CN117327392B - A halogen-free flame-retardant polyamide composition and its preparation method and application - Google Patents
A halogen-free flame-retardant polyamide composition and its preparation method and application Download PDFInfo
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- CN117327392B CN117327392B CN202311148349.5A CN202311148349A CN117327392B CN 117327392 B CN117327392 B CN 117327392B CN 202311148349 A CN202311148349 A CN 202311148349A CN 117327392 B CN117327392 B CN 117327392B
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- 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
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本发明公开了一种无卤阻燃聚酰胺组合物及其制备方法和应用。所述无卤阻燃聚酰胺组合物包括如下按照重量份计算的组分：聚酰胺树脂30～80份；玻璃纤维10～40份；无卤阻燃剂10～30份；含锌化合物0.1～3份；所述含锌化合物的熔点≤600℃；所述无卤阻燃剂为二烷基次磷酸盐。本发明通过加入特定熔点的无机含锌化合物，在火焰温度会发生离子化，生成锌离子，从而与聚酰胺树脂和无卤阻燃剂发生配位，来避免燃烧过程中发生熔滴现象，且不会影响聚酰胺组合物的流动性。The present invention discloses a halogen-free flame-retardant polyamide composition, a preparation method and an application thereof. The halogen-free flame-retardant polyamide composition comprises the following components calculated by weight: 30 to 80 parts of polyamide resin; 10 to 40 parts of glass fiber; 10 to 30 parts of halogen-free flame retardant; 0.1 to 3 parts of zinc-containing compound; the melting point of the zinc-containing compound is ≤ 600°C; the halogen-free flame retardant is dialkyl hypophosphite. The present invention adds an inorganic zinc-containing compound with a specific melting point, which will be ionized at the flame temperature to generate zinc ions, thereby coordinating with the polyamide resin and the halogen-free flame retardant to avoid the occurrence of droplets during the combustion process, and will not affect the fluidity of the polyamide composition.
Description
Technical Field
The invention relates to the technical field of engineering plastics, in particular to a halogen-free flame-retardant polyamide composition, and a preparation method and application thereof.
Background
The polyamide material is a material widely applied in engineering plastics, has excellent heat resistance, solvent resistance, mechanics and processing performance, and is widely applied to the fields of electronics and electrics, rail transit, electric tools, household appliances, sports equipment and the like. At present, the halogen-free flame retardant applied to glass fiber reinforcement mainly comprises two main types of basic systems, namely red phosphorus and a phosphorus-nitrogen flame retardant system. However, when the glass fiber reinforced halogen-free flame retardant polyamide material is subjected to flame retardant test, the problem of flame retardant failure caused by dripping is often caused. To solve this problem, it is common in the prior art to add an anti-dripping agent such as polytetrafluoroethylene to improve the anti-dripping effect of the material, but this method reduces the fluidity of the system, resulting in the composition having a phenomenon of lack of glue during injection molding and being expensive.
Therefore, there is a need in the art to develop a halogen-free flame retardant polyamide composition having both good anti-drip effect and good flowability.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a halogen-free flame retardant polyamide composition which has good anti-dripping performance and flowability.
It is another object of the present invention to provide a method for preparing the halogen-free flame retardant polyamide composition.
The invention further aims to provide application of the halogen-free flame retardant polyamide composition in a new energy connector and an energy storage connector.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the halogen-free flame retardant polyamide composition comprises the following components in parts by weight:
The melting point of the zinc-containing compound is less than or equal to 600 ℃, and the halogen-free flame retardant is dialkyl hypophosphite.
The present invention provides a halogen-free flame retardant polyamide composition, wherein the halogen-free flame retardant polyamide composition is prepared by adding a zinc-containing compound with a melting point of not more than 600 ℃. Generally, the flame temperature is 500-600 ℃, the melting point of the zinc-containing compound is below the flame temperature and can be ionized, generated metal ions can coordinate with polyamide resin and dialkyl hypophosphite, so that dripping during combustion is slowed down, the dripping resistance effect is achieved, the flowability of the polyamide composition cannot be affected by the addition of the zinc-containing compound, and the zinc-containing compound can be well molded in the subsequent processing process.
In the present invention, the melting point of the zinc-containing compound is not more than 600 ℃, and specifically may be 550 ℃, 500 ℃, 450 ℃, 400 ℃, 350 ℃, 300 ℃, 250 ℃, 200 ℃, 150 ℃, 100 ℃, or the like. In the present invention, anions of the zinc-containing compound are not particularly limited, such as, but not limited to, bromide, chloride, iodide, sulfate, acetate, carbonate, basic carbonate, octoate, nitrite, carboxylate. Zinc-containing compounds having melting points of no more than 600 ℃ are within the skill of the art to practice the present invention. Zinc-containing compounds having a melting point of no more than 600 ℃ include, but are not limited to, one or more of zinc bromide, zinc chloride, zinc iodide, zinc sulfate, zinc acetate, zinc carbonate, basic zinc carbonate, zinc octoate, zinc nitrite, zinc carboxylate.
Further, the melting point of the zinc-containing compound is 200-400 ℃.
Further, the melting point of the zinc-containing compound is 220-300 ℃.
Further, the zinc-containing compound accounts for 0.09wt% to 7.5wt% based on the sum of the polyamide resin and the dialkylhypophosphite. Such as but not limited to 0.1wt％、0.5wt％、1.0wt％、1.5wt％、2.0wt％、2.5wt％、3.0wt％、3.5wt％、4.0wt％、4.5wt％、5.0wt％、5.5wt％、6.0wt％、6.5wt％、7.0wt％ and 7.5wt%, etc.
Further, the halogen-free flame retardant polyamide composition comprises the following components in parts by weight:
Further, the dialkyl phosphinate is one or more of methyl ethyl aluminum phosphinate, diethyl zinc phosphinate or diethyl titanium phosphinate.
In the halogen-free flame retardant polyamide composition, the content of the polyamide resin is not less than 28wt%. Such as, but not limited to, 30wt%, 35wt%, 40wt%, 45wt%, 50wt%, 55wt%, 60wt%, etc.
Further, the polyamide resin is a semiaromatic polyamide and/or an aliphatic polyamide.
Specifically, the semi-aromatic polyamide is selected from one or more of PA6T/66, PA6I, PA T/6I, PA T/M5T, PA9T, PA T/66, PA10T, PA10T/66, PA10T/10I, PA10T/1010 and PA12T, PA I.
The aliphatic polyamide is selected from one or more of PA6, PA66, PA610, PA612, PA1010, PA1012, PA1212, PA11 and PA 12.
The present invention has no special requirement on the relative viscosity of the polyamide resin. When the relative viscosity of the polyamide resin is 2.1-2.7, the anti-dripping performance of the prepared halogen-free flame retardant polyamide composition is ensured, and meanwhile, the processing performance of the material can be further improved.
Further, the relative viscosity of the polyamide resin is 2.1-2.4.
Specifically, the polyamide resin was tested with a relative viscosity measurement standard of ISO 307-2017.
Further, the glass fiber comprises chopped strands A-, E-, C-, D-, S-, R-glass fiber, and the glass fiber has a cross-sectional shape of one of a circle, an ellipse or a square.
Further, the halogen-free flame retardant polyamide composition further comprises 0.1-1 part of antioxidant.
The invention can select one or more of common antioxidants including hindered phenol antioxidants, phosphite antioxidants, diphenylamine antioxidants, copper salt antioxidants and thioether antioxidants.
Specifically, the hindered phenol antioxidant is one or more of N, N' -hexamethylenebis (3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide (Irganox 1098), tetra [1093,5-di-tert-butyl-4-hydroxy-phenyl) -propionic acid ] pentaerythritol ester (Irganox 1010), triethylene glycol bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) -propionic acid ester (Iragnox 259), beta- (4-hydroxy-3, 5-di-tert-butylphenyl) propionic acid N-octadecyl ester (Iragno 1076) or spiro ethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) -propionic acid ester ] (ADK AO-80).
The phosphite antioxidant is one or more of 2, 4-di-tert-butylphenol (Irganox 168), bis (2, 6-di-tert-butyl-4-tolyl) pentaerythritol phosphite (PEP-36) or 627A.
The diphenylamine antioxidant is 4,4 '-bis (alpha, alpha' -dimethylbenzyl) diphenylamine.
The copper salt antioxidant is a mixture of 8:1:1K/Cu/ZnBLEND or KI/CuI.
The thioether antioxidant is sulfur distearyl ester of dipropionate one or more of dilauryl thiodipropionate or pentaerythritol dodecyl thiopropyl ester.
The invention provides a preparation method for protecting the halogen-free flame retardant polyamide composition, which comprises the following steps:
And (3) carrying out melt blending, extrusion granulation on the polyamide resin, the glass fiber, the halogen-free flame retardant and the zinc-containing compound to obtain the halogen-free flame retardant composition.
Further, the extrusion granulation is performed in a twin screw extruder.
Further, the temperature of a first area of the twin-screw extruder is 180-200 ℃, the temperature of a second area of the twin-screw extruder is 250-270 ℃, the temperature of a third area of the twin-screw extruder is 260-280 ℃, the temperature of a fourth area of the twin-screw extruder is 265-285 ℃, the temperature of a fifth area of the twin-screw extruder is 265-285 ℃, the temperature of a sixth area of the twin-screw extruder is 260-280 ℃, the temperature of a seventh area of the twin-screw extruder is 260-280 ℃, the temperature of a ninth area of the twin-screw extruder is 260-280 ℃, and the screw speed of the twin-screw extruder is 300-500 rpm.
The invention protects application of the halogen-free flame retardant polyamide composition in new energy connectors and energy storage connectors.
Compared with the prior art, the invention has the beneficial effects that:
The invention provides a halogen-free flame-retardant polyamide composition, wherein a zinc-containing compound with a melting point less than or equal to 600 ℃ is added into the polyamide composition, and the zinc-containing compound is ionized to generate zinc ions at a common flame temperature, so that the zinc ions can coordinate with polyamide resin and a halogen-free flame retardant, and further melt dripping during combustion is avoided, and the dripping-resistant mode has no obvious influence on the fluidity of the composition.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
The raw materials used in the examples and comparative examples of the present invention:
polyamide resin:
polyamide resin 1:pa66 u2501, resin relative viscosity 2.1, available from inflight;
polyamide resin 2:PA66 U3600 NC01, resin relative viscosity 2.4, available from inflight;
Polyamide resin 3:PA66 U4800 NC01, resin relative viscosity 2.7, available from inflight;
polyamide resin 4:pa6hy-2500A, resin relative viscosity 2.5, purchased from neopenttiming;
glass fiber, ECS10-30-568H, available from China boulder Co., ltd;
Halogen-free flame retardant:
flame retardant 1, diethyl aluminum hypophosphite, LFR-8003, available from Jiangsu Lishide New Material Co., ltd;
flame retardant 2, red phosphorus master batch, FR9950T, purchased from Tongcheng Xin Chemicals Co., ltd;
Zinc-containing compound:
zinc acetate with a melting point of 237 ℃;
zinc chloride with a melting point of 283 ℃;
Basic zinc carbonate with a melting point of 300 ℃;
Zinc bromide with a melting point of 394 ℃;
Zinc phosphate with a melting point of 900 ℃;
zinc sulfide with a melting point of 1700 ℃;
Sodium acetate with a melting point of 324 ℃;
Polytetrafluoroethylene, X-010, available from guangzhou silicon composite limited;
antioxidant 1098, which is commercially available, and the same antioxidant was used in the parallel experiments of examples and comparative examples.
Examples 1 to 10 and comparative examples 1 to 6
According to the formulations in tables 1-2, halogen-free flame retardant polyamide compositions were prepared according to the following preparation methods:
the preparation method comprises the steps of putting polyamide resin, glass fiber, halogen-free flame retardant and zinc-containing compound into a high-speed mixer, mixing for 1-2 minutes at the rotating speed of 600-800 r/min, then putting into a double-screw extruder, carrying out melt blending, extrusion and granulation to obtain the halogen-free flame retardant polyamide composition, wherein the temperature of a first area of the double-screw extruder is 180-200 ℃, the temperature of a second area of the double-screw extruder is 250-270 ℃, the temperature of a third area of the double-screw extruder is 260-280 ℃, the temperature of a fourth area of the double-screw extruder is 265-285 ℃, the temperature of a fifth area of the double-screw extruder is 265-285 ℃, the temperature of a sixth area of the double-screw extruder is 265-285 ℃, the temperature of a seventh area of the double-screw extruder is 260-280 ℃, and the rotating speed of a screw of the double-screw extruder is 300-500 r/min.
Table 1 amounts (parts by weight) of the components in the halogen-free flame retardant polyamide composition of examples 1 to 7
Table 2 amounts of the components (parts by weight) of the halogen-free flame retardant polyamide compositions of examples 8 to 10 and comparative examples 1 to 6
Performance testing
1. Test method
Performance testing was performed on the halogen-free flame retardant polyamide compositions prepared in examples 1 to 10 and comparative examples 1 to 6:
(1) Burning property test the halogen-free flame retardant polyamide compositions prepared in the above examples and comparative examples were tested according to UL94-2009 standard, the test bar thickness was 1.5mm;
(2) Melt flow Rate test the halogen-free flame retardant polyamide compositions prepared in the above examples and comparative examples were tested according to the standard ISO 1133-1-2022, with test conditions of 280℃per 2.16kg.
2. Test results
The results of the performance test of the halogen-free flame retardant polyamide compositions prepared in each of the examples and comparative examples are shown in Table 3.
Table 3 results of performance tests for examples 1 to 10 and comparative examples 1 to 6
As can be seen from Table 3, the halogen-free flame retardant polyamide composition prepared by the embodiments of the invention has a melt flow rate of 15-46 g/10min, and in this range, the halogen-free flame retardant polyamide composition has good processability, does not drip during combustion, has good flame retardant property, has a self-extinguishing time of not more than 3.3s, and has a self-extinguishing time of not more than 2.6s in most embodiments.
As can be seen from comparative examples 1 and 2, when the melting point of the zinc-containing compound selected is higher than 600 ℃, the halogen-free flame retardant polyamide composition prepared still has a molten drop phenomenon because ionization cannot occur and coordination with the polyamide resin and the flame retardant cannot be performed when the melting point of the added zinc-containing compound is above the flame temperature, thereby failing to exert an anti-dripping effect.
As can be seen from comparative example 3, when other metal compounds are selected instead of the zinc-containing compound, the halogen-free flame retardant polyamide composition produced still has a molten drop phenomenon even if the melting point is not more than 600 ℃, because the sodium element does not have a similar coordination ability, and it is impossible to prevent the dropping by the coordination.
As can be seen from comparative example 4, when polytetrafluoroethylene is selected instead of zinc-containing compound, the halogen-free flame retardant polyamide composition obtained has no melt dripping but has a melt flow rate of only 13g/10min, reduced flowability, shortened molding window during injection molding, and possibly occurrence of a gel shortage.
As can be seen from comparative example 5, when the zinc-containing compound is not added, the halogen-free flame retardant polyamide composition is produced which has a melt drop phenomenon and does not self-extinguish although the melt flow rate is high.
As can be seen from comparative example 6, when other halogen-free flame retardant agents are used instead of dialkylphosphinates, the halogen-free flame retardant polyamide composition obtained has a melt drop phenomenon.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (9)
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| PCT/CN2024/107013 WO2025050860A1 (en) | 2023-09-07 | 2024-07-23 | Halogen-free flame-retardant polyamide composition, and preparation method therefor and use thereof |
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| CN115449217A (en) * | 2022-08-31 | 2022-12-09 | 金发科技股份有限公司 | Halogen-free flame-retardant polyamide composition with good toughness and preparation and application thereof |
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| US20140288220A1 (en) * | 2013-03-25 | 2014-09-25 | E I Du Pont De Nemours And Company | Heat resistant polyamide compositions |
| DE102014001222A1 (en) * | 2014-01-29 | 2015-07-30 | Clariant lnternational Ltd | Halogen-free solid flame retardant mixture and its use |
| US9822239B2 (en) * | 2014-09-24 | 2017-11-21 | Shanghai Huihai Chemical Technology Co., Ltd. | Low-corrosion fire-resistant thermoplastic resin composition |
| CN111892811B (en) * | 2020-07-07 | 2022-12-27 | 浙江恒逸石化研究院有限公司 | Anti-dripping polyamide 6 and preparation method thereof |
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| CN115449217A (en) * | 2022-08-31 | 2022-12-09 | 金发科技股份有限公司 | Halogen-free flame-retardant polyamide composition with good toughness and preparation and application thereof |
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