WO2022110665A1 - Matériau composite de polyamide antistatique ignifuge, son procédé de préparation et son utilisation - Google Patents

Matériau composite de polyamide antistatique ignifuge, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2022110665A1
WO2022110665A1 PCT/CN2021/092777 CN2021092777W WO2022110665A1 WO 2022110665 A1 WO2022110665 A1 WO 2022110665A1 CN 2021092777 W CN2021092777 W CN 2021092777W WO 2022110665 A1 WO2022110665 A1 WO 2022110665A1
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WIPO (PCT)
Prior art keywords
flame
composite material
antistatic
retardant
polyamide composite
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PCT/CN2021/092777
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English (en)
Chinese (zh)
Inventor
王丰
黄险波
叶南飚
丁超
金雪峰
胡泽宇
张亚军
张永
易新
吴长波
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金发科技股份有限公司
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Publication of WO2022110665A1 publication Critical patent/WO2022110665A1/fr

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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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • 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
    • C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/41—Compounds containing sulfur bound to oxygen
    • C08K5/42—Sulfonic acids; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K2003/026—Phosphorus
    • 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
    • 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
    • C08L2201/04—Antistatic

Definitions

  • the present invention relates to the technical field of engineering plastics, and more particularly, to a flame-retardant and antistatic polyamide composite material and a preparation method and application thereof.
  • Polyamide has excellent mechanical properties, heat resistance, wear resistance, oil resistance, etc., and is widely used in the machinery industry, automobiles, power tools, electronic appliances, transportation and other fields. Polyamide is often used as a flame retardant material. Although it has strong polarity and strong water absorption, it still has a high surface resistance (above 10 10 ⁇ ) and is used in the occasions where gas gas is generated. The surface resistance should reach (10 8 ⁇ ) The following) can meet the requirements of use, otherwise it is easy to cause fire and explosion. Therefore, in the application of coal mining equipment, it is necessary to develop materials with both flame retardant and antistatic functions.
  • Chinese patent CN 1752142A discloses a preparation method of nylon 6/polyelectrolyte antistatic composite material. effect polyamide composite.
  • the processing temperature of PA66 is 230 ⁇ 280°C.
  • the antistatic additive will degrade, resulting in a significant deterioration of the composite material properties and a decrease in mechanical properties of more than 30%. It is impossible to obtain both good antistatic properties and Mechanical properties of flame retardant polyamide material.
  • the technical problem to be solved by the present invention is to overcome the defects and deficiencies that the existing flame retardant polyamide materials cannot have good antistatic properties and mechanical properties at the same time, and provide a flame retardant and antistatic polyamide composite material, which has good antistatic properties at the same time. performance and mechanical properties.
  • Another object of the present invention is to provide a method for preparing a flame retardant and antistatic polyamide composite material.
  • Another object of the present invention is to provide the application of a flame retardant and antistatic polyamide composite material.
  • a flame retardant and antistatic polyamide composite material comprising the following components calculated in parts by mass:
  • the composite antistatic agent is a compound of potassium diphenylsulfone sulfonate and carbon nanotubes, wherein the mass ratio of potassium diphenylsulfonesulfonate to carbon nanotubes is 1:1.5-2.5; the diameter of carbon nanotubes It is 8 to 15 nm, and the length is 10 to 70 ⁇ m.
  • the invention uses PA66 as the matrix material, which has excellent flame retardant performance, and adds a specific proportion of potassium diphenylsulfone sulfonate and carbon nanotubes of a certain size for compounding as a composite antistatic agent.
  • One is diphenylsulfone Potassium sulfonate itself has an antistatic effect.
  • potassium diphenylsulfone sulfonate can promote the dispersion of carbon nanotubes in PA66, improve the compatibility of carbon nanotubes in the system, and is conducive to the construction of a charge transfer network.
  • the obtained flame-retardant polyamide composite material can obtain good antistatic properties, and can still have good mechanical properties at the processing temperature of PA66 (230-280° C.).
  • the mass ratio of the potassium diphenylsulfone sulfonate to the carbon nanotubes is 1:2-2.5.
  • the mass ratio of potassium diphenylsulfone sulfonate to carbon nanotubes is 1:2.
  • the carbon nanotubes have a diameter of 10-12 nm and a length of 30-60 ⁇ m.
  • the number average molecular weight of the PA66 is 12000-30000.
  • the relative viscosity of the PA66 is 1.8-3.5.
  • the relative viscosity of the PA66 is 2.2-2.8.
  • test method for the relative viscosity of PA66 test standard ISO 307-2007, 96% sulfuric acid solution, sample concentration 0.005g/mL, test temperature 25°C.
  • the reinforcing material of the present invention includes, but is not limited to, one or more of glass fibers, carbon fibers, aramid fibers, and ceramic fibers.
  • the flame retardant is red phosphorus masterbatch.
  • the flame retardant is microcapsule red phosphorus masterbatch.
  • the mass content of red phosphorus in the microcapsule red phosphorus master batch is 40% to 60%.
  • the processing aids of the present invention include, but are not limited to, one or more of antioxidants, lubricants, light stabilizers, and colorants.
  • the antioxidants described in the present invention include but are not limited to N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexanediamine (1098), triethylenediamine Alcohol ether-bis(3-tert-butyl-4-hydroxy-5-methylphenyl) propionate (antioxidant 245), tetrakis[beta-(3,5-di-tert-butyl-4-hydroxybenzene base) propionic acid] pentaerythritol ester (antioxidant 1010), tris[2.4-di-tert-butylphenyl] phosphite (antioxidant 168), phosphite antioxidant P-EPQ, copper salt antioxidant One or more of the agent (a compound of potassium iodide, cuprous iodide, and zinc stearate, with a mass ratio of 8:1:1).
  • the agent a compound of potassium iodide
  • the lubricant of the present invention includes, but is not limited to, one or more of calcium stearate, modified ethylene bis-fatty acid amide, aliphatic fatty acid ester, and ethylene-acrylic acid copolymer.
  • the light stabilizer of the present invention includes, but is not limited to, benzotriazole light stabilizer.
  • the colorants of the present invention include, but are not limited to, black masterbatch.
  • the present invention protects the preparation method of the above-mentioned flame retardant and antistatic polyamide composite material, comprising the following steps:
  • a twin-screw extruder with side feeding is used for the melt blending, and the feeding port includes a main feeding port and a side feeding port; the uniformly mixed material is fed from the main feeding port, and the reinforcing material is fed from the main feeding port.
  • Side feeding port feeding is used for the melt blending, and the feeding port includes a main feeding port and a side feeding port; the uniformly mixed material is fed from the main feeding port, and the reinforcing material is fed from the main feeding port.
  • Side feeding port feeding is used for the melt blending, and the feeding port includes a main feeding port and a side feeding port; the uniformly mixed material is fed from the main feeding port, and the reinforcing material is fed from the main feeding port.
  • the temperature of the melt blending is 230-280°C.
  • the invention also protects the application of the above flame-retardant and antistatic polyamide composite material in coal mine equipment.
  • the flame retardant and antistatic polyamide composite material of the invention has excellent flame retardant performance, reaches V-0 level, the surface resistivity is 10 8 and below, the tensile strength reaches 133MPa and above, and the impact strength reaches 8.5kJ/m 2 and above, with good antistatic properties and mechanical properties.
  • the invention takes PA66 as the matrix material, adds a certain proportion of reinforcing materials, flame retardants, processing aids, and a certain proportion of potassium diphenylsulfone sulfonate and carbon nanotubes of a certain size to be compounded as a composite antistatic agent.
  • the flame retardant and antistatic polyamide composite material can not only obtain good antistatic properties, but also obtain good mechanical properties at the processing temperature of PA66, and has good flame retardant properties. It can be used in applications requiring antistatic properties, such as coal mines. equipment, etc.
  • the raw material reagents used in the examples of the present invention are conventionally purchased raw material reagents.
  • PA66 the grade is EPR24, the number average molecular weight is 13700, the relative viscosity is 2.4, purchased from Pingdingshan Shenma Group;
  • Reinforcing material glass fiber, grade ECS10-03-568H, purchased from Jushi Group;
  • Microcapsule red phosphorus masterbatch the brand is FR9950KF, the mass content of red phosphorus is 50%, purchased from Tongcheng Xinde New Materials Co., Ltd.;
  • antistatic agent the name is polyether antistatic agent, the brand name is PELESTAT-6500, purchased from Sanyo Chemicals in Japan;
  • Conductive carbon black purchased from Yiborui (Tianjin) Chemical Co., Ltd.;
  • KSS Potassium Diphenylsulfone Sulfonate
  • Carbon nanotube A the grade is LUCAN CP1002M, purchased from LG Chem; the diameter of the carbon nanotube is 8-12 nm, and the length is 50-70 ⁇ m.
  • Carbon nanotube B the grade is GC-21, purchased from Shandong Dazhan Nanomaterials Co., Ltd.; the diameter of the carbon nanotube is 12-15 nm, and the length is 10-50 ⁇ m;
  • Black mother the grade is N54/1044, purchased from Colly Plastics, UK;
  • Antioxidant 1098 N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexamethylenediamine, commercially available;
  • Lubricant ethylene-acrylic acid copolymer (EAA), trade name A-C540A, available from Honeywell.
  • Table 2 shows the components and mass parts of the flame-retardant and antistatic polyamide composite materials of each embodiment and comparative example.
  • a preparation method of a flame retardant and antistatic polyamide composite material comprising the following steps:
  • Composite antistatic agent 3 1 2.5 Composite antistatic agent 4 1 1 Composite antistatic agent 5 1 3 Composite antistatic agent 6 1 2
  • the flame retardant and antistatic polyamide composite material prepared by the present invention has high antistatic effect, the surface resistivity is 10 8 and below, and also has good notched impact strength, tensile strength and flame retardancy. performance, can be used in applications requiring antistatic, such as coal mining equipment.
  • Comparative Example 1 no composite antistatic agent was added, and its surface resistivity increased significantly.
  • Comparative Example 2 and Comparative Example 3 conductive carbon black and commercially available antistatic agent PELESTAT-6500 were used as substitutes for the composite antistatic agent. The ratio is still greater than 10 8 , and the mechanical properties such as notched impact strength and tensile strength are significantly reduced.
  • the existing conventional antistatic agent cannot reduce the surface resistivity of the material well, and will cause adverse effects on the mechanical properties of the material.
  • the composite antistatic agent used in Comparative Example 4 reduces the amount of carbon nanotubes, and the composite antioxidant in Comparative Example 5 increases the amount of carbon nanotubes, and the surface resistivity of the obtained material is still large, still 10 8 Above, the antistatic performance is not good enough, and the mechanical properties also have a certain degree of decline.

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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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Un matériau composite de polyamide antistatique ignifuge, son procédé de préparation et son utilisation sont divulgués. Le PA66 est utilisé en tant que matériau de base, et une certaine proportion d'un matériau de renforcement, un ignifuge, un additif, une proportion spéciale de sulfonate de diphénylméthylsulfone de potassium et une certaine taille d'un nanotube de carbone sont ajoutés pour être mélangés en tant qu'agent antistatique composite, qui est utilisé pour préparer le matériau composite de polyamide antistatique ignifuge, de telle sorte que le matériau composite de polyamide antistatique ignifuge présente de bonnes performances antistatiques et d'excellentes propriétés mécaniques et propriétés ignifuges, et peut être appliqué dans des situations nécessitant des performances antistatiques, telles que dans un équipement de charbonnage.
PCT/CN2021/092777 2020-11-27 2021-05-10 Matériau composite de polyamide antistatique ignifuge, son procédé de préparation et son utilisation WO2022110665A1 (fr)

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CN202011360931.4A CN112552679B (zh) 2020-11-27 2020-11-27 一种阻燃抗静电聚酰胺复合材料及其制备方法和应用
CN202011360931.4 2020-11-27

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Cited By (3)

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CN114957987A (zh) * 2022-07-04 2022-08-30 华润化学材料科技股份有限公司 一种阻燃性抗静电母粒及其制备方法与应用
CN115926453A (zh) * 2023-01-13 2023-04-07 深圳科立尔科技有限公司 一种具有抗静电作用的尼龙母粒及其制备方法
CN115948049A (zh) * 2023-03-15 2023-04-11 广东永鑫华新型材料有限公司 一种永久抗静电挤出级尼龙材料的制备方法

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CN112552679B (zh) * 2020-11-27 2022-01-11 金发科技股份有限公司 一种阻燃抗静电聚酰胺复合材料及其制备方法和应用
CN114621573B (zh) * 2022-03-15 2023-06-23 金发科技股份有限公司 一种无卤阻燃碳纤维增强聚碳酸酯组合物及其制备方法和应用

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114957987A (zh) * 2022-07-04 2022-08-30 华润化学材料科技股份有限公司 一种阻燃性抗静电母粒及其制备方法与应用
CN115926453A (zh) * 2023-01-13 2023-04-07 深圳科立尔科技有限公司 一种具有抗静电作用的尼龙母粒及其制备方法
CN115926453B (zh) * 2023-01-13 2024-05-17 深圳科立尔科技有限公司 一种具有抗静电作用的尼龙母粒及其制备方法
CN115948049A (zh) * 2023-03-15 2023-04-11 广东永鑫华新型材料有限公司 一种永久抗静电挤出级尼龙材料的制备方法

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