.0 times.
本发明所述的聚碳酸酯组合物，按重量份计，还可以包括0-24份矿物填料、0-1份抗氧剂和0-1份润滑剂；其中，所述矿物填料选自滑石粉、钛白粉、云母、蒙脱土、高岭土中的一种或几种。The polycarbonate composition according to the present invention may further include 0-24 parts of a mineral filler, 0-1 parts of an antioxidant, and 0-1 parts of a lubricant; wherein the mineral filler is selected from talc Powder, titanium dioxide, mica, montmorillonite, kaolin one or more.
此外，本发明还公开了上述聚碳酸酯组合物的制备方法，包括如下步骤：In addition, the present invention also discloses a method for preparing the polycarbonate composition, including the following steps:
将各组分按比例在高混机中混合均匀，加入到双螺杆挤出机中，在240℃-260℃的温度下进行熔融混合，然后造粒、冷却、干燥得到聚碳酸酯组合物。The components are uniformly mixed in a high-mixer in proportion, added to a twin-screw extruder, melt-mixed at a temperature of 240 ° C-260 ° C, and then pelletized, cooled, and dried to obtain a polycarbonate composition.
本发明还公开了上述聚碳酸酯组合物在电子电气领域的绝缘薄膜中的应用。The invention also discloses the application of the polycarbonate composition in an insulation film in the field of electronics and electricity.
本发明与现有技术相比，具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明选用在聚碳酸酯组合物配方中添加特定含量以及特定种类的抗滴落剂，和特定含量的聚碳酸酯、磺酸盐阻燃剂、协效阻燃剂和硅氧烷，能够在较低燃烧熔体粘度下实现良好的阻燃和抗滴落效果，该聚碳酸酯组合物在阻燃厚度为0.40mm薄膜情况下仍然具有良好的阻燃性能和热稳定性，以及成型外观性。In the present invention, a specific content and a specific type of anti-dripping agent are added to the formulation of the polycarbonate composition, and a specific content of polycarbonate, a sulfonate flame retardant, a synergistic flame retardant, and a siloxane can be used. Achieve good flame retardancy and anti-drip effect at lower combustion melt viscosity. The polycarbonate composition still has good flame retardancy and thermal stability in the case of 0.40mm film thickness, and molding appearance .
具体实施方式detailed description
下面通过具体实施方式来进一步说明本发明，以下实施例为本发明较佳的实施方式，但本发明的实施方式并不受下述实施例的限制。The following further describes the present invention through specific embodiments. The following examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the following examples.
各性能的测试标准或方法：Test standards or methods for each performance:
燃烧熔体指数的测试方法：测试标准ASTM D1238，300℃，1.2kg；燃烧熔体粘度的定义为：在燃烧过程中，样条收到相同的燃烧热的情况下，在碳层内部产生的熔体的粘度大小，其中粘度过大则会引起成炭速率不高且燃烧时间过长导致测试失败，粘度过小会导致碳层破裂引起的滴落从而测试失败，熔体粘度需要在恰当的范围内才能实现稳定的阻燃稳定性，其中V-0阻燃稳定性通过10根样条的燃烧时间和燃烧状态来判断，其中A等级代表10根中t1的燃烧时间小于3s，t2的燃烧平均时间均小于3s，单根燃烧总时间均不超过7s，且没有出现滴落；B级别代表10根中t1的燃烧时间小于5s，t2的燃烧时间不做限定，10根样条燃烧总时间均不能超过50s，且没有出现滴落；C级别代表10根中t1的燃烧时间小于5s，t2时间不做限定，10根样条燃烧总时间均不能超过50s，出现滴落但不引燃；Combustion melt index test method: Test standard ASTM D1238, 300 ° C, 1.2kg; The definition of combustion melt viscosity is: in the combustion process, the spline receives the same combustion heat, which is generated in the carbon layer. The viscosity of the melt. If the viscosity is too large, the carbon formation rate will be low and the burning time will be too long to cause the test to fail. If the viscosity is too small, it will cause the carbon layer to break down and cause the test to fail. Stable flame retardance can only be achieved within the range, among which V-0 flame retardance stability is judged by the burning time and burning state of the 10 splines, where the A grade represents the burning time of t1 among the ten is less than 3s, and the burning of t2 The average time is less than 3s, the total burning time of a single root does not exceed 7s, and no dripping occurs; the B level represents the burning time of t1 in 10 roots is less than 5s, the burning time of t2 is not limited, and the total burning time of 10 splines Neither can exceed 50s, and no dripping occurs; C level means that the burning time of t1 among the 10 is less than 5s, and the time of t2 is not limited. The total burning time of the 10 splines cannot exceed 50s, and dripping does not ignite;
阻燃等级(0.40mm)的测试方法：将聚碳酸酯组合物制备成0.40mm薄膜，测试阻燃等级，测试标准为UL94；Test method for flame retardancy (0.40mm): The polycarbonate composition is prepared into a 0.40mm film, and the flame retardancy is tested. The test standard is UL94;
室温缺口冲击强度的测试方法：测试标准ASTM D256；Test method for notched impact strength at room temperature: test standard ASTM D256;
弯曲强度的测试方法：测试标准ASTM D790；Bending strength test method: test standard ASTM D790;
拉伸强度的测试方法：测试标准ASTM D638；Test method for tensile strength: test standard ASTM D638;
热稳定性的测试方法：采用TGA初始热分解温度来表征：以TGA曲线中重量损失率为5％时所对应的温度作为初始热分解温度；TGA初始分解温度越高，材料的热稳定性越好；Test method for thermal stability: Use TGA initial thermal decomposition temperature to characterize: Use the temperature corresponding to the weight loss rate of 5% in the TGA curve as the initial thermal decomposition temperature; the higher the TGA initial decomposition temperature, the more thermally stable the material is. it is good;
外观等级的测试方法：将材料流延成0.40mm-0.45mm厚度薄膜，依据ASTM D 523标准测量60°角下的表面光泽度。测试结果大于30则定义为“1级”，测试结果30-15时定义为2级，测试结果小于15时定义为3级。Test method for appearance grade: cast the material into a film with a thickness of 0.40mm-0.45mm, and measure the surface gloss at 60 ° according to the ASTM D523 standard. A test result greater than 30 is defined as "level 1", a test result of 30-15 is defined as level 2, and a test result less than 15 is defined as level 3.
现对实施例及对比例所用的原材料做如下说明，但不限于这些材料：The raw materials used in the examples and comparative examples are described below, but are not limited to these materials:
本发明中使用的聚碳酸酯PC：Polycarbonate PC used in the present invention:
PC-1，粘均分子量为25000；PC-1, viscosity average molecular weight is 25000;
PC-2，粘均分子量为45000；PC-2, viscosity average molecular weight is 45000;
本发明中使用的协效阻燃剂：Synergistic flame retardant used in the present invention:
马来酸酐改性聚烯烃，在熔点为140℃下的粘度为150mPa·s，酸值为60；Maleic anhydride modified polyolefin with a viscosity of 150 mPa · s and an acid value of 60 at a melting point of 140 ° C;
氧化聚烯烃，在熔点为140℃下的粘度为8500mPa·s，酸值为16；Oxidized polyolefin has a viscosity of 8500 mPa · s and an acid value of 16 at a melting point of 140 ° C;
本发明中使用的硅氧烷：The siloxane used in the present invention:
聚苯基倍半硅氧烷，商品牌号KR-2710；Polyphenylsilsesquioxane, trade name KR-2710;
端羟基聚氨丙基倍半硅氧烷，商品牌号FCA-107；Hydroxy-terminated polyaminopropylsilsesquioxane, trade name FCA-107;
本发明中使用的抗滴落剂：Anti-dripping agent used in the present invention:
抗滴落剂-1：粘度为40cps，聚四氟乙烯的分子量为500000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-1: viscosity of 40cps, molecular weight of polytetrafluoroethylene of 500,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-2：粘度为15cps，聚四氟乙烯的分子量为800000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-2: viscosity of 15cps, molecular weight of polytetrafluoroethylene of 800,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-3：粘度为50cps，聚四氟乙烯的分子量为300000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-3: viscosity is 50cps, molecular weight of polytetrafluoroethylene is 300,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-4：粘度为5cps，聚四氟乙烯的分子量为500000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-4: viscosity is 5cps, molecular weight of polytetrafluoroethylene is 500,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-5：粘度为80cps，聚四氟乙烯的分子量为500000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-5: viscosity is 80cps, polytetrafluoroethylene has a molecular weight of 500,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-6：粘度为40cps，聚四氟乙烯的分子量为100000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-6: viscosity is 40cps, molecular weight of polytetrafluoroethylene is 100,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-7：粘度为40cps，聚四氟乙烯的分子量为1000000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-7: viscosity is 40cps, molecular weight of polytetrafluoroethylene is 1,000,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-8：粘度为5cps，聚四氟乙烯的分子量为1000000，硅酮包覆的聚四氟乙烯；Anti-dripping agent-8: viscosity is 5cps, molecular weight of polytetrafluoroethylene is 1,000,000, silicone-coated polytetrafluoroethylene;
抗滴落剂-9：粘度为40cps，聚四氟乙烯的分子量为500000，甲基丙烯酸酯聚合物包覆的聚四氟乙烯；Anti-dripping agent-9: viscosity of 40cps, molecular weight of polytetrafluoroethylene of 500,000, polytetrafluoroethylene coated with methacrylate polymer;
本发明中使用的磺酸盐阻燃剂：全氟丁基磺酸钾；The sulfonate flame retardant used in the present invention: potassium perfluorobutyl sulfonate;
本发明中使用的矿物填料：滑石粉，目数为3000目；Mineral filler used in the present invention: talc, the mesh size is 3000 mesh;
本发明中使用的抗氧剂：受阻酚类抗氧剂CHINOX 1076和硫醇类抗氧剂JADEWIN AN 412S的复配，且两者的复配比为1：1；Antioxidants used in the present invention: a compound of a hindered phenolic antioxidant CHINOX 1076 and a thiol antioxidant JADEWIN AN 412S, and the compounding ratio of the two is 1: 1;
本发明中使用的润滑剂：季戊四醇硬脂酸酯类润滑剂LOXIOL P 861/3.5，德国科宁。Lubricant used in the present invention: Pentaerythritol stearate lubricant LOXIOL P861 / 3.5, Corning, Germany.
实施例1-17及对比例1-8：聚碳酸酯组合物的制备Examples 1-17 and Comparative Examples 1-8: Preparation of Polycarbonate Composition
按表1的配比将各组分在高混机中混合均匀，加入到双螺杆挤出机中，在240℃-260℃的温度下进行熔融混合，然后造粒、冷却、干燥得到聚碳酸酯组合物；对聚碳酸酯组合物的燃烧熔体粘度、阻燃厚度、熔融指数、阻燃等级(0.40mm)、室温缺口冲击强度、弯曲强度、拉伸强度、热稳定性和外观等级等性能指标进行测试，测试数据如表1所示。According to the mixing ratio in Table 1, the components are mixed uniformly in a high-mixer, added to a twin-screw extruder, melt-mixed at a temperature of 240 ° C to 260 ° C, and then pelletized, cooled, and dried to obtain polycarbonate. Ester composition; Burning melt viscosity, flame retardant thickness, melting index, flame retardant grade (0.40mm), notched impact strength at room temperature, flexural strength, tensile strength, thermal stability, appearance grade, etc. of the polycarbonate composition Performance indicators were tested. The test data is shown in Table 1.
表1实施例1-17及对比例1-8的具体配比(重量份)及其测试性能结果Table 1 Specific proportions (parts by weight) of Examples 1-17 and Comparative Examples 1-8 and test performance results thereof
Figure PCTCN2019094312-appb-000002
Figure PCTCN2019094312-appb-000002
续表1Continued Table 1
Figure PCTCN2019094312-appb-000003
Figure PCTCN2019094312-appb-000003
续表2Continued Table 2
Figure PCTCN2019094312-appb-000004
Figure PCTCN2019094312-appb-000004

Claims (10)

  1. 一种聚碳酸酯组合物，按重量份计，包括以下组成：A polycarbonate composition, including by weight parts, the following composition:
    Figure PCTCN2019094312-appb-100001
    Figure PCTCN2019094312-appb-100001
  2. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述聚碳酸酯的粘均分子量为18000-50000。The polycarbonate composition according to claim 1, wherein the polycarbonate has a viscosity average molecular weight of 18,000 to 50,000.
  3. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述磺酸盐阻燃剂选自全氟烷基磺酸钾、苯磺酰基苯磺酰钾、对甲苯磺酸钠中的一种或几种，优选为全氟丁基磺酸钾。The polycarbonate composition according to claim 1, wherein the sulfonate flame retardant is selected from the group consisting of potassium perfluoroalkylsulfonate, potassium benzenesulfonylbenzenesulfonate, and sodium p-toluenesulfonate. One or more, preferably potassium perfluorobutyl sulfonate.
  4. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述协效阻燃剂在熔点为140℃下的粘度为80mPa·s-9000mPa·s，酸值为6-90；选自聚烯烃氧化物、马来酸酐改性聚烯烃、丙烯酸酯类中的一种或几种，优选为马来酸酐改性聚烯烃。The polycarbonate composition according to claim 1, wherein the viscosity of the synergistic flame retardant at a melting point of 140 ° C. is 80 mPa · s-9000 mPa · s, and the acid value is 6-90; One or more of polyolefin oxide, maleic anhydride-modified polyolefin, and acrylates, and preferably maleic anhydride-modified polyolefin.
  5. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述硅氧烷选自聚氨丙基苯基倍半硅氧烷、端羟基聚氨丙基倍半硅氧烷、聚甲基倍半硅氧烷、聚苯基倍半硅氧烷、聚二甲基硅氧烷、聚甲基苯基硅氧烷中的一种或几种，优选为聚苯基倍半硅氧烷。The polycarbonate composition according to claim 1, wherein the siloxane is selected from the group consisting of polyaminopropylphenylsilsesquioxane, hydroxyl-terminated polyaminopropylsilsesquioxane, and polymethylsiloxane One or more of a silsesquioxane, polyphenylsilsesquioxane, polydimethylsiloxane, polymethylphenylsiloxane, preferably polyphenylsilsesquioxane .
  6. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述抗滴落剂选自聚四氟乙烯、硅酮包覆的聚四氟乙烯、二氧化硅包覆聚四氟乙烯、甲基丙烯酸酯聚合物包覆的聚四氟乙烯、丙烯腈包覆的聚四氟乙烯中的一种或几种；优选为硅酮包覆的聚四氟乙烯；更加优选为粘度在25℃下为15cps-50cps，且聚四氟乙烯的分子量为300000-800000的硅酮包覆的聚四氟乙烯。The polycarbonate composition according to claim 1, wherein the anti-dripping agent is selected from the group consisting of polytetrafluoroethylene, silicone-coated polytetrafluoroethylene, silica-coated polytetrafluoroethylene, One or more of methacrylate polymer-coated polytetrafluoroethylene and acrylonitrile-coated polytetrafluoroethylene; preferably silicone-coated polytetrafluoroethylene; more preferably, the viscosity is 25 ° C The following is 15 cps to 50 cps, and the polytetrafluoroethylene has a molecular weight of 300,000 to 800,000 and is a silicone-coated polytetrafluoroethylene.
  7. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，所述硅氧烷的重量添加量为协效阻燃剂的重量添加量的0.56-1.53倍，优选0.75-1.25倍；所述抗滴落剂的重量添加量为协效阻燃剂的重量添加量的0.07-1.67倍，优选0.5-1.0倍。The polycarbonate composition according to claim 1, wherein the weight added amount of the siloxane is 0.56-1.53 times, preferably 0.75-1.25 times, the weight added amount of the synergistic flame retardant; The anti-dripping agent is added in an amount of 0.07-1.67 times, preferably 0.5-1.0 times, the weight-added amount of the synergistic flame retardant.
  8. 根据权利要求1所述的聚碳酸酯组合物，其特征在于，按重量份计，还包括0-24份矿物填料、0-1份抗氧剂和0-1份润滑剂；其中，所述矿物填料选自滑石粉、钛白粉、云母、蒙脱土、高岭土中的一种或几种。The polycarbonate composition according to claim 1, further comprising 0-24 parts of a mineral filler, 0-1 parts of an antioxidant, and 0-1 parts of a lubricant by weight parts; wherein, the The mineral filler is selected from one or more of talc, titanium dioxide, mica, montmorillonite, and kaolin.
  9. 一种如权利要求1-8任一项所述的聚碳酸酯组合物的制备方法，包括如下步骤：A method for preparing a polycarbonate composition according to any one of claims 1 to 8, comprising the following steps:
    将各组分按比例在高混机中混合均匀，加入到双螺杆挤出机中，在240℃-260℃的温度下进行熔融混合，然后造粒、冷却、干燥得到聚碳酸酯组合物。The components are uniformly mixed in a high-mixer in proportion, added to a twin-screw extruder, melt-mixed at a temperature of 240 ° C-260 ° C, and then pelletized, cooled, and dried to obtain a polycarbonate composition.
  10. 如权利要求1-8任一项所述的聚碳酸酯组合物在电子电气领域的绝缘薄膜中的应用。The use of the polycarbonate composition according to any one of claims 1 to 8 in an insulating film in the field of electronics and electricity.
PCT/CN2019/094312 2018-07-12 2019-07-02 Polycarbonate composition and preparation method therefor and application thereof WO2020011058A1 (en)

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CN116285332B (en) * 2023-03-14 2024-05-07 金发科技股份有限公司 Heat-conducting glass fiber reinforced nylon material and preparation method and application thereof

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