WO2020184839A1 - Composition de résine polyamide ignifuge, son procédé de fabrication, et procédé de fabrication d'un produit moulé la comprenant - Google Patents

Composition de résine polyamide ignifuge, son procédé de fabrication, et procédé de fabrication d'un produit moulé la comprenant Download PDF

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Publication number
WO2020184839A1
WO2020184839A1 PCT/KR2020/001621 KR2020001621W WO2020184839A1 WO 2020184839 A1 WO2020184839 A1 WO 2020184839A1 KR 2020001621 W KR2020001621 W KR 2020001621W WO 2020184839 A1 WO2020184839 A1 WO 2020184839A1
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Prior art keywords
flame
polyamide resin
resin composition
retardant
weight
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Ceased
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PCT/KR2020/001621
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English (en)
Korean (ko)
Inventor
정윤선
김한솔
이현석
김형석
황순규
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LG Chem Ltd
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LG Chem Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • 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
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/004—Additives being defined by their length

Definitions

  • the present invention relates to a flame-retardant polyamide resin composition, a method for manufacturing the same, and a method for manufacturing a molded article including the same, and in more detail, the tensile strength and impact strength are greatly improved by using a specific glass fiber, and high It relates to a flame-retardant polyamide resin composition and the like that provide an effect of providing a grade of flame retardancy.
  • Aliphatic polyamides represented by nylon 6 and nylon 66 have excellent properties such as heat resistance, chemical resistance, rigidity, abrasion resistance, and moldability, and are therefore used in many applications as engineering plastics.
  • engineering plastics used in the electric and electronic field in addition to the flame-retardant standard based on UL 94 standard, additional glow-resistant wire characteristics are newly required, and this can be seen as a plan to identify more practical flame-retardant behavior and prevent fire in advance. have.
  • the flame retardant evaluation method of UL 94 standard is a method of simulating the flame retardant behavior based on the premise that a fire has already occurred by using a flame as a heat source, and the method for evaluating the characteristics of the glow wire according to the International Electrotechnical Commission (IEC) standard (Glow Wire) Flammability Index (GWFI) provides a heat source that can cause fire as a glow wire, and by understanding its behavior, it can be seen as an evolved flame retardant test method that considers safety in the event of a fire.
  • IEC International Electrotechnical Commission
  • GWFI Flammability Index
  • Halogen-based flame retardants introduced to impart flame retardancy to polyamides decompose due to low thermal stability due to high temperatures and pressures generated during processing, and as a result, corrosive toxic gases are generated, which adversely affects the working environment and human body.
  • non-halogen-based flame retardants, especially melamine-based flame retardants are being replaced, but melamine-based flame retardants have the advantage that they can achieve flame retardancy with a lower content than halogen-based flame retardants, but when applied to resins reinforced with inorganic fillers, flame retardant grade V- It is difficult to implement 0, and mechanical properties such as tensile properties are deteriorated.
  • the polyamide resin is given a high level of flame retardancy that passes GWFI measured at 960 °C according to the International Electrotechnical Commission (IEC) standard IEC 60695-2-12, and has excellent mechanical properties, especially high tensile properties. There is a need for research on a technology that can implement this.
  • IEC International Electrotechnical Commission
  • the present invention is a flame-retardant polyamide resin that implements flame-retardant properties by using a phosphorus-based flame retardant, and the E-glass type chopped strands glass fiber having a filament diameter of 10.6 to 11.9 ⁇ m. It is intended to provide a flame-retardant polymide resin composition having very excellent mechanical properties such as tensile strength and impact strength as well as flame retardancy by blending, a manufacturing method thereof, and a molded article including the same.
  • the present invention comprises 50 to 75% by weight of a polyamide resin, 5 to 30% by weight of glass fiber having a filament diameter of 10.6 to 11.9 ⁇ m, and 13 to 20% by weight of a phosphorus-based flame retardant, wherein the glass fiber is It provides a flame-retardant polyamide resin composition, characterized in that the chopped strands of the E-glass type have a chopped length of 2 to 6 mm.
  • the present invention comprises a step of kneading and extruding, including 50 to 75% by weight of a polyamide resin, 5 to 30% by weight of glass fiber having a filament diameter of 10.5 to 12 ⁇ m, and 13 to 20% by weight of a phosphorus-based flame retardant, wherein the glass fiber Provides a method of preparing a flame-retardant polyamide resin composition, characterized in that the E-glass type chopped strands have a chopped length of 2 to 6 mm.
  • the present invention provides a molded article comprising the flame-retardant polyamide resin composition.
  • a flame-retardant polyamide resin having a flame-retardant property using a phosphorus-based flame retardant is blended with E-glass type chopped strands glass fibers having a filament diameter of 10.6 to 11.9 ⁇ m in a specific content ratio to UL94 V-
  • E-glass type chopped strands glass fibers having a filament diameter of 10.6 to 11.9 ⁇ m in a specific content ratio to UL94 V-
  • the flame-retardant polyamide resin composition of the present invention comprises 50 to 75% by weight of a polyamide resin, 5 to 30% by weight of glass fiber, and 13 to 20% by weight of a phosphorus-based flame retardant, wherein the glass fiber has a filament diameter of 10.6 to 11.9 ⁇ m. It features, and in this case, it is possible to secure a high level of flame retardancy passing through GWFI, and there is an effect of excellent mechanical strength.
  • the polyamide may be included in 50 to 75% by weight or 56 to 65% by weight, preferably 56 to 61% by weight based on the flame retardant polyamide resin composition, and within this range, mechanical properties, extrusion processability, and appearance quality There is an advantage of excellent balance of physical properties such as.
  • the polyamide resin is a polymer having an amide bond (-NHCO-) in the main chain, and one obtained by condensation polymerization of two or more lactams or w-amino acids having a ring structure may be used.
  • the cyclic lactam may be, for example, ⁇ -caprolactam or ⁇ -laurolactam
  • the w-amino acid is, for example, 6-aminocapronic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid and paraamino. It may be one or more selected from the group consisting of methylbenzoic acid.
  • the polyamide resin may be a polyamide resin in which diacids and diamines are condensed.
  • the diacid is, for example, malonic acid, dimethylmalonic acid, succinic acid, glutaric acid, adipic acid, 2-methyladipic acid, trimethyladipic acid, pimelic acid, 2,2-dimethylglutaric acid, 3,3 -Diethylsuccinic acid, azelaic acid, sebacic acid, sveric acid, dodecanoic acid, eicodioic acid, terephthalic acid, isophthalic acid, naphthalenedicarboxylic acid, 2-chloroterephthalic acid, 2-methylterephthalic acid, 5-methylisophthalic acid , 5-sodium sulfoisophthalic acid, hexahydroterephthalic acid, diglycolic acid, etc., may be one or more selected from the group consisting of aliphatic, alicyclic or aromatic dicarboxylic acids, and the diamine is, for example, tetramethylenediamine, hexamethylene Di
  • the polyamide resin may be one or more selected from the group consisting of nylon 6, nylon 66, nylon 610, nylon 1010, nylon 46, nylon 11, nylon 12, nylon MXD6 and polyphthalamide, for example, and preferably nylon 6 In this case, heat resistance, chemical resistance, and mechanical properties are excellent.
  • the polyamide resin may be, for example, a semi-crystalline or amorphous polyamide resin, and preferably may be semi-crystalline, and in this case, it has excellent effects such as chemical resistance.
  • the semi-crystalline polyamide resin and the amorphous polyamide resin are not particularly limited in the case of a polyamide resin commonly recognized as a semi-crystalline polyamide resin and an amorphous polyamide resin in the technical field to which the present invention belongs.
  • the polyamide resin may have a melting temperature of 150 to 350°C, 200 to 300°C, or 220 to 280°C, for example, and has excellent heat resistance within this range.
  • the polyamide resin may have a relative viscosity (RV) of 1.5 to 5.0, 2 to 4, or 2.0 to 3.5, preferably 2.1 to 2.5, and has excellent moldability and processability within this range.
  • RV relative viscosity
  • the relative viscosity can be measured at 20° C. using a solution prepared by dissolving 1 g of polyamide in 100 ml of a 96% by weight sulfuric acid aqueous solution unless otherwise noted.
  • the polyamide resin may have a number average molecular weight of 8,000 to 100,000 g/mol, 10,000 to 700,000 g/mol, 10,000 to 500,000 g/mol, or 10,000 to 50,000 g/mol, for example, and the appearance of the final molded product within this range Properties, mechanical strength, and the like are improved.
  • the number average molecular weight of this description is a relative value for a standard PS (Standard polystyrene) sample using tetrahydrofuran (THF) as a solvent at a temperature of 40°C through gel chromatography (GPC) filled with porous silica as a column packing material. Can be measured.
  • PS Standard polystyrene
  • THF tetrahydrofuran
  • GPC gel chromatography
  • the glass fiber may be included in an amount of 5 to 30% by weight or 15 to 30% by weight, preferably 20 to 25% by weight, based on the flame-retardant polyamide resin composition, and has excellent surface appearance and tensile properties within this range. It works.
  • the glass fiber may have, for example, a filament diameter of 10.6 to 11.9 ⁇ m or 10.6 to 11.5 ⁇ m, preferably 11.0 to 11.5 ⁇ m, and has a more excellent effect in tensile strength and impact strength within this range.
  • the glass fiber may be, for example, E-glass type chopped strands.
  • the E-glass type is in accordance with ASTM D578-00, for example 52 to 62% by weight silicon dioxide, 12 to 16% by weight aluminum oxide, 16 to 25% by weight calcium oxide, 0 to 10% by weight borax, 0 to 5% by weight magnesium oxide, 0 to 2% by weight alkali metal oxide, 0 to 1.5% by weight titanium dioxide and 0 to 0.3% by weight iron oxide.
  • the E-glass type is 52 to 62% by weight silicon dioxide, 12 to 16% by weight aluminum oxide, 16 to 25% by weight calcium oxide, 0.1 to 10% by weight borax, 0.1 to 5% by weight magnesium oxide, 0.01 to It is composed of 2% by weight of alkali metal oxide, 0.01 to 1.5% by weight of titanium dioxide and 0.001 to 0.3% by weight of iron oxide.
  • the glass fiber is characterized in that, for example, chopped strands having a chopped length of 2 to 6 mm or 3.0 to 4.5 mm, preferably 3.0 to 3.5 mm, and tensile strength and impact within this range The strength is more excellent effect.
  • the filament diameter and the swell length of the glass fiber were measured by SEM (Scanning Electron Microscope) for 30 pieces, and the average value was calculated.
  • the glass fiber may be surface-treated with a silane-based compound as an example, and in this case, the glass fiber is evenly dispersed in the polyamide resin due to its excellent compatibility with the polyamide resin, and thus mechanical properties and thermal properties are excellent, It has an excellent effect on the surface properties of.
  • the silane-based compound is not particularly limited if it is an amino silane used as a coating agent for glass fibers, but examples include gamma-glycidoxypropyl triethoxy silane, gamma-glycidoxypropyl trimethoxy silane, gamma-gly Cydoxypropyl methyldiethoxy silane, gamma-glycidoxypropyl triethoxy silane, 3-mercaptopropyl trimethoxy silane, vinyl trimethoxysilane, vinyl triethoxy silane, gamma-methacryloxypropyl trimethoxy Silane, gamma-methacryloxy propyl triethoxy silane, gamma-aminopropyl trimethoxy silane, gamma-aminopropyl triethoxy silane, 3-isocyanato propyltriethoxy silane, gamma-acetoacetatepropyl trimethoxy It may be one or more selected
  • the glass fiber may be, for example, CPIC's ECS301HP-3-H (filament diameter 11 ⁇ m), and in this case, it is readily available, and the quality or composition is determined so that there is no change, excellent reproducibility. In particular, the tensile properties and Mechanical properties such as impact strength are more excellent.
  • the glass fiber may be characterized by having a limiting oxygen index (LOI) of 0.45 ⁇ 0.1% by volume, for example, and in this case, the composition has excellent properties such as tensile strength and impact strength.
  • LOI limiting oxygen index
  • the limiting oxygen index of the glass fiber is a value measured according to ISO 1887.
  • the glass fiber may be characterized by having a water content of 0.05% by weight or less, for example, and in this case, the mechanical properties of the composition are excellent.
  • the moisture content of the glass fiber is a value measured according to ISO 3344.
  • the glass fiber may be characterized by having a bulk density of 0.7 ⁇ 0.1 g/cm 3 , for example, and in this case, the product molding of the composition and the balance of physical properties are excellent.
  • the bulk density of the glass fiber is a value measured according to ISO 15100.
  • the glass fiber may be, for example, a fiber having a circular cross section, and in this case, both the appearance quality and mechanical properties of the final product may be excellent.
  • the phosphorus-based flame retardant may be included in an amount of 13 to 20% by weight, or 15 to 20% by weight, preferably 15 to 19% by weight, based on the flame-retardant polyamide resin composition, and within this range, the IEC 60695-2-12 standard It passes through the GWFI measured at 960 °C and has excellent flame retardancy and mechanical properties.
  • the phosphorus-based flame retardant may include, for example, at least one selected from the group consisting of phosphate ester, phosphonate, phosphinate, phosphine oxide, and phosphazene.
  • the weight ratio of the phosphorus-based flame retardant and the polyamide resin may be, for example, 1:3 to 1:5 or 1:3.5 to 1:4.5, and within this range, tensile strength and impact strength Etc. There are more excellent advantages.
  • the flame-retardant polyamide resin composition of the present disclosure may further include a flame-retardant auxiliary agent if necessary, and the flame-retardant auxiliary agent may be, for example, magnesium hydroxide, aluminum hydroxide, or a mixture thereof, and in this case, flame retardancy is improved and the surface appearance is excellent. There is.
  • the magnesium hydroxide and/or aluminum hydroxide may be surface-treated with phosphorus, for example, and in this case, flame retardancy is improved and surface appearance is excellent.
  • the flame-retardant auxiliary agent may be included in an amount of less than 3% by weight, or 0.01 to 3% by weight, based on the flame-retardant polyamide resin composition as an example, and within this range, there is an advantage of having excellent flame retardancy and high surface appearance and mechanical properties.
  • the flame-retardant polyamide resin composition of the present disclosure may optionally be selected from the group consisting of lubricants, colorants, antistatic agents, plasticizers, thermal stabilizers, antioxidants, light stabilizers, anti-drip agents, pigments and inorganic fillers (excluding glass fibers). It may include at least one selected.
  • the flame-retardant polyamide resin composition of the present disclosure for example, has a tensile strength (thickness of 40 mm, ASTM D638) of 148 MPa or more or 148 to 170 MPa, preferably 150 to 165 MPa, and a tensile elongation (thickness of 40 mm, ASTM D638) of 3.0% or more or 3.0 to 4.0%, the flexural strength (thickness 40 mm, ASTM D790) is 7800 MPa or more or 7800 to 8200 MPa, preferably 8000 to 8200 MPa, and the Charpy impact strength (thickness 40 mm, ASTM D256) is 12 kJ/m 2 or more or 12 to It is 15kJ/m 2 and its flame retardancy (UL 94 V TEST) is V-1 or higher, V-1 or VO, and it has the effect of providing a molded article with excellent flame retardancy and mechanical properties within this range.
  • a tensile strength thickness of 40 mm
  • the present description provides a method of manufacturing the flame-retardant polyamide resin composition, and in describing this, a description overlapping with the above will be omitted. It is obvious that the contents described above in the flame-retardant polyamide resin composition are equally included in the method for preparing the flame-retardant polyamide resin composition described later.
  • the method for preparing the flame-retardant polyamide resin composition of the present disclosure includes, for example, 50 to 75% by weight of a polyamide resin, 5 to 30% by weight of glass fibers having a filament diameter of 10.6 to 11.9 ⁇ m, and 13 to 20% by weight of a phosphorus-based flame retardant.
  • the kneading and extruding step is 200 to 280 °C and 200 to 400 rpm, for example; Alternatively 220 to 260° C. and 200 to 300 rpm; Although it may be performed under conditions, it is not limited thereto, and may be performed by appropriately selecting within the range commonly practiced in the art.
  • the kneading and extrusion step may be performed using a Banbari mixer, a single screw extruder, a twin screw extruder, a kneader reactor, etc., for example, and is not particularly limited.
  • the extrusion step is one selected from the group consisting of flame retardant aids, lubricants, colorants, antistatic agents, plasticizers, heat stabilizers, antioxidants, light stabilizers, anti-drip agents, pigments and inorganic fillers (excluding glass fibers). It may include more than one.
  • the flame-retardant polyamide resin composition manufactured according to the above manufacturing method may be provided as a molded article through injection molding.
  • the molded article of the present disclosure is characterized in that it contains the flame-retardant polyamide resin composition.
  • the molded article may be, for example, a housing for an MCCB circuit breaker, a housing for an ACB circuit breaker, and a housing for an MCB circuit breaker.
  • Polyamide resin Nylon 6 (melting temperature 250 ⁇ 270°C, relative viscosity 2.2 ⁇ 2.4, number average molecular weight 30,000g/mol)
  • Glass fiber 1 As a bb strand glass fiber having a circular cross section, a filament diameter of 10 ⁇ m, and a bulging length of 3 mm, CPIC's ECS301HP-3 (filament diameter 10 ⁇ m) was used.
  • Glass fiber 2 As a bb strand glass fiber having a circular cross section, a filament diameter of 11 ⁇ m, and a bulging length of 3 mm, CPIC's ECS301HP-3-H (filament diameter 11 ⁇ m) was used.
  • Glass fiber 3 A bb strand glass fiber having a circular cross section, a filament diameter of 13 ⁇ m, and a puff length of 3 mm, and CPIC's ECS301HP (filament diameter 13 ⁇ m) was used.
  • a flame-retardant polyamide resin composition was prepared by melt-kneading and extruding in a temperature range of 220 to 290°C using a twin screw extruder. After extrusion, the pellets were pelletized using a pelletizer, dried at 120° C. for 4 hours or more, and then allowed to stand for 48 hours or more in a state where contact with air was blocked by injection molding, and then physical properties were measured.
  • Charpy impact strength was measured using a 40 mm thick specimen according to ASTM D256.
  • UL 94 manufactures a specimen of a predetermined thickness by injection molding, the specimen is placed vertically, and the specimen is lit with a burner, so that the fire on the specimen should be extinguished by itself within a certain period of time. It was divided into grades of -2, V-1, and V-0. The V-0 grade has the best flame retardancy.
  • the flame-retardant polyamide resin compositions of Examples 1 to 3 according to the present invention were excellent in flame retardancy of V-1 or higher, and excellent in tensile strength, tensile elongation, flexural strength, and impact strength.
  • the tensile strength and impact strength are significantly improved compared to Comparative Examples 1 and 4 using different types of glass fibers from the examples.

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

Abstract

La présente invention concerne une composition de résine polyamide ignifuge, son procédé de fabrication, et un produit moulé la comprenant. De façon spécifique, la présente invention concerne une composition de résine polyamide ignifuge, son procédé de fabrication, et un produit moulé la comprenant, la composition de résine comprenant : 50 à 75 % en poids d'une résine polyamide ; 5 à 30 % en poids d'une fibre de verre ayant un diamètre de filament de 10,6 à 11,9 µm ; et 13 à 20 % en poids d'un ignifuge à base de phosphore, la fibre de verre étant une fibre hachée E-Glass et ayant une longueur hachée de 2 à 6 mm. Selon la présente invention, la composition de résine est grandement améliorée en termes de résistance à la traction et de résistance au choc en utilisant une fibre de verre spécifique et est dotée d'un niveau élevé d'ignifugibilité en utilisant un ignifuge écologique.
PCT/KR2020/001621 2019-03-12 2020-02-04 Composition de résine polyamide ignifuge, son procédé de fabrication, et procédé de fabrication d'un produit moulé la comprenant Ceased WO2020184839A1 (fr)

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KR1020190027867A KR102578733B1 (ko) 2019-03-12 2019-03-12 난연 폴리아미드 수지 조성물, 이의 제조방법 및 이를 포함하는 성형품의 제조방법

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US11401416B2 (en) 2017-10-17 2022-08-02 Celanese Sales Germany Gmbh Flame retardant polyamide composition
CN116622224A (zh) * 2022-02-18 2023-08-22 旭化成株式会社 纤维增强聚酰胺树脂组合物和成型体

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MX376512B (es) 2014-06-20 2025-03-07 Performance Polyamides Sas Composiciones para moldeado de poliamida, partes moldeadas obtenidas de ellas y usos de las mismas.

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JP2008163317A (ja) * 2006-12-04 2008-07-17 Mitsubishi Engineering Plastics Corp 難燃性ポリアミド樹脂組成物および成形品
KR20100044193A (ko) * 2007-08-01 2010-04-29 가부시키가이샤 구라레 폴리아미드 조성물
KR20150111855A (ko) * 2014-03-26 2015-10-06 란세스 도이치란트 게엠베하 폴리아미드 조성물
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11401416B2 (en) 2017-10-17 2022-08-02 Celanese Sales Germany Gmbh Flame retardant polyamide composition
US11981812B2 (en) 2017-10-17 2024-05-14 Celanese Sales Germany Gmbh Flame retardant polyamide composition
CN116622224A (zh) * 2022-02-18 2023-08-22 旭化成株式会社 纤维增强聚酰胺树脂组合物和成型体

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