CN102964688B - 一种高cti值、高gwit值环保阻燃玻纤增强pp/pa11合金材料及其制备方法 - Google Patents

一种高cti值、高gwit值环保阻燃玻纤增强pp/pa11合金材料及其制备方法 Download PDF

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CN102964688B
CN102964688B CN201210512087.1A CN201210512087A CN102964688B CN 102964688 B CN102964688 B CN 102964688B CN 201210512087 A CN201210512087 A CN 201210512087A CN 102964688 B CN102964688 B CN 102964688B
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alloy material
glass fibre
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oxidation inhibitor
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CN102964688A (zh
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郭建鹏
孟诚铭
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Shanghai Rizhisheng New Technology Development Co Ltd
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Abstract

本发明涉及一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料，由以下重量百分比含量的原料制成：PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％。本发明还提供该合金材料的制备方法。本发明优点在于：本发明的高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料灼热丝温度（GWIT）较高，漏电起痕指数（CTI）较高，环保，综合性能均衡，可广泛用于低压电子电容器外壳，负载断路开关，碳刷支架，塑壳断路器。

Description

一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料及其制备方法
技术领域
本发明涉及合金材料领域，具体地说，是一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料及其制备方法。
背景技术
尼龙（Nylon），中文名聚酰胺，英文名称Polyamide（简称PA），是分子主链上含有重复酰胺基团—[NHCO]—的热塑性树脂总称。其命名由合成单体具体的碳原子数而定，如：尼龙-6、66、1010、610.它结晶度高、熔点明显；表面硬度大、耐磨耗、摩擦系数小、有自润滑性和消音性。低温性能良好，有一定的耐热性（可以在100度以下使用）。无毒、无臭、不霉烂，有自熄性、耐候性好，但染色性差。尼龙PA11的密度 为1.04g/cm3,熔点185℃，吸水率0.1-0.4℅，拉伸强度47-58MPa。具有吸水率低、耐油性好、耐低温、易加工等优点。
聚丙烯分子式：(C3H6)n，是由丙烯聚合而制得的一种热塑性树脂。按甲基排列位置分为等规聚丙烯（isotaetic polyprolene）、无规聚丙烯（atactic polypropylene）和间规聚丙烯（syndiotatic polypropylene）三种。无毒、无味，密度小，强度、刚度、硬度耐热性均优于低压聚乙烯，可在100℃左右使用。具有良好的电性能和高频绝缘性不受湿度影响。适于制作一般机械零件、耐腐蚀零件和绝缘零件。常见的酸、碱等有机溶剂对它几乎不起作用，可用于食具。
PP/PA11合金材料综合了两种材料的优点。21世纪电子电气通讯家电机电设备向高性能微型化发展，对阻燃PP/PA11合金材料的要求越来越高，同时，随着人类对环保的认识，绿色环保产品受到普遍关注。因此，阻燃PP/PA11合金材料发展方向是：高性能功能化阻燃PP/PA11合金材料成为主流；绿色环保型阻燃PP/PA11合金材料的品种与需求越来越多；阻燃PP/PA11合金材料的生产向多品种系列化方向发展；阻燃剂的使用多元化，复合型发展。一些传统的方式为(GF+十溴二苯乙烷+三氧化二锑)复配体系，(GF+溴化聚苯乙烯+三氧化二锑)复配体系，但是这些复配体系的CTI值（漏电起痕指数）和GWIT值（灼热丝温度）都不高，不适用于高要求的用电环境。
中国专利文献CN1789336A公开了一种高强阻燃聚合物PA/PP合金，原料配方(重量)为：主料:(1).尼龙6(PA6)50～60份;(2).聚丙烯(PP)25～35份;辅料:(1).复合阻燃剂-聚磷酸胺4～6份、三聚氰胺1～3份和氨基硅烷1份;(2).相容剂-磺化聚苯乙烯锌8～12份;(3).抗氧剂-抗氧剂1010/168,0.2/0.2份，可广泛应用于制造高强、阻燃以及各种厚度的电气零部件及汽车结构件。中国专利文献CN 102775782A公开了一种阻燃玻纤增强PA66/PP合金组合物及其制备方法，所述组合物包括以下重量百分比含量的各组分：PA116 20-41％，PP 20-41％，相容剂0-10%，复配阻燃母粒0-15％，玻璃纤维20-40%，抗氧剂0.1-1％，润滑分散剂0.1-1％。但是关于一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料及其制备方法目前还未见报道。
发明内容
本发明的目的是针对现有技术中的不足，提供一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料。
本发明的再一的目的是，提供一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料的制备方法。
为实现上述目的，本发明采取的技术方案是：一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料，由以下重量百分比含量的原料制成：PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％。
所述的PA11的特性粘度为2.8dl/g。
所述的复配型阻燃剂由三种组分混合而成，其质量百分比为BPS 50%，次磷酸镁 25%，滑石粉 25%。
所述的玻璃纤维为无碱玻璃纤维，其表面经硅烷偶联剂处理。
所述的抗氧剂为受阻酚类抗氧剂。
所述的抗氧剂为抗氧剂1330。
所述的相容剂为马来酸酐接枝PP。
所述的氧化物为氧化铁。
为实现上述第二个目的，本发明采取的技术方案是：一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料的制备方法，包括以下步骤：按重量配比称取原料：PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ。
本发明优点在于：
本发明的高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料灼热丝温度（GWIT）较高，漏电起痕指数（CTI）较高，环保，综合性能均衡，可广泛用于低压电子电容器外壳，负载断路开关，碳刷支架，塑壳断路器。
具体实施方式
下面结合实施例对本发明提供的具体实施方式作详细说明。
本发明提供一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料，由以下重量配比的原料制成：PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％。
所述的PP为市售聚丙烯。所述的PA11为市售聚酰胺6，其特性粘度为2.8dl/g。所述的复配型阻燃剂，由三种组分混合而成，其质量百分比为溴化聚苯乙烯（BPS）：50%，次磷酸镁：25%，滑石粉：25%。所述的玻璃纤维为无碱玻璃纤维，将玻璃纤维加入硅烷偶联剂中，使其表面经硅烷偶联剂处理。所述的相容剂为市售马来酸酐接枝PP。所述的抗氧剂为受阻酚类抗氧剂，优选的抗氧剂为抗氧剂1330。所述的氧化物为氧化铁。
制备方法包括以下步骤：按重量配比称取原料： PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ。
对比例1
按重量配比称取原料：PP 25％，PA11 38.6%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 20%，抗氧剂0.4％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
表1 双螺杆挤出机参数
对比例2
按重量配比称取原料：PP 25％，PA11 25.1%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
对比例3
按重量配比称取原料：PP 25％，PA11 25.1%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
对比例4
按重量配比称取原料：PP 25％，PA11 25.1%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
对比例5
按重量配比称取原料：PP 25％，PA11 25.1%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
对比例6
按重量配比称取原料：PP 25％，PA11 25.1%，阻燃剂（十溴二苯乙烷）12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
对比例7
按重量配比称取原料：PP 25％，PA11 23%，阻燃剂（溴化聚苯乙烯）12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 5％，抗氧剂0.4％，氧化物0.6％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
实施例1
按重量配比称取原料：PP 25％，PA11 25.1%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 3％，抗氧剂0.4％，氧化物0.5％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
实施例2
按重量配比称取原料：PP 25％，PA11 23%，复配型阻燃剂12％，三氧化二锑 4％，玻璃纤维 30%，相容剂 5％，抗氧剂0.4％，氧化物0.6％；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ，双螺杆挤出机参数参照表1。
需要说明的是，对比例1-5和实施例1-2所述的复配型阻燃剂，由三种组分混合而成，其质量百分比为溴化聚苯乙烯（BPS）：50%，次磷酸镁：25%，滑石粉：25%。所述的玻璃纤维为无碱玻璃纤维，其表面经硅烷偶联剂处理。所述的相容剂为市售马来酸酐接枝PP。
表2对比例1-7及实施例1-2的原材料配方（wt%）
实施例3 性能测试
根据对比例1-7及实施例1-2制得的样品，进行性能测试对比，采用ASTM标准，测试性能对比如下表所示。
表3 对比例1-7和实施例1-2的样品性能测试对比
   由上表可以看出，本发明采用新型阻燃复配体系，和传统的阻燃体系相比，在阻燃剂百分含量相同的情况下，新型复配体系能使材料的灼热丝温度提高50到100℃，能够通过850℃灼热丝。随着新型复配型阻燃剂含量的提高，产品的灼热丝温度也逐渐提高。同时，玻璃纤维的加入也使材料的灼热丝明显的提高，加入相容剂改善了材料的冲击性能，抗氧剂为一种受阻酚类抗氧剂提高了组合物在加工过程的抗氧化性能和使用过程中的抗老化性能，采用氧化铁作为提高CTI助剂，显著提高漏电起痕指数，提高材料加工流动性，降低摩擦系数，提高滑爽性，在特定的加工条件下采用分散性较好，停留时间短，剪切稍弱的组合，防止阻燃剂分解，从而保证了材料的质量稳定。
    本发明的高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料灼热丝温度（GWIT）较高，漏电起痕指数（CTI）较高，环保，综合性能均衡，可广泛用于低压电子电容器外壳，负载断路开关，碳刷支架，塑壳断路器。
实施例4
按重量配比称取原料：PP 23％，PA11 41%，复配型阻燃剂6％，三氧化二锑3％，玻璃纤维 20%，市售马来酸酐接枝PP 5％，抗氧剂(1330) 1％，氧化铁1％；放入高混机中混合2分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在220℃，螺杆转数在30HZ。
实施例5
按重量配比称取原料：PP 41％，PA11 22%，复配型阻燃剂6％，三氧化二锑 8.8％，玻璃纤维20%，市售马来酸酐接枝PP 2％，抗氧剂(1330) 0.1％，氧化铁0.1％；放入高混机中混合5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在220℃，螺杆转数在40HZ。
实施例6
按重量配比称取原料：PP 23％，PA11 22%，复配型阻燃剂20％，三氧化二锑4％，玻璃纤维20%，市售马来酸酐接枝PP 10％，抗氧剂（1330）0.5％，氧化铁0.5％；放入高混机中混合3分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在210℃，螺杆转数在35HZ。
实施例7
按重量配比称取原料：PP 25％，PA11 25%，复配型阻燃剂10％，三氧化二锑15％，玻璃纤维20%，市售马来酸酐接枝PP 4％，抗氧剂（1330）0.4％，氧化铁0.6％；放入高混机中混合4分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200℃，螺杆转数在38HZ。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员，在不脱离本发明方法的前提下，还可以做出若干改进和补充，这些改进和补充也应视为本发明的保护范围。

Claims (2)

1.一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料，其特征在于，由以下重量百分比含量的原料制成：PP 23-41％，PA11 22-41%，复配型阻燃剂6-20％，三氧化二锑 3-15％，玻璃纤维 20-30%，相容剂 2-10％，抗氧剂0.1-1％，氧化物0.1-1％；所述的PA11的特性粘度为2.8dl/g；所述的复配型阻燃剂由三种组分混合而成，其质量百分比为BPS 50%，次磷酸镁 25%，滑石粉 25%；所述的玻璃纤维为无碱玻璃纤维，其表面经硅烷偶联剂处理；所述的抗氧剂为抗氧剂1330；所述的相容剂为马来酸酐接枝PP；所述的氧化物为氧化铁。
2.根据权利要求1所述的一种高CTI值、高GWIT值环保阻燃玻纤增强PP/PA11合金材料的制备方法，其特征在于，包括以下步骤：按重量配比称取原料；放入高混机中混合2-5分钟，出料，然后用双螺杆挤出机挤出造粒，加工温度在200-220℃，螺杆转数在30-40HZ。
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