CN103709708A - 高流动性的玻纤增强无卤阻燃pc材料及其制备方法 - Google Patents

高流动性的玻纤增强无卤阻燃pc材料及其制备方法 Download PDF

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CN103709708A
CN103709708A CN201310703410.8A CN201310703410A CN103709708A CN 103709708 A CN103709708 A CN 103709708A CN 201310703410 A CN201310703410 A CN 201310703410A CN 103709708 A CN103709708 A CN 103709708A
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free flame
halogen
flame retardant
parts
polycarbonate
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朱明源
陈晓东
杨涛
孟成铭
王尹杰
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Shanghai Rizhisheng New Technology Development Co Ltd
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Abstract

本发明涉及高流动性的玻纤增强无卤阻燃PC材料及其制备方法，按照重量份配比如下：聚碳酸酯PC50-90份，玻璃纤维10-30份，流动改性剂0-10份，相容剂0-10份，无卤阻燃剂0.1-1份，阻燃协效剂0-2份，润滑剂0.1-1份，抗氧剂0.1-1份。本发明与现有技术相比，其特点在于：通过添加流动改性剂以及采用合适的相容剂，克服同类产品流动性不佳的缺点，大幅提高了材料流动性；同时优选复配一种阻燃效率极高的磺酸盐(酯)类阻燃剂，配合高效阻燃协效剂，可显著降低阻燃剂用量，进而降低材料成本且材料机械性能优异，阻燃性UL94 V-0级(1.6mm)；该材料完全满足注塑成型薄壁电子电器设备外壳的材质要求。

Description

高流动性的玻纤增强无卤阻燃PC材料及其制备方法
技术领域
本发明涉及玻纤增强聚碳酸酯改性技术领域，尤其涉及一种低成本高流动性的玻纤增强无卤阻燃PC材料及其制备方法。这种玻纤增强无卤阻燃PC材料可以满足薄壁、长流程注塑要求。
背景技术
聚碳酸酯(PC)是一种综合性能优良的工程塑料，由于其具有优异的耐候性能、高抗冲击性能、良好的电绝缘性，因而广泛应用于电子电气、汽车、机械工业等领域。PC阻燃等级为UL94 V-2，但可燃，燃烧时滴下热熔体，引起附近的材料着火，所以难以满足某些领域对阻燃性能的要求，因此需对PC进行阻燃改性。
卤系阻燃剂由于环境污染问题，越来越多的高效含卤阻燃剂被禁用，尤其是在西欧、日本、北美等发达国家或地区；有机磷酸酯是一类被广泛应用的无卤阻燃剂，但其本身分解温度较低，虽然添加量为5％-15％时对PC有较好的阻燃作用，但是单独添加时会对机械性能损害很大；有机硅化合物是一类高效、无毒、低烟、环境友好性的阻燃剂，但其价格昂贵，很难普及，并且单独使用时阻燃作用不够，需与其它阻燃剂复合使用；磺酸盐类阻燃剂是近几年发展起来的一类适用于PC阻燃的高效阻燃剂，其阻燃效率高，添加量少，几乎不损害材料机械性能。
未经改性的玻纤增强中粘度聚碳酸酯原料在加工流动性方面仍有不足，限制了其在薄壁、长流程注塑产品领域中的应用。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种低成本高流动性的玻纤增强无卤阻燃PC材料及其制备方法，该种无卤阻燃PC材料成本低，机械性能优异，加工流动性强，阻燃性达UL94V-0级(1.6mm)。
本发明的目的可以通过以下技术方案来实现：
高流动性的玻纤增强无卤阻燃PC材料，采用以下组分及重量份含量的原料制备得到：
聚碳酸酯50-90、玻璃纤维10-30、流动改性剂0-10、相容剂0-10、无卤阻燃剂0.1-1、阻燃协效剂0-2、润滑剂0.1-1、抗氧剂0.1-1，上述组分不同时为0。
作为优选的实施方式，聚碳酸酯为相对密度为1.2g/cm3，熔融温度为220-230℃的中粘度聚碳酸酯。
作为优选的实施方式，玻璃纤维为经表面处理的无碱长玻璃纤维。
作为优选的实施方式，流动改性剂的含量优选3-5重量份，采用一种超低分子量苯乙烯类功能聚合物。
作为更加优选的实施方式，此超低分子量苯乙烯类功能聚合物是一种由苯乙烯、丙烯腈单体聚合而成的无规共聚物。
作为优选的实施方式，相容剂的含量优选3-5重量份，采用苯乙烯-马来酸酐共聚物。
作为优选的实施方式，无卤阻燃剂选自无机或有机磺酸盐或磺酸酯的一种或几种。
作为更加优选的实施方式，无卤阻燃剂选自全氟丁基磺酸钾，二苯基砜磺酸盐或2，4，5-三氯苯磺酸钠中的任意一种或几种。
作为优选的实施方式，阻燃协效剂为片状的有机硅不规则固体，选自苯基硅树脂，苯甲基有机硅中间体或聚甲基苯基硅氧烷中的任意一种或几种。
作为优选的实施方式，润滑剂选自低分子量聚乙烯、硬脂酸酰胺、甲撑双硬脂酸酰胺、N，N-乙撑双硬脂酸酰胺EBS或季戊四醇硬脂酸酯(PETS)中的任意一种或几种。
作为优选的实施方式，抗氧剂选自抗氧剂168、抗氧剂1010或抗氧剂245中的任意一种或几种。
高流动性的玻纤增强无卤阻燃PC材料的制备方法采用以下步骤：
按照以下组分和重量份准备原料：聚碳酸酯50-90、玻璃纤维10-30、流动改性剂0-10、相容剂0-10、无卤阻燃剂0.1-1、阻燃协效剂0-2、润滑剂0.1-1、抗氧剂0.1-1；
将上述聚碳酸酯、流动改性剂、相容剂、无卤阻燃剂、阻燃协效剂、润滑剂以及抗氧剂混合均匀后送入双螺杆挤出机中，然后再与玻璃纤维共混，控制双螺杆挤出机各段螺杆温度为240-280℃，螺杆转速在200-500转/分钟，经混炼、挤出、拉条、冷却、切粒后获得成品。
与现有技术相比，本发明采用的配方与工艺制备的玻纤增强无卤阻燃PC材料阻燃体系阻燃效率高，添加量小，材料成本低且机械性能损失小，阻燃性达UL94 V-0级(1.6mm)；同时本专利采用的流动改性剂可显著降低材料的熔体粘度，因此该材料充模流动性好，易注塑成型，是一种更适合于注塑成型薄壁、长流程产品的玻纤增强改性聚碳酸酯材料。
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。
实施例1
按如下配方配制预混合料：聚碳酸酯90份、磺酸盐类无卤阻燃剂0.5份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例2
按如下配方配制预混合料：聚碳酸酯90份、磺酸盐类无卤阻燃剂0.2份、有机硅协效阻燃剂0.5份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例3
按如下配方配制预混合料：聚碳酸酯84份、流动改性剂3份、相容剂3份、磺酸盐类无卤阻燃剂0.5份、有机硅协效阻燃剂0.5份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例4
按如下配方配制预混合料：聚碳酸酯80份、流动改性剂5份、相容剂5份、磺酸盐类无卤阻燃剂0.8份、有机硅协效阻燃剂1份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例5
按如下配方配制预混合料：聚碳酸酯75份、流动改性剂10份、相容剂5份、磺酸盐类无卤阻燃剂1份、有机硅协效阻燃剂2份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例6
按如下配方配制预混合料：聚碳酸酯70份、流动改性剂5份、相容剂5份、磺酸盐类无卤阻燃剂0.8份、有机硅协效阻燃剂1份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与20份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
实施例7
按如下配方配制预混合料：聚碳酸酯60份、流动改性剂5份、相容剂5份、磺酸盐类无卤阻燃剂0.8份、有机硅协效阻燃剂1份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与30份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
比较例1
按如下配方配制预混合料：聚碳酸酯90份、FR-2025(市售常用磺酸盐类阻燃剂)0.8份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
比较例2
按如下配方配制预混合料：聚碳酸酯80份、磷酸酯类阻燃剂10份、润滑剂0.5份、抗氧剂0.5份。将混合好的预混合料置于双螺杆挤出机中与10份玻璃纤维共混，经熔融挤出造粒，得到的粒子在100℃干燥2小时，即得成品。其工艺为：双螺杆挤出机各段螺杆温度控制在250-275℃之间，螺杆转速为300转/分钟。
将实施例1-7制备得到的复合物及比较例1、2按标准尺寸注塑成测试用的标准样条，进行性能测试，性能测试标准见表1，性能测试结果见表2。
表1
物理性能 测试方法
拉伸强度 ISO 527-2
弯曲强度 ISO 178
弯曲模量 ISO 178
缺口冲击强度 ISO 179-1
融指 ISO 1133
阻燃性 UL 94
表2
通过对比可以看到本发明低成本高流动性的玻纤增强无卤阻燃PC材料的有益效果：
对比实施例1与比较例1，可看出本发明优选的磺酸盐阻燃剂比市售常用的阻燃剂更高效，添加量更小；同时对比实施例1与实施例2，可看出本发明添加的有机硅协效阻燃剂可有效降低主阻燃剂用量，阻燃体系更高效，进而可降低材料成本；而对比实施例1与比较例2，可看出本发明所采用的磺酸盐类阻燃剂对材料机械性能的损害比通常采用的磷酸酯类阻燃剂要小得多。
对比实施例3-5与实施例1可看出本发明采用的流动改性剂配合适量的相容剂可有效提高改性聚碳酸酯材料的流动性，本发明该玻纤增强无卤阻燃PC材料加工流动性优异，是一种更适合于注塑成型薄壁、长流程产品的玻纤增强改性聚碳酸酯材料。

Claims (10)

1.高流动性的玻纤增强无卤阻燃PC材料，其特征在于，该材料采用以下组分及重量份含量的原料制备得到：
聚碳酸酯50-90、玻璃纤维10-30、流动改性剂0-10、相容剂0-10、无卤阻燃剂0.1-1、阻燃协效剂0-2、润滑剂0.1-1、抗氧剂0.1-1，上述组分不同时为0。
2.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的聚碳酸酯为相对密度为1.2g/cm3，熔融温度为220-230℃的中粘度聚碳酸酯。
3.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的玻璃纤维为经表面处理的无碱长玻璃纤维。
4.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的流动改性剂的含量优选3-5重量份，采用一种超低分子量苯乙烯类功能聚合物，包括苯乙烯与丙烯腈聚合而成的无规共聚物。
5.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的相容剂的含量优选3-5重量份，采用苯乙烯-马来酸酐共聚物。
6.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的无卤阻燃剂选自无机或有机磺酸盐或磺酸酯，选自全氟丁基磺酸钾，二苯基砜磺酸盐或2，4，5-三氯苯磺酸钠中的任意一种或几种。
7.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的阻燃协效剂为片状的有机硅不规则固体，选自苯基硅树脂，苯甲基有机硅中间体或聚甲基苯基硅氧烷中的任意一种或几种。
8.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的润滑剂选自低分子量聚乙烯、硬脂酸酰胺、甲撑双硬脂酸酰胺、N，N-乙撑双硬脂酸酰胺EBS或季戊四醇硬脂酸酯(PETS)中的任意一种或几种。
9.根据权利要求1所述的高流动性的玻纤增强无卤阻燃PC材料，其特征在于，所述的抗氧剂选自抗氧剂168、抗氧剂1010或抗氧剂245中的任意一种或几种。
10.如权利要求1-9中任一项所述的高流动性的玻纤增强无卤阻燃PC材料的制备方法，其特征在于，该方法采用以下步骤：
按照以下组分和重量份准备原料：聚碳酸酯50-90、玻璃纤维10-30、流动改性剂0-10、相容剂0-10、无卤阻燃剂0.1-1、阻燃协效剂0-2、润滑剂0.1-1、抗氧剂0.1-1；
将上述聚碳酸酯、流动改性剂、相容剂、无卤阻燃剂、阻燃协效剂、润滑剂以及抗氧剂混合均匀后送入双螺杆挤出机中，然后再与玻璃纤维共混，控制双螺杆挤出机各段螺杆温度为240-280℃，螺杆转速在200-500转/分钟，经混炼、挤出、拉条、冷却、切粒后获得成品。
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Application publication date: 20140409