WO2023211148A1 - Matériau composite ignifuge et procédé de préparation associé - Google Patents

Matériau composite ignifuge et procédé de préparation associé Download PDF

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Publication number
WO2023211148A1
WO2023211148A1 PCT/KR2023/005679 KR2023005679W WO2023211148A1 WO 2023211148 A1 WO2023211148 A1 WO 2023211148A1 KR 2023005679 W KR2023005679 W KR 2023005679W WO 2023211148 A1 WO2023211148 A1 WO 2023211148A1
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Prior art keywords
composite material
flame
polymer composite
retardant polymer
flame retardant
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PCT/KR2023/005679
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English (en)
Korean (ko)
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김초원
서종환
이진우
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성균관대학교산학협력단
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Publication of WO2023211148A1 publication Critical patent/WO2023211148A1/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
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • 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
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C08K2003/3063—Magnesium sulfate

Definitions

  • the present application relates to flame retardant polymer composite materials and methods for manufacturing the same.
  • imparting flame retardancy through metal inorganic hydroxide filling requires excessive filler filling, which poses a problem of deteriorating processability and mechanical properties when manufacturing polymer composite materials.
  • Republic of Korea Patent No. 10-0996715 relates to a flame retardant composition containing magnesium hydroxide particles and a flame retardant fiber using the same.
  • the patent discloses a flame retardant composition in which magnesium hydroxide particles, a metal inorganic hydroxide, are uniformly dispersed and do not gel, but does not mention providing a composite material with improved flame retardancy and mechanical properties by including expanded graphite in the flame retardant composition. not doing it
  • the purpose of the present application is to solve the problems of the prior art described above, and to provide a flame-retardant polymer composite material with improved flame retardancy and mechanical properties.
  • the object is to provide a method for manufacturing the flame-retardant polymer composite material.
  • the object is to provide building materials containing the flame-retardant polymer composite material.
  • the first aspect of the present application is a thermoplastic polymer; Flame retardants including magnesium oxysulfate whisker and expandable graphite (EG); It provides a flame retardant polymer composite material containing.
  • the flame-retardant polymer composite material may be exposed to a heat source and a dense char layer may be formed on the surface of the flame-retardant polymer composite material by the magnesium oxysulfate whisker and the expandable graphite. , but is not limited to this.
  • the flame retardant polymer composite material may have a flame retardancy grade of V-1 or higher according to UL 94, but is not limited thereto.
  • the flame-retardant polymer composite material may have a tensile strength of 50 Mpa or more, but is not limited thereto.
  • the flame-retardant polymer composite material may have an elastic modulus of 7.5 Mpa or more, but is not limited thereto.
  • the magnesium oxysulfate whisker may have an aspect ratio (L/D) of 40 to 80, but is not limited thereto.
  • the expandable graphite may have a particle size of 250 to 350 ⁇ m, but is not limited thereto.
  • the magnesium oxysulfate whisker may be included in an amount of 20 to 50 parts by weight based on 100 parts by weight of the flame-retardant polymer composite material, but is not limited thereto.
  • the expandable graphite may be included in an amount of 1 to 20 parts by weight based on 100 parts by weight of the flame-retardant polymer composite material, but is not limited thereto.
  • the thermoplastic polymer is ABS resin (acrylonitrile butadiene-styrene), polystyrene (PS), polyoxymethylene (POM), polymethyl methacrylate (PMMA), cellulose acetate (CA), and polytetramer.
  • ABS resin acrylonitrile butadiene-styrene
  • PS polystyrene
  • POM polyoxymethylene
  • PMMA polymethyl methacrylate
  • CA cellulose acetate
  • polytetramer polytetramer
  • Fluoroethylene PTFE
  • PCTEF polychlorotrifluoroethylene
  • PVDF vinyl fluoride
  • PMP polyvinylidene fluoride
  • PA polyamide
  • PC polycarbonate
  • PE polyethylene
  • PET polyethylene terephthalate
  • PI polyimide
  • PPO polyphenylene oxide
  • PP polypropylene
  • PSul polysulfone
  • PVDC polyvinylidene chloride
  • PVC polyvinyl chloride
  • a second aspect of the present application provides a method for producing a flame-retardant polymer composite material, comprising adding and mixing magnesium oxysulfate whisker and expandable graphite (EG) to a thermoplastic polymer.
  • EG expandable graphite
  • the kneading step may be performed under conditions equal to or higher than the melting temperature of the thermoplastic polymer, but is not limited thereto.
  • thermoplastic polymer magnesium oxysulfate whisker, and expandable graphite may be dried at high temperature, but are not limited thereto.
  • the kneading may be performed through a polymer mixer, but is not limited thereto.
  • a third aspect of the present disclosure provides a building material comprising the flame retardant polymer composite material according to the first aspect of the present disclosure.
  • the flame retardant polymer according to the present invention can provide a polymer composite material with excellent flame retardancy and mechanical properties by using a mixture of magnesium oxysulfate whiskers and expanded graphite in an appropriate ratio to provide flame retardancy. This allows overall application to exterior and interior materials that require flame retardancy and mechanical properties in various industries.
  • Figure 1 is a schematic diagram of a method for manufacturing a flame-retardant polymer composite material according to an embodiment of the present application.
  • the term "combination thereof" included in the Markushi format expression means a mixture or combination of one or more components selected from the group consisting of the components described in the Markushi format expression, It means including one or more selected from the group consisting of.
  • the first aspect of the present application is a thermoplastic polymer; Flame retardants including magnesium oxysulfate whisker and expandable graphite (EG); It provides a flame retardant polymer composite material containing.
  • the flame retardant polymer according to the present invention Composite materials can provide polymer composite materials with excellent flame retardancy and mechanical properties by composite filling with magnesium oxysulfate whiskers and expanded graphite. This allows overall application to exterior and interior materials that require flame retardancy and mechanical properties in various industries. You can.
  • the flame-retardant polymer composite material may be exposed to a heat source and a dense char layer may be formed on the surface of the flame-retardant polymer composite material by the magnesium oxysulfate whisker and the expandable graphite. , but is not limited to this. More specifically, the flame-retardant polymer composite material may include the magnesium oxysulfate whisker and the expandable graphite dispersed in the thermoplastic polymer resin.
  • the magnesium oxysulfate whisker has a fiber shape, there may be limitations in forming a dense char layer when used alone. Therefore, by composite filling expanded graphite with the magnesium oxysulfate whisker, a dense char layer can be formed on the surface of the flame-retardant polymer composite material.
  • compounds such as sulfur and nitrogen compounds may be inserted between the layers of the expandable graphite, and when exposed to a heat source, the compounds present between the layers volatilize and escape in the form of gas, expanding the graphite, thereby providing the flame retardancy.
  • a dense char layer can be formed on the surface of the polymer composite material.
  • the magnesium oxysulfate whisker may have an aspect ratio (L/D) of 40 to 80, but is not limited thereto.
  • the flame-retardant polymer composite material according to the present application can have better mechanical properties when filled at the same content compared to magnesium hydroxide, an inorganic flame retardant with a similar composition and low aspect ratio.
  • the magnesium oxysulfate whisker may be included in an amount of 20 to 50 parts by weight based on 100 parts by weight of the flame-retardant polymer composite material, but is not limited thereto.
  • magnesium oxysulfate whiskers in a flame-retardant polymer composite material increases, flame retardancy may improve. However, if the content exceeds a certain amount, the dispersibility of magnesium oxysulfate whiskers may decrease, which may reduce the mechanical properties of the entire composite material. Therefore, it may be desirable for the magnesium oxysulfate whisker to be included in an amount of 20 to 50 parts by weight, but it is not limited thereto.
  • the expandable graphite may be included in an amount of 1 to 20 parts by weight based on 100 parts by weight of the flame-retardant polymer composite material, but is not limited thereto.
  • the flame-retardant polymer composite material according to the present application can provide a composite material with excellent flame retardancy and mechanical properties by adding a small amount of expanded graphite, a flame retardant auxiliary, to a magnesium oxysulfate whisker base.
  • expanded graphite is included in a certain amount or more, a problem may arise in that expanded graphite that does not form char may fly off as dust during combustion. Therefore, it may be preferable that the expandable graphite is included in an amount of 1 to 20 parts by weight based on 100 parts by weight of the flame-retardant polymer composite material.
  • the expandable graphite may have a particle size of 250 to 350 ⁇ m, but is not limited thereto.
  • the flame retardant polymer composite material may have a flame retardancy grade of V-1 or higher according to UL 94, but is not limited thereto.
  • UL Underwriter's Laboratories
  • UL 94 is an item that evaluates flame retardancy, and is currently the most commonly used flame retardant. It is an evaluation standard.
  • Flame retardancy grades are evaluated as having high flame retardancy in the order of HB, V-2, V-1, V-0, 5VB, and 5VA, and the flame retardant polymer composite material according to the present invention may have a flame retardancy grade of V-1 or higher, but is limited to this. It doesn't work.
  • the flame-retardant polymer composite material may have a tensile strength of 50 Mpa or more, but is not limited thereto.
  • the flame-retardant polymer composite material may have an elastic modulus of 7.5 Mpa or more, but is not limited thereto.
  • the thermoplastic polymer is ABS resin (acrylonitrile butadiene-styrene), polystyrene (PS), polyoxymethylene (POM), polymethyl methacrylate (PMMA), cellulose acetate (CA), and polytetramer.
  • ABS resin acrylonitrile butadiene-styrene
  • PS polystyrene
  • POM polyoxymethylene
  • PMMA polymethyl methacrylate
  • CA cellulose acetate
  • polytetramer polytetramer
  • Fluoroethylene PTFE
  • PCTEF polychlorotrifluoroethylene
  • PVDF vinyl fluoride
  • PMP polyvinylidene fluoride
  • PA polyamide
  • PC polycarbonate
  • PE polyethylene
  • PET polyethylene terephthalate
  • PI polyimide
  • PPO polyphenylene oxide
  • PP polypropylene
  • PSul polysulfone
  • PVDC polyvinylidene chloride
  • PVC polyvinyl chloride
  • a second aspect of the present application provides a method for producing a flame-retardant polymer composite material, comprising adding and mixing magnesium oxysulfate whisker and expandable graphite (EG) to a thermoplastic polymer.
  • EG expandable graphite
  • Figure 1 is a schematic diagram of a method for manufacturing a flame-retardant polymer composite material according to an embodiment of the present application.
  • thermoplastic polymer magnesium oxysulfate whisker, and expandable graphite may be dried at high temperature, but are not limited thereto.
  • the method for manufacturing a flame-retardant polymer composite material manufactures a composite material by a melt-kneading process performed above the melting point of the thermoplastic polymer. At this time, the moisture of the thermoplastic polymer, magnesium oxysulfate whisker whisker, and expanded graphite is not removed. In this case, thermal decomposition of the polymer chain may occur during the process, resulting in an undesirable decrease in mechanical properties. Therefore, prior to performing kneading, each material may undergo a drying process at high temperature. For example, the magnesium oxysulfate whiskers and expanded graphite can be dried in a vacuum oven at 70°C for 8 hours.
  • thermoplastic polymer resin can be dried in a vacuum oven at 100°C for 8 hours. Accordingly, moisture is evaporated from the magnesium oxysulfate whisker, the expanded graphite, and the thermoplastic polymer resin, but the flame retardant polymer composite material produced may have excellent flame retardant properties. Meanwhile, unlike the embodiments of the present application, when the magnesium oxysulfate whisker is dried at a temperature of 100°C or higher, the crystal water present in the crystal structure may be excessively evaporated. Accordingly, the flame retardant properties of the manufactured flame retardant may deteriorate.
  • the magnesium oxysulfate whisker can be dried at 70 ° C or higher and 100 ° C or lower, and accordingly, the flame retardant polymer produced while easily evaporating moisture from the magnesium oxy sulfate whisker
  • the flame retardant properties of composite materials can be excellent.
  • the kneading step may be performed under conditions equal to or higher than the melting temperature of the thermoplastic polymer, but is not limited thereto.
  • thermoplastic polymer, magnesium oxysulfate whisker, and expanded graphite dried at high temperature are kneaded under conditions equal to or higher than the melting temperature of the thermoplastic polymer to finally produce the flame-retardant polymer composite material according to the present disclosure.
  • the kneading may be performed through a polymer mixer, but is not limited thereto.
  • a reinforcing agent such as carbon fiber or ceramic particles may be added in the kneading step.
  • a plasticizer may be added in the kneading step.
  • the ductility of the flame-retardant polymer composite material produced may be excellent.
  • excellent ductility may mean that the elongation at break of the flame-retardant polymer composite material is improved. This may be because the plasticizer has friendly properties with the organic thermoplastic polymer.
  • the plasticizer in the kneading step, may be added in an amount of more than 3.2 wt% to less than 6.4 wt%, for example, about 5 wt%. Accordingly, the manufactured flame-retardant polymer composite material may have excellent ductility.
  • the plasticizer when added at 3.2 wt% or less, elongation at break may not be substantially improved.
  • the elastic modulus and strength of the flame-retardant polymer composite material produced may be reduced because the plasticizer is excessively included.
  • the plasticizer may be added in an amount of more than 3.2 wt% to less than 6.4 wt%, and thus the ductility of the flame-retardant polymer composite material manufactured may be excellent.
  • the plasticizer may have an alkyl chain.
  • the plasticizer includes diisononyl phthalate (DINP), diisodecyl phthalate (DIDP), dioctyl adipate (DOA), and dioctyl phthalate (DOP). , diethylhexyl adipate (DEHA), diethylhexyl phthalate (DEHP), and butyl benzyl phthalate (BBP).
  • a third aspect of the present disclosure provides a building material comprising the flame retardant polymer composite material according to the first aspect of the present disclosure.
  • a fourth aspect of the present application provides a vehicle material comprising the flame-retardant polymer composite material according to the first aspect of the present application.
  • vehicle materials may include, for example, automobile interior materials, automobile exterior materials, etc.
  • Example 1 when the flame-retardant polymer composite material is applied to a vehicle material, Example 1, described later, may be used as the automobile interior material, and Example 2, described later, may be used as the automobile exterior material.
  • Example 2 herein may contain more of the expanded graphite than Example 1.
  • the automobile interior material may include a automobile dashboard cover.
  • the automobile exterior material may include automobile parts, such as an electric vehicle battery pack cover, bumper, trunk cover, etc.
  • the automobile exterior material can be applied to include more expanded graphite than the automobile interior material. Therefore, when the flame-retardant polymer composite material is applied to the vehicle material, the automobile exterior material containing a relatively larger amount of the expanded graphite can easily protect the occupants inside the vehicle from external shock, and the expanded graphite The automobile interior material containing relatively less material can easily support the occupants.
  • the flame-retardant polymer composite material according to the present application is not limited to the above-described embodiments and can be widely applied to the aerospace, marine, construction, electrical and electronic industries, etc. Furthermore, the flame-retardant polymer composite material is not limited to the above-mentioned scope and can be applied to replace all plastic parts or metal parts that require flame retardancy.
  • Magnesium oxysulfate whisker and expanded graphite to remove moisture from pellet-type thermoplastic polymer resin (Acrylonitrile Butadiene Styrene, ABS), magnesium oxysulfate whisker (diameter 0.46 ⁇ m, length 25.5mm) and expanded graphite (particle size) 297um) were dried in a vacuum oven at 70°C for 8 hours, and the thermoplastic polymer resins were dried in a vacuum oven at 100°C for 8 hours. Accordingly, moisture is evaporated from the magnesium oxysulfate whisker and the expandable graphite, and the flame retardant polymer composite material manufactured including the magnesium oxysulfate whisker and the expandable graphite may have excellent flame retardant properties.
  • pellet-type thermoplastic polymer resin Adiameter 0.46 ⁇ m, length 25.5mm
  • expanded graphite particle size 297um
  • the crystal water present in the crystal structure may be excessively evaporated. Accordingly, the flame retardant properties of the manufactured flame retardant may deteriorate.
  • the magnesium oxysulfate whisker can be dried at 70 ° C or higher and 100 ° C or lower, and accordingly, the flame retardant polymer produced while easily evaporating moisture from the magnesium oxy sulfate whisker
  • the flame retardant properties of composite materials can be excellent.
  • thermoplastic polymer resin magnesium oxysulfate whisker, and expanded graphite were added in a weight ratio of 60:39:1, dispersed uniformly, and mixed with a polymer mixer above the melting temperature of the thermoplastic polymer resin to form the magnesium oxysulfate whisker.
  • a flame-retardant polymer composite material filled with expandable graphite.
  • the manufactured flame-retardant polymer composite material may include the magnesium oxysulfate whisker and the expandable graphite dispersed in the thermoplastic polymer resin.
  • thermoplastic polymer resin magnesium oxysulfate whiskers, and expanded graphite were added in a weight ratio of 60:37:3.
  • thermoplastic polymer resin magnesium oxysulfate whisker, and expanded graphite were added in a weight ratio of 60:35:5.
  • thermoplastic polymer resin without the addition of magnesium oxysulfate whiskers and expanded graphite was used in Comparative Example 1.
  • thermoplastic polymer resin and magnesium oxysulfate whiskers were added in a ratio of 90:10 by weight, and expandable graphite was not added.
  • thermoplastic polymer resin and magnesium oxysulfate whiskers were added in a weight ratio of 80:20, and expandable graphite was not added.
  • thermoplastic polymer resin and magnesium oxysulfate whiskers were added in a weight ratio of 70:30, and expandable graphite was not added.
  • thermoplastic polymer resin and magnesium oxysulfate whiskers were added in a weight ratio of 60:40, and expandable graphite was not added.
  • Table 1 shows the addition ratios of thermoplastic polymer resin, magnesium oxysulfate whisker, and expanded graphite in composite materials according to examples and comparative examples of the present application.
  • the composite materials of Examples 1 to 3 and Comparative Examples 1 to 5 were pelletized with a pelletizer and then stretched at 180°C and under a 9 ton load using an injection molding machine and a hot press. Test specimens and flame retardancy test specimens were produced, and mechanical property evaluation and flame retardancy evaluation were performed.
  • flame retardant test specimens of approximately 13 mm in width, 125 mm in height, and 3 mm in thickness were produced for each example and comparative example. Flame retardancy evaluation was performed by contacting the flame retardant test specimen twice for 10 seconds using a butane gas torch. The time it took for the flame to be extinguished (t1, t2) was measured. As a result of the flame retardancy evaluation, Example 3 filled with magnesium oxysulfate whisker and expanded graphite was evaluated as having the highest flame retardancy rating of V-0.
  • Example 2 filled with magnesium oxysulfate whisker and expanded graphite, it was confirmed that the tensile strength and elastic modulus were improved by 35% and 277%, respectively, compared to Comparative Example 1 (pure thermoplastic resin).
  • Table 2 below shows the results of evaluation of flame retardancy and mechanical properties according to an experimental example herein.

Abstract

La présente demande concerne un matériau composite polymère ignifuge comprenant : un polymère thermoplastique ; et un retardateur de flamme contenant des trichites d'oxysulfate de magnésium et du graphite expansible (EG).
PCT/KR2023/005679 2022-04-28 2023-04-26 Matériau composite ignifuge et procédé de préparation associé WO2023211148A1 (fr)

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Citations (3)

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CN103045047A (zh) * 2012-12-21 2013-04-17 厦门大学 一种基于可膨胀石墨和晶须体系的水性超薄膨胀型钢结构防火涂料
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JP2001158814A (ja) * 1999-09-22 2001-06-12 Shikoku Chem Corp 難燃性樹脂組成物
CN103045047A (zh) * 2012-12-21 2013-04-17 厦门大学 一种基于可膨胀石墨和晶须体系的水性超薄膨胀型钢结构防火涂料
CN109593226A (zh) * 2018-11-16 2019-04-09 山东省海洋化工科学研究院 一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及其制备泡沫材料的方法

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DANG LI, TANG DELIN, DU XINLIU, ZHAO YUNTIAN, LV ZHIHUI, ZHU DONGHAI, CUI XIANGMEI: "Synergistic effects of magnesium oxysulte whisker and multiwalled carbon nanotube on flame retardancy, smoke suppression, and thermal properties of polypropylene", JOURNAL OF APPLIED POLYMER SCIENCE, JOHN WILEY & SONS, INC., US, vol. 137, no. 40, 20 October 2020 (2020-10-20), US , XP093105159, ISSN: 0021-8995, DOI: 10.1002/app.49210 *
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