WO2024125296A1 - 一种溴系阻燃聚酰胺复合材料及其制备方法和应用 - Google Patents

一种溴系阻燃聚酰胺复合材料及其制备方法和应用 Download PDF

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WO2024125296A1
WO2024125296A1 PCT/CN2023/134883 CN2023134883W WO2024125296A1 WO 2024125296 A1 WO2024125296 A1 WO 2024125296A1 CN 2023134883 W CN2023134883 W CN 2023134883W WO 2024125296 A1 WO2024125296 A1 WO 2024125296A1
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composite material
retardant
flame
brominated
brominated flame
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PCT/CN2023/134883
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French (fr)
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金雪峰
陈平绪
叶南飚
王丰
胡泽宇
张亚军
易新
吴长波
张志超
王冰
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金发科技股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant

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  • the invention relates to the technical field of engineering plastics, and in particular to a bromine-based flame-retardant polyamide composite material and a preparation method and application thereof.
  • bromine/antimony flame retardant system is a commonly used flame retardant system for polyamide materials due to its high flame retardant efficiency and low price.
  • brominated flame retardants such as brominated polystyrene
  • they are easily decomposed during high-temperature processing to produce low-molecular bromides with pungent odors, which remain in the product.
  • the small molecules will evaporate and emit an unpleasant odor, which seriously affects the consumer experience.
  • Odor control of brominated flame-retardant nylon has always been a difficult problem in the industry.
  • porous structure adsorbents such as alumina, activated carbon, diatomaceous earth, molecular sieves, etc.
  • this method can only achieve a short-term deodorization effect. Since the adsorbent still remains in the product, when the external environment changes, such as encountering high temperature and other conditions, small molecules will still be released, producing a strong odor.
  • the object of the present invention is to provide a bromine-based flame-retardant polyamide composite material with low odor and good demoulding performance.
  • Another object of the present invention is to provide a method for preparing the above-mentioned brominated flame-retardant polyamide composite material.
  • Another object of the present invention is to provide an application of the above-mentioned brominated flame retardant polyamide composite material
  • a brominated flame-retardant polyamide composite material comprises the following components in parts by weight:
  • the bromine/antimony flame retardant is a compound of brominated polystyrene and antimony trioxide, wherein the total chlorine content of the brominated polystyrene is less than 6000 ppm.
  • the present invention adds a specific amount of aromatic polyamide, which contains more benzene rings and has a certain barrier effect on odor, and can effectively reduce the emission of irritating odor; at the same time, aromatic polyamide also has a strong carbon-forming effect, which can reduce the amount of flame retardant (flame retardant will be partially decomposed during production, resulting in a strong odor), further reducing the odor of the material, while the material can still maintain good demoulding performance.
  • the weight percentage of the aromatic polyamide is 10-14 parts.
  • the aromatic polyamide of the present invention is selected from any one or more of PA MXD6, PA MXD8, PA MXD10 or PA MXD12; preferably, the aromatic polyamide is selected from any one or more of PA MXD6 or PA MXD10; more preferably, the aromatic polyamide is selected from PA MXD6.
  • the aliphatic polyamide resin of the present invention is derived from an aliphatic dibasic acid monomer and an aliphatic diamine monomer, or is derived from a lactam monomer, or is derived from an aminocarboxylic acid monomer, or is derived from two or more monomers of an aliphatic dibasic acid, an aliphatic diamine, a lactam, and an aminocarboxylic acid, and has an amide bond functional group; preferably, the aliphatic polyamide resin is selected from any one or more of PA6, PA56, or PA66.
  • the weight ratio of the brominated flame retardant to antimony trioxide in the bromine/antimony flame retardant is 2.5:1-9:1, more preferably 3:1-6:1.
  • the present invention has been found through research that the chlorine content of brominated polystyrene is one of the key factors causing the odor problem of polyamide materials. Materials using brominated polystyrene with high chlorine content have poor thermal stability and strong odor.
  • the present invention can effectively reduce the odor of polyamide materials by selecting a brominated polystyrene/antimony trioxide flame retardant system with a specific chlorine content.
  • the total chlorine content of the brominated polystyrene is 300ppm-1500ppm.
  • the total chlorine content is determined by ion chromatography IC.
  • Bromine chloride or a stronger Lewis acid such as aluminum chloride is used in the synthesis process of brominated polystyrene.
  • the total chlorine content of the final brominated polystyrene can be controlled by the number of water washings during the post-treatment process.
  • the antioxidant includes but is not limited to antioxidant 1098 (N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexanediamine); the lubricant includes but is not limited to stearyl stearate.
  • the present invention has no special requirements on the types and sources of antioxidants and lubricants, and technicians can select the types of antioxidants and lubricants to add according to actual needs.
  • the present invention also provides a method for preparing the brominated flame-retardant polyamide composite material, comprising the following steps:
  • each component is put into a mixer and mixed evenly to obtain a premix; the premix is put into a twin-screw extruder for melt mixing, and extruded into granules to prepare a brominated flame-retardant polyamide composite material; wherein the screw aspect ratio of the twin-screw extruder is 40 to 48:1, the barrel temperature is 220 to 270°C, and the screw speed is 200 to 450 rpm.
  • the present invention also provides the application of the brominated flame-retardant polyamide composite material in new energy vehicles, specifically, it can be used in connectors, battery brackets, electric control boxes, etc. of new energy vehicles.
  • the brominated flame-retardant polyamide composite material of the present invention can effectively solve the odor problem of the brominated flame-retardant polyamide material by adopting a flame-retardant system of brominated polystyrene with a specific chlorine content and antimony white, and adding a specific amount of aromatic polyamide, while ensuring the excellent demolding performance of the material (the material has a lower demolding force during the injection molding demolding process and can be demolded quickly and completely).
  • Aliphatic polyamide 1 PA66, grade PA66 EP-158, Zhejiang Huafeng Group;
  • Aliphatic polyamide 2 PA6, brand PA6 HY-2500A, Jiangsu Haiyang Chemical Fiber Co., Ltd.;
  • Aromatic polyamide 1 PA MXD6, grade AP-250, Yinggu Co., Ltd.
  • Aromatic polyamide 2 PA MXD10, Yinggu Co., Ltd.
  • Brominated polystyrene 2 CG-701, total chlorine content 5872ppm, Shandong Tianyi;
  • Glass fiber ECS301CL-3, Chongqing International Composite Materials Co., Ltd.
  • antioxidant IRGANOX 1098
  • lubricant stearyl stearate
  • Odor evaluation Injection molded into 100*100*1.5mm square plates, according to VDA_270 standard, use 20g sample, 1L sealed container baked at 80°C for 2h, 3 professionals perform odor rating, and calculate the average value (retain 1 decimal place). Odor evaluation The levels are: Level 1: no odor; Level 2: slight odor, but non-disturbing; Level 3: obvious odor, but non-disturbing; Level 4: disturbing odor; Level 5: strong disturbing odor; Level 6: unbearable odor; for the situation between the two levels, a half level will be added between the two levels, namely Level 1.5, Level 2.5, Level 3.5, Level 4.5, and Level 5.5.
  • Table 1 Distribution ratio of each group in Examples 1-11 (by weight) and related performance test results
  • the bromine-based flame-retardant polyamide composite material of the present invention is prepared by adopting a flame-retardant system in which brominated polystyrene having a total chlorine content of less than 6000 ppm and antimony white are compounded in a certain proportion, and a specific amount of aromatic polyamide is added at the same time.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

本发明公开一种溴系阻燃聚酰胺复合材料，包括组分：脂肪族聚酰胺36-52份；芳香族聚酰胺6-18份；玻璃纤维15-50份；溴/锑阻燃剂17-30份；所述溴/锑阻燃剂为溴化聚苯乙烯与三氧化二锑复配，其中，所述溴化聚苯乙烯的总氯含量小于6000ppm。本发明的溴系阻燃聚酰胺复合材料，通过采用特定氯含量的溴化聚苯乙烯与锑白复配的阻燃体系，同时加入特定量的芳香族聚酰胺，能够有效解决溴系阻燃聚酰胺材料的气味问题，且保证材料优异的脱模性能。

Description

一种溴系阻燃聚酰胺复合材料及其制备方法和应用 技术领域
本发明涉及工程塑料技术领域，具体涉及一种溴系阻燃聚酰胺复合材料及其制备方法和应用。
背景技术
阻燃聚酰胺材料具有良好的强度以及韧性，广泛应用于电子电气领域中。随着新能源汽车的电气化进程步伐加快，越来越多的汽车部件提出了阻燃要求。溴/锑阻燃体系因其阻燃效率高、价格低廉等因素，为聚酰胺材料较常采用的阻燃体系。然而，由于溴系阻燃剂(如溴化聚苯乙烯)的热稳定性较差，在高温加工中容易分解产生带刺激性气味的低分子溴化物，残留在制品中，而在后期使用过程中小分子物会挥发出来，散发出令人不悦的气味，严重影响了消费端使用感受。
溴系阻燃尼龙的气味控制一直是行业难题。目前解决塑胶气味最常用的方法一般是通过加入多孔结构物质吸附剂(如氧化铝、活性炭、硅藻土、分子筛等)来吸附产生的挥发性刺激性气味，但该方法只能起到短期除味效果，由于吸附物依然残留在制品中，当外界环境变化时，如遇到高温等条件，小分子物依然会释放出来，产生较大气味。
另外，汽车部件通常是模塑制件，而材料的脱模性能好坏直接影响到注塑效率及产品使用性能。脱模性能较差的材料，会导致产品制件变形、尺寸偏差、制品表面缺陷等问题。因此，要求在解决气味问题的同时，要保证材料的脱模性能。
发明内容
为了克服上述现有技术存在的不足，本发明的目的在于提供一种低气味且脱模性能好的溴系阻燃聚酰胺复合材料。
本发明的另一目的在于提供上述溴系阻燃聚酰胺复合材料的制备方法。
本发明的再一目的在于提供上述溴系阻燃聚酰胺复合材料的应用
本发明是通过以下技术方案实现的：
一种溴系阻燃聚酰胺复合材料，按重量份数计，包括以下组分：
所述溴/锑阻燃剂为溴化聚苯乙烯与三氧化二锑复配，其中，所述溴化聚苯乙烯的总氯含量小于6000ppm。
本发明加入特定量的芳香族聚酰胺，其含有较多的苯环，对气味有一定的阻隔作用，能够有效减少刺激性气味的散发；同时芳香族聚酰胺还具有较强的成碳作用，可以降低阻燃剂用量(阻燃剂在生产中会有部分分解，导致气味大)，进一步降低材料的气味，同时材料仍能保持较好的脱模性能。优选的，所述芳香族聚酰胺的重量份数为10-14份。
本发明所述芳香族聚酰胺选自PA MXD6、PA MXD8、PA MXD10或PA MXD12中的任意一种或几种；优选的，所述芳香族聚酰胺选自PA MXD6或PA MXD10中的任意一种或几种；更优选的，所述芳香族聚酰胺选自PA MXD6。
本发明所述脂肪族聚酰胺树脂衍生自脂肪族二元酸单体和脂肪族二元胺单体，或者衍生自内酰胺单体，或者衍生自氨基羧酸单体，或者衍生自脂肪族二元酸、脂肪族二元胺、内酰胺、氨基羧酸中的两种或两种以上单体，具有酰胺键的官能团；优选的，所述脂肪族聚酰胺树脂选自PA6、PA56或PA66中的任意一种或几种。
优选的，所述溴/锑阻燃剂中溴系阻燃剂与三氧化二锑的重量比例为2.5:1-9:1，更优选为3:1-6:1。
本发明经研究发现，溴化聚苯乙烯的氯含量是导致聚酰胺材料的气味问题的关键因素之一。使用高氯含量溴化聚苯乙烯的材料热稳定性差，气味重，本发明通过选用特定氯含量的溴化聚苯乙烯/三氧化二锑阻燃体系，可以有效减小聚酰胺材料的气味。优选的，所述溴化聚苯乙烯的总氯含量为300ppm-1500ppm。所述总氯含量通过离子色谱IC测定。
溴化聚苯乙烯在合成过程中会使用到氯化溴或者较强的路易斯酸如氯化铝，通过在后处理过程中的水洗次数，可以控制最终溴化聚苯乙烯的总氯含量。
根据材料性能需求，所述的溴系阻燃聚酰胺复合材料，按重量份数计，还包括0.5-1.5份助剂。所述助剂选自抗氧剂或润滑剂中的任意一种或几种。
所述抗氧剂包括但不限于抗氧剂1098(N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺)；所述润滑剂包括但不限于硬脂酸硬脂醇酯。
本发明对抗氧剂和润滑剂的种类和来源没有特别要求，技术人员可以根据实际情况需求选择抗氧剂和润滑剂种类添加。
本发明还提供上述溴系阻燃聚酰胺复合材料的制备方法，包括以下步骤：
按照配比，将各组分投入混合机，混合均匀后得到预混物；将预混物投入双螺杆挤出机中进行熔融混合，并挤出造粒，制备得到溴系阻燃聚酰胺复合材料；其中，双螺杆挤出机的螺杆长径比为40～48:1，螺筒温度为220～270℃，螺杆转速为200～450rpm。
本发明还提供上述溴系阻燃聚酰胺复合材料在新能源汽车的应用。具体的，可用于新能源汽车连接器、电池支架、电控盒等。
本发明具有如下有益效果：
本发明的溴系阻燃聚酰胺复合材料，通过采用特定氯含量的溴化聚苯乙烯与锑白复配的阻燃体系，同时加入特定量的芳香族聚酰胺，能够有效解决溴系阻燃聚酰胺材料的气味问题，且保证材料优异的脱模性能(材料在注塑脱模过程中具有较低的脱模力，能够快速完整脱模)。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
对本发明实施例及对比例所用的原材料做如下说明，但不限于这些材料：
脂肪族聚酰胺1：PA66，牌号PA66 EP-158，浙江华峰集团；
脂肪族聚酰胺2：PA6，牌号PA6 HY-2500A，江苏海阳化纤有限公司；
芳香族聚酰胺1：PA MXD6，牌号AP-250，盈固有限公司；
芳香族聚酰胺2：PA MXD10，盈固有限公司；
溴化聚苯乙烯1：SAYTEX 5010，总氯含量799ppm，美国雅宝公司；
溴化聚苯乙烯2：CG-701，总氯含量5872ppm，山东天一；
溴化聚苯乙烯3：XZ-6700，总氯含量10153ppm，山东兄弟；
三氧化二锑：闪星锑业；
玻璃纤维：ECS301CL-3，重庆国际复合材料股份有限公司；
助剂：抗氧剂(IRGANOX 1098)、润滑剂(硬脂酸硬脂醇酯)，市售，实施例和对比例中采用相同助剂。
实施例和对比例的溴系阻燃聚酰胺复合材料的制备方法：
按照配比，将各组分投入混合机，混合均匀后得到预混物；将预混物投入双螺杆挤出机中进行熔融混合，并挤出造粒，制备得到溴系阻燃聚酰胺复合材料；其中，双螺杆挤出机的螺杆长径比为40～48:1，螺筒温度为220～270℃，螺杆转速为200～450rpm。
相关性能测试方法：
(1)阻燃性能：通过注射成型制成125×13×1.6mm方板，根据UL 94-2021标准进行测试。
(2)气味评价：注塑成100*100*1.5mm方板，按照VDA_270标准，采用20g样品，1L密闭容器80℃烘烤2h，3名专业人员进行气味评级，计算平均值(保留1位小数)。气味评价 等级为：1级：无气味；2级：有轻微气味，但无干扰性；3级：有明显气味，但无干扰性；4级：干扰性气味；5级：强烈干扰性气味；6级：难以忍受的气味；介于两个等级之间的情况，则在两个等级中再补充一个半数等级，即1.5级、2.5级、3.5级、4.5级、5.5级。
(3)脱模力：注塑机400T，注塑温度(下料口到射嘴)260℃、270℃、275℃、280℃，速度60％，压力50Mpa，测试脱模过程中制件所需的脱模力。脱模力越小，材料的脱模性能越好。
表1：实施例1-11各组分配比(按重量份数计)及相关性能测试结果
接表1：
表2：对比例1-6各组分配比(按重量份数计)及相关性能测试结果

由上述实施例和对比例看出，本发明的溴系阻燃聚酰胺复合材料，通过采用总氯含量小于6000ppm的溴化聚苯乙烯与锑白以一定比例复配的阻燃体系，同时加入特定量的芳香族聚酰胺，制备得到阻燃聚酰胺材料，其阻燃性达到UL-94标准1.6mmV-0等级，同时能够有效解决溴系阻燃聚酰胺材料的气味问题(气味等级低于4级，不产生干扰性气味)，且保证材料优异的脱模性能(材料在注塑脱模过程中的脱模力≤1054N，能够快速完整脱模)。

Claims (9)

  1. 一种溴系阻燃聚酰胺复合材料，其特征在于，按重量份数计，包括以下组分：
    所述溴/锑阻燃剂为溴化聚苯乙烯与三氧化二锑复配，其中，所述溴化聚苯乙烯的总氯含量小于6000ppm。
  2. 根据权利要求1所述的溴系阻燃聚酰胺复合材料，其特征在于，所述芳香族聚酰胺选自PA MXD6、PA MXD8、PA MXD10或PA MXD12中的任意一种或几种；优选的，所述芳香族聚酰胺选自PA MXD6或PA MXD10中的任意一种或几种；更优选的，所述芳香族聚酰胺选自PA MXD6。
  3. 根据权利要求1所述的溴系阻燃聚酰胺复合材料，其特征在于，所述芳香族聚酰胺的重量份数为10-14份。
  4. 根据权利要求1所述的溴系阻燃聚酰胺复合材料，其特征在于，所述脂肪族聚酰胺树脂选自PA6、PA56或PA66中的任意一种或几种。
  5. 根据权利要求1所述的溴系阻燃聚酰胺复合材料，其特征在于，所述溴/锑阻燃剂中溴系阻燃剂与三氧化二锑的重量比例为2.5:1-9:1，优选为3:1-6:1。
  6. 根据权利要求5所述的溴系阻燃聚酰胺复合材料，其特征在于，所述溴化聚苯乙烯的总氯含量为300ppm-1500ppm。
  7. 根据权利要求1所述的溴系阻燃聚酰胺复合材料，其特征在于，按重量份数计，还包括0.5-1.5份助剂；所述助剂选自抗氧剂或润滑剂中的任意一种或几种。
  8. 根据权利要求1-7任一项所述的溴系阻燃聚酰胺复合材料的制备方法，其特征在于，包括以下步骤：
    按照配比，将各组分投入混合机，混合均匀后得到预混物；将预混物投入双螺杆挤出机中进行熔融混合，并挤出造粒，制备得到溴系阻燃聚酰胺复合材料；其中，双螺杆挤出机的螺杆长径比为40～48:1，螺筒温度为220～270℃，螺杆转速为200～450rpm。
  9. 根据权利要求1-7任一项所述的溴系阻燃聚酰胺复合材料在新能源汽车领域的应用。
PCT/CN2023/134883 2022-12-15 2023-11-29 一种溴系阻燃聚酰胺复合材料及其制备方法和应用 WO2024125296A1 (zh)

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