Halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) composition as well as preparation method and application thereof

By adding halogen-free flame retardant and specific synergistic agent to the PBT material, the high-temperature free radical reaction is suppressed, and the glow wire ignition temperature and heat resistance stability of halogen-free flame retardant PBT material is improved, and the material phase in the prior art is solved The problems of poor capacitance and degraded mechanical properties achieve high flame retardancy and good mechanical properties.

CN119307071APending Publication Date: 2025-01-14KINGFA SCI & TECH CO LTD

Patent Information

Application Number
CN202411542010.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-31
Publication Date
2025-01-14

AI Technical Summary

Technical Problem

The existing halogen-free flame-retardant PBT materials have shortcomings in improving the ignition temperature and heat resistance stability of the glow wire. Moreover, the compatibility with PBT when the halogen-free flame-retardant content is too high, resulting in a decrease in mechanical properties and affecting product application.

Method used

Polybutylene terephthalate is used as the matrix, and the synergistic effect of halogen-free flame retardant, phenolamide metal deactivator, free radical capture agent and hydroperoxide capture agent is added to inhibit the freedom of PBT at high temperatures. The base chain depolymerization reaction improves the ignition temperature and heat resistance of the glow wire, and increases the tensile strength through glass fibers.

Benefits of technology

Halogen-free flame retardant enhancement PBT composition is achieved with high flame retardancy, glow wire ignition temperature and heat resistance stability, and has high mechanical properties, meeting the requirements of IEC60695 standard.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure BDA0005113006070000021
    Figure BDA0005113006070000021
  • Figure BDA0005113006070000041
    Figure BDA0005113006070000041
  • Figure BDA0005113006070000081
    Figure BDA0005113006070000081
Patent Text Reader

Abstract

The invention discloses a halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) composition as well as a preparation method and application thereof, and relates to the technical field of high polymer materials. The halogen-free flame-retardant reinforced PBT composition comprises polybutylene terephthalate, a halogen-free flame retardant, a melamine flame-retardant synergist, glass fibers, a phenol amide metal deactivator, a free radical trapping agent and a hydroperoxide trapping agent. According to the halogen-free flame-retardant reinforced PBT composition disclosed by the invention, under the combined action of all the components, the effects of improving the flame retardance, the ignition temperature of a glowing filament and the heat-resistant stability can be achieved, and the halogen-free flame-retardant reinforced PBT composition has relatively high mechanical properties. The flame retardant property of the halogen-free flame-retardant reinforced PBT composition reaches V-0 or above, the tensile strength is 95 Mpa or above, the glowing filament ignition temperature is 800 DEG C or above, and the thermal weight loss T1% temperature is 335 DEG C or above.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and more specifically to a halogen-free flame-retardant reinforced PBT composition and a preparation method and application thereof. Background Art

[0002] More than 40% of the weight of modern electronic and electrical equipment is made of flammable plastic insulating materials. These devices can cause fires due to overheating, leakage, sparks and aging, which can cause huge losses to people's lives and property safety. The glow-wire test simulates the thermal stress effect of heat sources such as overheating components or overload resistors on surrounding parts in a short period of time, which can reflect the stability of electronic and electrical products at work. According to the IEC60695 standard, for unattended electrical appliances, when the rated current is greater than 0.2A, it must meet the following requirements: UL94V-0 level and 750℃ glow-wire contact material does not catch fire within 30s or the burning time is less than 5s, that is, the glow-wire ignition temperature (GWIT) is greater than 775℃; for specific components such as connectors, contact switches, motors and circuit breaker housings, the GWIT temperature is also required to be 850℃ and the glow-wire flammability index (GWFI) is 960℃.

[0003] As one of the five commonly used engineering plastics, polybutylene terephthalate (PBT) has the advantages of high temperature resistance, oil resistance, chemical corrosion resistance, good electrical properties, and short molding cycle. It is widely used in many fields such as electronics, electrical appliances, and home appliances. Therefore, the demand for high glow wire performance of products is increasing day by day. In order to make PBT materials have a higher GWIT temperature, it is usually necessary to compound brominated flame retardants and halogen-free flame retardants in PBT materials. For example, patent CN113956621A discloses a flame-retardant PBT composition and its preparation method and application, which has the advantages of good thin-wall flame retardant performance, GWIT ≥ 850℃, less mold fouling and corrosion; but it requires the addition of a large amount of brominated flame retardants. However, when the solid waste of brominated flame retardants is incinerated, toxic substances will be produced, which will cause lasting harm to the environment and humans, so the halogen-free and environmentally friendly PBT materials are the development trend.

[0004] For halogen-free flame retardant PBT compositions, it is difficult to effectively increase the glow-wire ignition temperature due to the catalytic degradation of PBT by halogen-free flame retardants; at the same time, when the content of halogen-free flame retardants is too high, the compatibility with PBT is poor, and the heat resistance of the composition is poor under high-temperature molding conditions, resulting in a significant decrease in the mechanical properties of PBT, which seriously affects the application of the product. Patent CN117384471A discloses a halogen-free flame retardant PBT composition and a preparation method thereof, comprising PBT resin, halogen-free flame retardant, phosphite synergist, melamine synergist and glass fiber, and uses hydrated zinc borate as a heat-resistant modifier. Based on the combination of specific heat-resistant modifiers and lubricants, the halogen-free flame retardant and flame retardant synergist in the product can fully exert their flame retardant properties, achieve extremely high glow-wire ignition temperatures, and maintain excellent flame retardant properties under the thinnest 0.4mm thickness processing. However, it relies on the effect of hydrated zinc borate to inhibit product burning; however, hydrated zinc borate is easy to degrade and has poor high-temperature stability, which reduces the heat resistance of PBT materials; and fails to take into account both the improvement of GWIT temperature and heat resistance stability. Summary of the invention

[0005] The object of the present invention is to overcome the defects and shortcomings of the prior art and provide a halogen-free flame retardant reinforced PBT composition, which can improve the flame retardancy, glow-wire ignition temperature and heat stability of the PBT composition and has higher mechanical properties.

[0006] Another object of the present invention is to provide a method for preparing a halogen-free flame retardant reinforced PBT composition.

[0007] Another object of the present invention is to provide a use of a halogen-free flame retardant reinforced PBT composition in the preparation of electronic appliances.

[0008] The above-mentioned purpose of the present invention is achieved through the following technical solutions:

[0009] The present invention protects a halogen-free flame retardant reinforced PBT composition, comprising the following components in parts by weight:

[0010]

[0011] In the halogen-free flame-retardant enhanced PBT composition of the present invention, polybutylene terephthalate is used as a matrix, and an appropriate amount of halogen-free flame retardant and melamine flame retardant synergist are added to improve the flame retardancy of the PBT composition and increase the GWIT temperature; at the same time, the synergistic effect of adding a phenolamide metal deactivator, a free radical scavenger and a hydroperoxide scavenger can reduce alkyl radicals and hydroperoxide radicals, inhibit the free radical chain depolymerization reaction of PBT at high temperature, slow down the degradation of the material system, and reduce the release of combustible gas butadiene, thereby improving the effect of glow wire. Among them, the residual metal ions in the system are complexed by the phenolamide metal deactivator, thereby reducing the generation of initial alkyl radicals; the free radical scavenger is used to quench the active alkyl radicals and hydroperoxide radicals in the system and convert them into inactive substances; and the hydroperoxide scavenger is used to convert the hydroperoxide in the system into an inactive product; thereby, the free radical chain depolymerization reaction of PBT at high temperature is inhibited under the synergistic effect of the compound, and the GWIT temperature and heat resistance stability are improved. In addition, glass fiber is added to improve the tensile strength. The halogen-free flame retardant reinforced PBT composition of the present invention can improve the flame retardancy, glow wire ignition temperature and heat resistance stability through the joint action of various components, and has higher mechanical properties.

[0012] In some embodiments, the content of polybutylene terephthalate that can achieve the purpose of the present invention can be 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, 46 parts, 47 parts, 48 ​​parts, 49 parts, 50 parts, 51 parts, 52 parts, 53 parts, 54 parts or 55 parts or any range therebetween.

[0013] In some embodiments, the content of glass fiber that can achieve the purpose of the present invention can be 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts or 38 parts or any range therebetween.

[0014] In some embodiments, the content of the halogen-free flame retardant that can achieve the purpose of the present invention can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts or 18 parts or any range between the above values.

[0015] In some embodiments, the content of the melamine flame retardant synergist that can achieve the purpose of the present invention can be 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts or 15 parts or any range therebetween.

[0016] In some embodiments, the content of the phenolamide metal deactivator that can achieve the purpose of the present invention can be 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts or 2.0 parts or any range between the above values.

[0017] In some embodiments, the content of the free radical scavenger that can achieve the purpose of the present invention can be 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts or 2.0 parts or any range between the above values.

[0018] In some embodiments, the content of the hydroperoxide capture agent that can achieve the purpose of the present invention can be 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts or 2.0 parts or any range therebetween.

[0019] Preferably, the following components are included in parts by weight:

[0020]

[0021] In some embodiments, the polybutylene terephthalate has an intrinsic viscosity of 0.6-2 dL / g at 25°C; preferably, the intrinsic viscosity of the polybutylene terephthalate is 0.7-1.5 dL / g at 25°C.

[0022] In some embodiments, the mass ratio of the free radical scavenger to the hydroperoxide scavenger is 1:(1.5-2.5), and / or the amount of the phenolamide metal deactivator is 0.5-1.5 parts. By optimizing the proportion of each component, the GWIT temperature and heat resistance stability of the material can be improved.

[0023] In addition, the content of phenolamide metal deactivators, free radical scavengers or hydroperoxide scavengers in the PBT composition is also an important influencing factor. When the added amount is too low, the effect of increasing the GWIT temperature cannot be achieved; when the added amount is too high, since these three are small molecular substances, excessive addition will easily precipitate during long-term actual injection molding production, resulting in mold deposits on the mold surface, which will affect the surface performance and appearance of the product.

[0024] In some embodiments, the minimum mass percentage of polybutylene terephthalate (PBT) in the halogen-free flame retardant reinforced PBT composition is 35%.

[0025] In some embodiments, the phenolamide metal deactivator is a compound containing a hydrazide group, an oxalamide group and / or a benzamide group; specifically, the phenolamide metal deactivator is one or more of 1,2-bis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]hydrazine, (3,5-di-tert-butyl-4-hydroxyphenyl)propionate oxalyl(diimino-2,1-ethylene ester), 2-hydroxy-N-1H-1,2,4-triazol-3-ylbenzamide or dodecanedioic acid bis[2-(2-hydroxybenzoyl)hydrazide].

[0026] In some embodiments, the free radical scavenger of the present invention is a compound that can react with free radicals to stabilize or eliminate free radicals, especially for reacting alkyl free radicals and / or hydroperoxide free radicals; the free radical scavenger does not contain hydrazide groups, oxalamide groups and / or benzamide groups, and specifically, the free radical scavenger is one or more of hindered amine compounds, hydroxylamine compounds, aniline compounds, hydroxylamine compounds, hindered phenol compounds or semi-hindered phenol compounds. Preferably, it is an aniline compound and a semi-hindered phenol compound, and more preferably, it is an aniline compound.

[0027] Optionally, the aniline compound is 4,4'-di(phenylisopropyl)diphenylamine.

[0028] Optionally, the hindered amine compound is selected from one or more of poly[[6-[(1,1,3,3-tetramethylbutyl)amino]-1,3,5-triazine-2,4-diyl][(2,2,6,6-tetramethyl-4-piperidinyl)imino]-1,6-hexanediyl[(2,2,6,6-tetramethyl-4-piperidinyl)imino]] or bis(2,2,6,6-tetramethyl-4-piperidinyl)sebacate.

[0029] Optionally, the hydroxylamine compound is selected from bis(octadecyl)hydroxylamine.

[0030] Optionally, the hindered phenol compound is selected from one or more of pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate and N,N'-(hexane-1,6-diyl)bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionamide].

[0031] Optionally, the semi-hindered phenol compound is n-octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate.

[0032] In some embodiments, the hydroperoxide scavenger of the present invention is used to react with hydroperoxide to convert it into an inactive product, and the hydroperoxide scavenger does not contain a hydrazide group, an oxalamide group and / or a benzamide group. Specifically, the hydroperoxide scavenger is one or more of an aryl phosphite compound, an alkyl phosphite compound and a thioester compound. Preferably, the hydroperoxide scavenger is an aryl phosphite compound.

[0033] Preferably, the aromatic phosphite compound is tris(2,4-di-tert-butylphenyl) phosphite.

[0034] Preferably, the alkyl phosphite compound is selected from one or more of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol diphosphate, bis(2,4-dicumylphenyl)pentaerythritol-diphosphite or 3,9-bis(octadecyl)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane.

[0035] Preferably, the thioester compound is selected from pentaerythritol tetrakis(3-laurylthiopropionate) and / or distearyl thiodipropionate.

[0036] In some embodiments, the melamine flame retardant synergist includes melamine polyphosphate and melamine cyanurate (MCA), and the mass ratio of melamine polyphosphate to melamine cyanurate is (0.5-5): (3-10). Melamine polyphosphate can play a condensed phase flame retardant role, and melamine cyanurate can play a gas phase flame retardant role. The two have a synergistic effect to improve the flame retardant synergistic performance.

[0037] Preferably, the mass ratio of the melamine polyphosphate to melamine cyanurate is (0.7-3.5):(5.5-8.5).

[0038] In some embodiments, the halogen-free flame retardant comprises organic hypophosphite and / or inorganic hypophosphite. Preferably, the halogen-free flame retardant is diethyl aluminum hypophosphite.

[0039] In some embodiments, the composition further comprises 1-5 parts of a toughening agent and 0.5-1.5 parts of a lubricant.

[0040] Preferably, the toughening agent is ethylene-methyl acrylate-glycidyl methacrylate block copolymer.

[0041] Preferably, the lubricant is an ester lubricant.

[0042] The invention discloses a method for preparing a halogen-free flame-retardant reinforced PBT composition, comprising the following steps: uniformly mixing raw material components in a formula amount, and granulating the raw materials by melt extrusion to obtain the halogen-free flame-retardant reinforced PBT composition.

[0043] In some embodiments, the method for preparing the halogen-free flame retardant reinforced PBT composition comprises the following steps:

[0044] S1, uniformly mixing the other components except PBT resin, glass fiber and toughening agent to obtain mixture A;

[0045] S2, mixing the PBT resin and the toughening agent uniformly to obtain a mixture B;

[0046] S3, melt-extrude and granulate the mixture A, the mixture B and the glass fiber to obtain the halogen-free flame-retardant reinforced PBT composition.

[0047] Preferably, in step S1, the mixing speed is 700-900 rpm, and the mixing time is 2-4 minutes.

[0048] Preferably, in step S2, the mixing speed is 600-800 rpm, and the mixing time is 2-4 minutes.

[0049] Preferably, the melt extrusion granulation is carried out in a twin-screw extruder.

[0050] Preferably, the temperature of zone 1 of the twin-screw extruder is 200-230°C, the temperature of zone 2 is 240-260°C, the temperature of zone 3 is 235-255°C, the temperature of zone 4 is 235-255°C, the temperature of zone 5 is 235-255°C, the temperature of zone 6 is 240-260°C, the temperature of zone 7 is 240-260°C, the temperature of zone 8 is 220-240°C, the temperature of zone 9 is 220-240°C, and the temperature of zone 10 is 240-260°C.

[0051] Preferably, the screw speed of the twin-screw extruder is 200 to 450 rpm.

[0052] The invention protects the application of a halogen-free flame-retardant reinforced PBT composition in the preparation of electronic appliances, especially in appliances with high working current (rated current above 0.2A), which can meet the requirements of IEC60695 standard.

[0053] hit

[0054] Compared with the prior art, the present invention has the following beneficial effects:

[0055] The present invention provides a halogen-free flame retardant enhanced PBT composition, in which polybutylene terephthalate is used as a matrix, and an appropriate amount of halogen-free flame retardant and melamine flame retardant synergist are added to improve the flame retardancy of the PBT composition and increase the GWIT temperature; at the same time, the synergistic effect of adding a phenolamide metal deactivator, a free radical scavenger and a hydroperoxide scavenger can reduce alkyl radicals and hydroperoxide radicals, inhibit the free radical chain depolymerization reaction of PBT at high temperature, slow down the degradation of the material system, and reduce the release of combustible gas butadiene, thereby improving the effect of glow wire. Among them, the residual metal ions in the system are complexed by the phenolamide metal deactivator, thereby reducing the generation of initial alkyl radicals; the free radical scavenger is used to quench the active alkyl radicals and hydroperoxide radicals in the system and convert them into inactive substances; and the hydroperoxide scavenger is used to convert the hydroperoxide in the system into an inactive product; thereby, the free radical chain depolymerization reaction of PBT at high temperature is inhibited under the synergistic effect of the compound, and the GWIT temperature and heat resistance stability are improved. DETAILED DESCRIPTION

[0056] The present invention is further described below in conjunction with specific embodiments, but the embodiments do not limit the present invention in any form. Unless otherwise specified, the raw materials and reagents used in the embodiments of the present invention are conventionally purchased raw materials and reagents.

[0057] The raw materials used in the following examples and comparative examples are as follows:

[0058] PBT resin 1#: PBT 1200-211M, Changchun Chemical Company, Taiwan; intrinsic viscosity at 25°C is 0.8 dL / g.

[0059] PBT resin 2#: PBT GX121, Sinopec Yizheng Chemical Fiber Co., Ltd.; intrinsic viscosity at 25°C is 0.98 dl / g.

[0060] PBT resin 3#: PBT GL236, Sinopec Yizheng Chemical Fiber Co., Ltd.; intrinsic viscosity at 25°C is 1.28 dl / g.

[0061] Halogen-free flame retardant 1#: diethyl aluminum hypophosphite; Exolit OP 1230, Clariant, Germany.

[0062] Halogen-free flame retardant 2#: Inorganic aluminum hypophosphite; 5213, Guangdong Tongcheng New Materials Co., Ltd.

[0063] Halogen-free flame retardant synergist 1#: melamine polyphosphate; BUDIT 3141, Budenheim, Germany.

[0064] Halogen-free flame retardant synergist 2#: melamine cyanurate (MCA); MCA-01, Sichuan Fine Chemical Research and Design Institute.

[0065] Toughening agent: ethylene-methyl acrylate-glycidyl methacrylate block copolymer; ELVALOY REINSPTW, DuPont Company, USA.

[0066] Glass fiber: HMG436S-10-4.0, Taishan Glass Fiber Co., Ltd.

[0067] Lubricant: ester lubricant, PETS-AP, Italy Faji Company.

[0068] Phenolamide metal deactivator 1#: (3,5-di-tert-butyl-4-hydroxyphenyl) propionate oxalyl (diimino-2,1-ethylene ester); SONOX 1027, Sanfeng Chemical Company.

[0069] Phenolamide metal deactivator 2#: 1,2-bis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]hydrazine; RIANOXMD-1024, Rianlon Corporation.

[0070] Free radical scavenger 1#: 4,4'-di(phenylisopropyl)diphenylamine, NAUGARD 445, Chemtura Corporation, USA.

[0071] Free radical scavenger 2#: β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, SONOX 1076, Sanfeng Chemical Co., Ltd.

[0072] Free radical scavenger 3#: pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, SONOX1010, Sanfeng Chemical Co., Ltd.

[0073] Hydroperoxide scavenger 1#: tris(2,4-di-tert-butylphenyl) phosphite, SONOX 168, Sanfeng Chemical Co., Ltd.

[0074] Hydroperoxide scavenger 2#: pentaerythritol tetrakis (3-laurylthiopropionate), RIANOX 412S, Rianlon Corporation.

[0075] The preparation method of the halogen-free flame retardant reinforced PBT composition of the following examples and comparative examples comprises the following steps:

[0076] S1, mixing the other components except PBT resin, glass fiber and toughening agent uniformly to obtain a mixture A; the mixing speed is 800 rpm, and the mixing time is 3 minutes;

[0077] S2, mixing the PBT resin and the toughening agent uniformly to obtain a mixture B; the mixing speed is 700 rpm, and the mixing time is 3 minutes;

[0078] S3, melt-extrude and granulate the mixture A, the mixture B and the glass fiber through a twin-screw extruder to obtain the halogen-free flame-retardant reinforced PBT composition.

[0079] Among them, the temperature of zone 1 of the twin-screw extruder is 215°C, the temperature of zone 2 is 250°C, the temperature of zone 3 is 245°C, the temperature of zone 4 is 245°C, the temperature of zone 5 is 245°C, the temperature of zone 6 is 250°C, the temperature of zone 7 is 250°C, the temperature of zone 8 is 230°C, the temperature of zone 9 is 230°C, and the temperature of zone 10 is 250°C; the screw speed is 325 rpm.

[0080] Examples 1 to 21

[0081] This embodiment provides a halogen-free flame retardant reinforced PBT composition, the components of which are shown in Table 1.

[0082] Table 1 Examples 1 to 10 (parts by weight)

[0083]

[0084]

[0085] Table 2 Examples 11 to 21 (parts by weight)

[0086]

[0087]

[0088] Comparative Examples 1 to 7

[0089] This comparative example provides a halogen-free flame retardant reinforced PBT composition, the components of which are shown in Table 3.

[0090] Table 3 Comparative Examples 1 to 7 (parts by weight)

[0091]

[0092] Performance Testing

[0093] The halogen-free flame retardant reinforced PBT composition samples prepared in Examples 1-21 and Comparative Examples 1-7 were respectively subjected to the following tests, and the test results are shown in Table 4;

[0094] 1. Tensile strength: The PBT composition prepared above was tested according to standard ISO 527.

[0095] 2. Flame retardant properties: The PBT composition prepared above was tested according to the UL94 vertical combustion standard.

[0096] 3. Glow Wire Ignition Temperature (GWIT): The PBT composition prepared above was tested and confirmed at different temperatures according to standard IEC 60695-2-2013.

[0097] 4. Heat resistance: The PBT composition prepared above was subjected to a thermogravimetric analysis test, and the temperature at which the mass loss percentage reached 1% (T1%) was used to characterize the heat resistance of the material. The higher the T1% temperature, the better the heat resistance of the material.

[0098] Table 4

[0099]

[0100]

[0101] The halogen-free flame-retardant reinforced PBT composition of the present invention has a flame retardant property of V-0 or above, a tensile strength of 95 MPa or above, a glow-wire ignition temperature of 800° C. or above, and a thermal weight loss T1% temperature of 335° C. or above; and has good flame retardant properties, mechanical properties, GWIT temperature and heat resistance stability.

[0102] Compared with Example 1, Comparative Example 1 does not contain a metal deactivator, a free radical scavenger, and a hydroperoxide scavenger, and its GWIT temperature and thermal weight loss T1% temperature are lower. When one of the metal deactivator, free radical scavenger, and hydroperoxide scavenger is used alone in Comparative Examples 2-4, there is no obvious improvement in its GWIT temperature and thermal weight loss T1% temperature. When any two of the metal deactivators, free radical scavengers, and hydroperoxide scavengers are used in combination in Comparative Examples 5-7, the GWIT temperature and thermal weight loss T1% temperature are improved, but the effect is not lower than the halogen-free flame retardant reinforced PBT composition of Example 1, proving that the metal deactivator, free radical scavenger, and hydroperoxide scavenger of the present application have a synergistic effect, which can increase the GWIT temperature and improve thermal stability.

[0103] The above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the embodiments here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A halogen-free flame retardant reinforced PBT composition, characterized in that: The composition includes the following components in parts by weight:

2. The halogen-free flame retardant reinforced PBT composition according to claim 1, characterized in that: The mass ratio of the free radical scavenger to the hydroperoxide scavenger is 1:(1.5-2.5), and / or the amount of the phenolamide metal deactivator is 0.5-1.5 parts.

3. The halogen-free flame-retardant reinforced PBT composition according to claim 1, characterized in that: The phenolamide metal deactivator is one or more of 1,2-bis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]hydrazine, (3,5-di-tert-butyl-4-hydroxyphenyl)propionyl oxalyl(diimino-2,1-ethylene ester), 2-hydroxy-N-1H-1,2,4-triazol-3-ylbenzamide or dodecanedioic acid bis[2-(2-hydroxybenzoyl)hydrazide].

4. The halogen-free flame retardant reinforced PBT composition according to claim 1, characterized in that: The free radical scavenger is one or more of aniline compounds, hindered amine compounds, hydroxylamine compounds, hindered phenol compounds or semi-hindered phenol compounds.

5. The halogen-free flame retardant reinforced PBT composition according to claim 1, characterized in that: The hydroperoxide scavenger is one or more of an aryl phosphite compound, an alkyl phosphite compound or a thioester compound.

6. The halogen-free flame retardant reinforced PBT composition according to claim 1, characterized in that: The polybutylene terephthalate has an intrinsic viscosity of 0.7-1.5 dL / g at 25°C.

7. The halogen-free flame-retardant reinforced PBT composition according to claim 1, characterized in that: The melamine flame retardant synergist comprises melamine polyphosphate and melamine cyanurate, and the mass ratio of the melamine polyphosphate to the melamine cyanurate is (0.5-5):(3-10).

8. The halogen-free flame-retardant reinforced PBT composition according to claim 1, characterized in that: The halogen-free flame retardant is an organic hypophosphite.

9. A method for preparing the halogen-free flame-retardant reinforced PBT composition according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: uniformly mixing the raw material components in the formula amount, and granulating the raw materials by melt extrusion to obtain the halogen-free flame retardant reinforced PBT composition.

10. Use of the halogen-free flame-retardant reinforced PBT composition according to any one of claims 1 to 8 in the preparation of electronic appliances.

Citation Information

Patent Citations

  • Copper ion migration inhibitor, PBT composite material and preparation method thereof

    CN116515168A

  • Halogen-free flame-retardant PBT composition and preparation method thereof

    CN117384471A

  • Low-smoke density high-performance halogen-free flame-retardant reinforced PBT composite and preparation method therefor

    WO2021253772A1

Cited By

  • PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof

    CN121673771A

  • PBT composite material, preparation method and application thereof

    CN121673771B

  • Polybutylene terephthalate resin composition, preparation method therefor and use thereof

    WO2026200757A1