High glowing filament flame-retardant reinforced high-performance PET modified material and preparation method thereof

By using bromine flame retardant, flame retardant synergist and glow wire coefferent compound in PET materials, combined with glass fiber and polyester nucleating agent, the shortcomings of existing PET materials in high glow wire temperature and environmental protection requirements are solved, and high-performance and environmentally friendly flame retardant enhancement effect is achieved.

CN119798939APending Publication Date: 2025-04-11GUANGDONG SHUNDE SHUNYAN NEW MATERIALS
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Patent Information

Application Number
CN202510285870.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-12
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The existing PET materials have shortcomings in high glow wire temperature and environmental protection requirements, especially the traditional red phosphorus flame retardant is prone to ignition at high temperatures and does not meet environmental protection standards.

Method used

A bromine-based flame retardant, flame retardant synergist and treated glow wire coefferent compound is used to combine glass fiber and polyester nucleating agent, and high-performance PET modified materials are prepared through the twin-screw extrusion mechanism.

Benefits of technology

The UL94 V0 flame retardant grade of the material is realized, the ignition temperature and stability of the glow wire are improved, the latest environmental protection requirements are met, and the mechanical properties, fire resistance and processing properties of the products are improved.

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Abstract

The invention relates to the technical field of PET (polyethylene terephthalate) materials, and discloses a high glowing filament flame-retardant reinforced high-performance PET modified material and a preparation method thereof, the raw materials comprise the following components by weight: 44.5%-52.5% of PET resin, 11%-15% of a brominated flame retardant, 2%-5% of a flame retardant synergist, 1%-5% of a glowing filament synergist compound, 1%-4% of a flexibilizer, 0.2%-1% of an antioxidant, 0.2%-1% of a lubricant, 0.1%-0.5% of a nucleating agent and 15%-40% of glass fiber. According to the high-glowing filament flame-retardant reinforced high-performance PET modified material and the preparation method thereof, the high-glowing filament flame-retardant reinforced high-performance PET modified material is high in mechanical property, good in fireproof performance, capable of meeting the requirement that a glowing filament at the temperature of 750 DEG C is not ignited in the whole process, excellent in processability, good in size stability and good in product surface glossiness, meets the requirements of the PET modified material on the market, meets the latest environment-friendly management and control requirements on the market, and has wide application prospects. The market application prospect is wide.
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Description

Technical Field

[0001] The invention relates to the technical field of PET materials, in particular to a high glow-wire flame-retardant enhanced high-performance PET modified material and a preparation method thereof. Background Art

[0002] Polyethylene terephthalate (PET) is an engineering plastic with excellent comprehensive properties. It has excellent mechanical properties, high rigidity, high hardness, good toughness, impact resistance, friction resistance, creep resistance, and good chemical resistance.

[0003] With the rapid development of electronic and electrical, new energy and other industries, higher requirements are placed on the flame retardancy and heat resistance of PET materials. High glow wire flame retardant reinforced PET modified materials came into being to meet these needs.

[0004] Patent CN102604340A discloses a high glow-wire flame retardant reinforced PET / PTT alloy and production process. The product is composed of PET, PTT, composite flame retardant, toughening agent, flame retardant synergist, inorganic filler, stabilizer, lubricant, antioxidant, nucleating agent, and glass fiber. The technical solution mainly uses bromine antimony plus MPP, triphenyl phosphate and other synergists to achieve flame retardancy and increase the glow-wire temperature.

[0005] Patent CN104672817A discloses a flame-retardant reinforced PET material with a high glow-wire temperature, including the following components: PET, flame retardant, glass fiber, toughening agent and additives (antioxidant, lubricant, nucleating agent). In this technical solution, a large amount of bromine antimony compound or red phosphorus flame retardant is added to achieve the effect of flame retardancy and increasing the glow-wire temperature. However, this technical solution uses decabromodiphenylethane, which cannot meet the market's environmental protection needs; in addition, red phosphorus is used for flame retardancy, which is easy to ignite under high temperature conditions, and there are great safety hazards in the production process. In addition, red phosphorus is dark red in color and cannot be used in light-colored system materials, so its application range is narrow.

[0006] Patent CN118834510A discloses a PET resin composition with a high glow-wire flammability index and a preparation method thereof. The PET resin composition with a high glow-wire flammability index is prepared by the following raw materials by mass percentage: 40.0-60.0% polyethylene terephthalate, 20.0-40.0% glass fiber, 3.0% toughening agent, 8.0-10.0% bromine flame retardant, 2.0-5.0% phosphorus flame retardant, 3.0-4.0% synergistic flame retardant, 0.5% antioxidant, and 0-0.5% pigment. A flame retardant effect is achieved and the glow-wire temperature is increased. The phosphorus flame retardant added in this technical solution is at least one of aluminum hypophosphite, ammonium polyphosphate or triphenyl phosphate. The addition of aluminum hypophosphite and ammonium polyphosphate increases with the addition amount, which will cause the degradation of the PET material, resulting in a significant decrease in the mechanical properties of the PET material.

[0007] Therefore, the development of high glow-wire flame-retardant reinforced high-performance PET modified materials that meet the requirements of high glow-wire, high performance, and excellent fire resistance, meet the latest environmental protection control requirements, and have broad application prospects. Summary of the invention

[0008] In view of the deficiencies in the prior art, the present invention provides a high glow-wire flame retardant enhanced high-performance PET modified material and a preparation method thereof, which solves the problems in the above-mentioned background technology.

[0009] To achieve the above objectives, the present invention is implemented through the following technical scheme: a high glow-wire flame retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: PET resin 44.5%-52.5%, brominated flame retardant 11%-15%, flame retardant synergist 2%-5%, glow-wire synergist compound 1%-5%, toughening agent 1%-4%, antioxidant 0.2%-1%, lubricant 0.2%-1%, nucleating agent 0.1%-0.5% and glass fiber 15%-40%.

[0010] Preferably, the brominated flame retardant is one or more of brominated epoxy, brominated polystyrene, and brominated triazine; The flame retardant synergist is one or more of antimony trioxide and sodium antimonate; The toughening agent is one or more of POE-g-GMA, POE grafted maleic anhydride, ethylene-methyl acrylate-glycidyl methacrylate and ethylene-butyl acrylate-glycidyl methacrylate; The antioxidant is one or more of antioxidant 1010, antioxidant 168, and antioxidant 1098; The lubricant is one or more of PETS, 540A, and silicone powder; The nucleating agent is polyester nucleating agent Sanulater HK250; The diameter of the glass fiber is 8-16 microns.

[0011] Preferably, the intrinsic viscosity of the PET resin is 0.660-0.700 dl / g, the melt flow rate is 90-110 g / 10 min under the test conditions of 265° C. / 2.16 kg, and the model of the PET resin is KH2678C.

[0012] Preferably, the glow-wire synergist compound is a compound of boehmite, 1,3-phenylene phosphate tetrakis(2,6-dimethylphenyl) ester and barium dihydrogen phosphate, the mass ratio of the three being 1-2:3-4:2, wherein the boehmite is nano-boehmite with an average particle size of 10-20 nm.

[0013] A method for preparing a high glow-wire flame-retardant enhanced high-performance PET modified material, which is specifically prepared by the following steps: A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder, and the mixture was treated to obtain a glow-wire synergist compound; A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0014] Preferably, the melt extrusion temperature in A3 is 220-280° C., and the screw speed is 300-600 r / min.

[0015] The present invention provides a high glow-wire flame retardant enhanced high-performance PET modified material and a preparation method thereof. It has the following beneficial effects: 1. By adding brominated flame retardants, flame retardant synergists, and treated glow-wire synergist compounds, the material can meet the UL94 V0 flame retardancy rating, and improve the glow-wire ignition temperature and glow-wire stability of the material to meet the latest environmental protection requirements.

[0016] 2. By adding polyester nucleating agent, the thermal crystallization temperature is effectively increased during the melt cooling crystallization process, the crystallization speed is accelerated, and the sticking film problem is solved; the dimensional stability of the product is improved, the post-shrinkage of the product is reduced; and the surface gloss of the product is improved.

[0017] 3. The high glow-wire flame-retardant reinforced high-performance PET modified material prepared by the present invention has high mechanical properties, good fire resistance, can meet the 750°C glow-wire non-ignition throughout the whole process, excellent processing performance (non-stick mold), good dimensional stability, and good surface gloss of the product. It meets the market demand for PET modified materials and the latest environmental protection control requirements in the market, and has broad market application prospects.

[0018] 4. The production process is simple, the operability is strong, and it is easy to promote and apply on a large scale to produce a high-glow-wire flame-retardant enhanced high-performance PET modified material.

[0019] 5. Boehmite, 1,3-phenylene tetrakis (2,6-dimethylphenyl) phosphate and barium dihydrogen phosphate are mixed to prepare a glow-wire synergist compound, which mainly improves the temperature and stability of the glow-wire through the following principles: Function of boehmite: Boehmite (AlO(OH)) decomposes at high temperature to form aluminum oxide ( ) and water, the endothermic reaction helps to reduce the surface temperature of the material, while the generated aluminum oxide forms a protective layer to improve thermal stability.

[0020] The role of 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate: As an organophosphorus flame retardant, this compound decomposes at high temperatures to generate phosphoric acid and phosphorus-containing free radicals, promotes carbonization of the material surface, forms a carbon layer, isolates heat and oxygen, and improves flame retardancy and thermal stability.

[0021] The role of barium dihydrogen phosphate: barium dihydrogen phosphate ( ) decomposes at high temperature to produce barium phosphate and phosphoric acid. Phosphoric acid further promotes carbonization, while barium phosphate acts as an inert filler to enhance the thermal stability and mechanical strength of the material.

[0022] Effect: Increase the glow-wire temperature: The compound delays the temperature rise of the material and increases the glow-wire temperature through endothermic reaction and carbonization.

[0023] Enhanced thermal stability: The generated alumina and carbon layer protect the material, reduce thermal degradation at high temperatures, and extend service life. After pretreatment, the compound has a smaller particle size, and the three materials have better dispersion, which interact with each other. The synergistic effect of heat absorption, carbonization and inert fillers significantly improves the temperature and thermal stability of the glow wire. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] Embodiment 1, A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 44.5% PET resin, 11% bromine flame retardant, 2% flame retardant synergist, 1% glow-wire synergist compound, 1% toughening agent, 0.2% antioxidant, 0.2% lubricant, 0.1% nucleating agent, and 40% glass fiber.

[0026] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 1:3:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0027] Embodiment 2, A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 53.5% PET resin, 15% bromine flame retardant, 5% flame retardant synergist, 5% glow-wire synergist compound, 4% toughening agent, 1% antioxidant, 1% lubricant, 0.5% nucleating agent, and 15% glass fiber.

[0028] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 2:4:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0029] Embodiment 3, A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 47.7% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 3% glow-wire synergist compound, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0030] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 1:4:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0031] Embodiment 4, A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 47.4% PET resin, 14% bromine flame retardant, 4% flame retardant synergist, 4% glow-wire synergist compound, 4% toughening agent, 0.6% antioxidant, 0.6% lubricant, 0.4% nucleating agent, and 25% glass fiber.

[0032] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 1:4:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0033] Comparative Example 1 A high glow-wire flame-retardant reinforced high-performance PET modified material, wherein the raw materials comprise the following components by weight percentage: 45.5% PET resin, 11% bromine flame retardant, 2% flame retardant synergist, 1% toughening agent, 0.2% antioxidant, 0.2% lubricant, 0.1% nucleating agent, and 40% glass fiber.

[0034] A method for preparing a high glow-wire flame-retardant enhanced high-performance PET modified material, which is specifically prepared by the following steps: A1, putting the PET resin, brominated flame retardant, flame retardant synergist, toughening agent, antioxidant, lubricant and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A2. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extrude them, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0035] Comparative Example 2 A high glow-wire flame-retardant reinforced high-performance PET modified material, wherein the raw materials comprise the following components by weight percentage: 58.5% PET resin, 15% bromine flame retardant, 5% flame retardant synergist, 4% toughening agent, 1% antioxidant, 1% lubricant, 0.5% nucleating agent and 15% glass fiber.

[0036] A1, putting the PET resin, brominated flame retardant, flame retardant synergist, toughening agent, antioxidant, lubricant and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A2. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extrude them, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0037] Comparative Example 3 A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 50.2% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 0.5% glow-wire synergist compound, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0038] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 1:3:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0039] Comparative Example 4 A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 45.2% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 5.5% glow-wire synergist compound, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0040] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 1:3:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0041] Comparative Example 5 A high glow-wire flame-retardant reinforced high-performance PET modified material, wherein the raw materials comprise the following components by weight percentage: 47.7% PET resin, 12% bromine flame retardant, 3% glow-wire synergist compound a, 3% flame retardant synergist, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0042] A1. Mix 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate in a powder grinder for 5 minutes in a mass ratio of 4:2. After treatment, a glow-wire synergist compound a is obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound a, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0043] Comparative Example 6 A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 47.7% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 3% glow-wire synergist compound b3%, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0044] A1. Mix boehmite and barium dihydrogen phosphate in a powder grinder for 5 minutes in a mass ratio of 1:2. After treatment, a glow-wire synergist compound b is obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound b, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0045] Comparative Example 7 A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 47.7% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 3% glow-wire synergist compound c3%, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0046] A1. Boehmite and 1,3-phenylene phosphate tetrakis (2,6-dimethylphenyl) ester were mixed in a powder mill at a mass ratio of 1:4 for 5 minutes, and then treated to obtain a glow-wire synergist compound c; A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0047] Comparative Example 8 A high glow-wire flame-retardant reinforced high-performance PET modified material, the raw materials comprising the following components by weight percentage: 47.7% PET resin, 12% bromine flame retardant, 3% flame retardant synergist, 3% glow-wire synergist compound, 3% toughening agent, 0.5% antioxidant, 0.5% lubricant, 0.3% nucleating agent, and 30% glass fiber.

[0048] A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder. The mass ratio of the three was 2:3:2. After treatment, a glow-wire synergist compound was obtained. A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0049] Comparative Example 9 A high glow-wire flame-retardant reinforced high-performance PET modified material, wherein the raw materials comprise the following components by weight percentage: 47.8% PET resin, 14% bromine flame retardant, 4% flame retardant synergist, 4% glow-wire synergist compound, 4% toughening agent, 0.6% antioxidant, 0.6% lubricant, and 25% glass fiber.

[0050] A1. Put boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate, barium dihydrogen phosphate, PET resin, brominated flame retardant, flame retardant synergist, toughening agent, antioxidant and lubricant into a blender, mix and stir evenly to obtain a mixture B; A2. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extrude them, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

[0051] The performance standards and performance test methods are as follows: 1. Tensile strength (GB / T1040.2-2022) my country's national standard number: GB / T1040.2-2022 my country's national standard name: Determination of tensile properties of plastic materials Part 2: Modulus, tensile stress-strain curve Test method: The specimen is dumbbell-shaped or flat (thickness ≥ 1 mm) and is cut along the tensile direction of the material.

[0052] The sample is stretched at a constant rate (e.g., 50 mm / min) until it breaks, and the stress-strain curve is recorded.

[0053] Number of tests: at least 5 times (GB / T1040.2 requires ≥5 parallel tests).

[0054] Calculation of results: Take the arithmetic mean of 5 fracture stresses, accurate to ±1%.

[0055] 2. Bending strength (GB / T9341-2008) my country's national standard number: GB / T9341-2008 Name of my country's national standard: Determination of bending properties of plastic materials Test method: The specimen is a rectangular plate (thickness ≥ 2 mm) with a span of 4 times the thickness.

[0056] Apply load at a constant rate (e.g. 1 mm / min) until the specimen breaks in mid-span bending.

[0057] Number of tests: at least 5 times. If the deviation is greater than 5%, retest is required.

[0058] Result calculation: Take the average value of 5 bending stresses (unit: MPa).

[0059] 3. Izod beam notched impact strength (GB / T1843-2008) my country's national standard number: GB / T1843-2008 Name of my country's national standard: Determination of Izod notched impact strength of plastic materials Test method: The specimen is a strip sample with a notch (such as a V-shaped notch, with a depth of 2mm).

[0060] The sample was placed on the support of the impact tester and the pendulum impact was released at a rate of 2.75 J / s.

[0061] Test times: Each group of samples is tested 5 times (GB / T1843 requires ≥5 times).

[0062] Result calculation: Take the average value of 5 impact strengths (unit: kJ / m²).

[0063] 4. Flame retardancy (UL94) International standard: UL 94.

[0064] International standard name: Standard for Safety Testing for Flammability of Electrical and Electronic Materials Test method: UL94-2023 Section 8 5. Glow wire flammability index (IEC 60695-2-13:2021) International standard: IEC 60695-2-13:2021 Use a nickel-chromium wire (temperature set to 750℃±5℃) to contact the surface of the sample and observe whether it ignites or drips.

[0065] Number of tests: Each sample needs to be tested 5 times.

[0066] Result calculation: If there is no combustion in all 5 tests, it is judged as "passed"; otherwise, the worst result is taken.

[0067] General instructions Sample preparation: All tests must be prepared according to standard requirements (such as injection temperature, annealing conditions).

[0068] Data consistency: If the range of the five test results is greater than 10%, new samples must be prepared and retested.

[0069] The glow-wire synergist compound a in Comparative Examples 1 to 9 does not contain boehmite; the glow-wire synergist compound b does not contain 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate; the glow-wire synergist compound c does not contain barium dihydrogen phosphate; the boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate in Comparative Example 9 are not pretreated, and the specific composition is shown in the following table: The specific proportions of Example 1 to Example 4 are as follows: The data of Comparative Examples 1-9 and Examples 1-4 are as follows: The data of Comparative Examples 1-8 and Examples 1-3 show that the addition of the glow-wire synergist compound will cause the material performance to decline. When the addition amount is low, the impact on the performance is relatively slight. When the addition amount is higher than 5%, the impact on the material's bending strength and Izod notched impact strength performance is significantly reduced. However, the glow-wire synergist compound can significantly improve the glow-wire of the material, help to increase the glow-wire temperature, and improve the stability of the glow-wire of the product. Therefore, the addition amount of the compound should be selected in a suitable addition ratio to meet the use requirements of the material. In addition, the pretreatment of the glow-wire synergist compound can significantly improve the stability of the glow-wire of the product.

[0070] The data of comparative examples 6-8 show that the addition of boehmite will cause a decrease in material performance, but significantly improve the dark fire of the glow wire of the product. The effects of 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate on material performance are negligible, and can effectively improve the glow wire temperature and glow wire stability of the product.

[0071] The data of Comparative Example 9 and Example 4 show that the addition of nucleating agent significantly improves the sticking condition and the surface of the product. The nucleating agent can be evenly dispersed in the polymer melt, provide and generate tiny crystal nuclei, form a uniform and dense crystal structure, accelerate the crystallization of PET, have extremely high nucleation efficiency for PET, and reduce the molecular weight very little. In the process of melt cooling crystallization, the thermal crystallization temperature is effectively increased, the crystallization speed is accelerated, and the sticking condition can be significantly improved, and the surface of the product can be improved.

[0072] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions. The sentence "includes an element defined by ... does not exclude the existence of other identical elements in the process, method, article or device including the element".

[0073] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A high glow-wire flame retardant enhanced high-performance PET modified material, characterized in that: The raw materials include the following components by weight percentage: PET resin 44.5%-52.5%, brominated flame retardant 11%-15%, flame retardant synergist 2%-5%, glow wire synergist compound 1%-5%, toughening agent 1%-4%, antioxidant 0.2%-1%, lubricant 0.2%-1%, nucleating agent 0.1%-0.5% and glass fiber 15%-40%; The glow-wire synergist compound is a compound of boehmite, 1,3-phenylene phosphate tetrakis (2,6-dimethylphenyl) ester and barium dihydrogen phosphate, the mass ratio of the three being 1-2:3-4:2, wherein the boehmite is nano-boehmite with an average particle size of 10-20 nm.

2. The high glow-wire flame retardant enhanced high-performance PET modified material according to claim 1, characterized in that: The brominated flame retardant is one or more of brominated epoxy, brominated polystyrene, and brominated triazine; The flame retardant synergist is one or more of antimony trioxide and sodium antimonate; The toughening agent is one or more of POE-g-GMA, POE grafted maleic anhydride, ethylene-methyl acrylate-glycidyl methacrylate and ethylene-butyl acrylate-glycidyl methacrylate; The antioxidant is one or more of antioxidant 1010, antioxidant 168, and antioxidant 1098; The lubricant is one or more of PETS, 540A, and silicone powder; The nucleating agent is polyester nucleating agent Sanulater HK250; The diameter of the glass fiber is 8-16 microns.

3. The high glow-wire flame retardant enhanced high-performance PET modified material according to claim 1, characterized in that: The intrinsic viscosity of the PET resin is 0.660-0.700 dl / g, the melt flow rate is 90-110 g / 10 min under the test conditions of 265° C. / 2.16 kg, and the model of the PET resin is KH2678C.

4. A method for preparing a high glow-wire flame retardant enhanced high-performance PET modified material according to any one of claims 1, 2, and 3, characterized in that: Specifically prepared by the following steps: A1. Boehmite, 1,3-phenylene tetrakis(2,6-dimethylphenyl)phosphate and barium dihydrogen phosphate were mixed evenly for 5 minutes using a powder grinder, and the mixture was treated to obtain a glow-wire synergist compound; A2, putting the PET resin, brominated flame retardant, flame retardant synergist, glow-wire synergist compound, toughening agent, antioxidant, lubricant, and nucleating agent into a blender, mixing and stirring evenly to obtain a mixture B; A3. Put the mixture B and glass fiber into a twin-screw extruder, heat them until they are melted and extruded, so as to obtain a high glow-wire flame-retardant and reinforced high-performance PET modified material.

5. The method for preparing a high glow-wire flame retardant enhanced high-performance PET modified material according to claim 4, characterized in that: The melt extrusion temperature in A3 is 220-280° C., and the screw speed is 300-600 r / min.

Citation Information

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