CN101875761B - 一种阻燃增强pet材料及其制备方法 - Google Patents

一种阻燃增强pet材料及其制备方法 Download PDF

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CN101875761B
CN101875761B CN2010102278437A CN201010227843A CN101875761B CN 101875761 B CN101875761 B CN 101875761B CN 2010102278437 A CN2010102278437 A CN 2010102278437A CN 201010227843 A CN201010227843 A CN 201010227843A CN 101875761 B CN101875761 B CN 101875761B
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徐东
徐永
李超
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Polymer Science Shenzhen New Materials Co Ltd
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Abstract

本发明公开了一种阻燃增强PET材料及其制备方法。本发明的阻燃增强PET材料，按重量百分比由以下组分组成：PET树脂50.0-55.0％；十溴二苯乙烷4.0-6.0％；磷氮阻燃剂2.0-6.0％；无机阻燃剂1.5-2.0％。复合成核剂1.0-2.0％；增韧剂2.0-4.0％；玻璃纤维30.0-35.0％；润滑剂0.5-1.0％；抗氧剂0.3-0.5％，制备工艺为双螺杆熔融挤出造粒。本发明通过复配的阻燃剂，利用十溴二苯乙烷高效阻燃特性及溴系、磷系和氮系阻燃剂的不同阻燃机理共同作用，可制得灼热丝850℃不起燃，各项物理机械性能优异的阻燃增强PET材料。

Description

一种阻燃增强PET材料及其制备方法
[技术领域]
本发明属于工程塑料改性技术领域，尤其涉及一种阻燃增强PET材料及其制备方法。
[背景技术]
聚对苯二甲酸乙二醇酯(PET)具有价格低廉，具有优良的耐磨性、耐热性、耐化学药品性、电绝缘性和力学强度高等特性，因此，20世纪60年代便开始了作为工程塑料的应用开发。目前PET工程塑料已应用于汽车、电机、电子、家用电器及机械等行业。
电子电器中的元件在过载、短路等情况下会造成局部过热并可能引起燃烧，因此，电子电器产品中的部件的着火危险必须降低到一定程度。2010年，IEC 60335-1标准要求非金属材料灼热丝起燃温度(Glow-wire Ignitability Test，GWIT)从750℃提高到850℃以上。目前，少数阻燃尼龙能达到这一要求，但是尼龙的价格很高，阻燃尼龙需添加的阻燃剂也较多，如果用PET能达到这些要求，在成本上会更具优势。
[发明内容]
本发明要解决的技术问题是提供一种阻燃性能优良，物理机械性能较好的阻燃增强PET材料及其制备方法。
为了解决上述技术问题，本发明采用的技术方案是，一种阻燃增强PET材料，按重量百分比由以下组分组成：
PET树脂         50-55％；
十溴二苯乙烷    4.0-6.0％；
磷氮阻燃剂      2.0-6.0％；
无机阻燃剂    1.5-2.0％；
复合成核剂    1.0-2.0％；
增韧剂        2.0-4.0％；
玻璃纤维      30-35％；
润滑剂        0.5-1.0％；
抗氧剂        0.3-0.5％。
所述的十溴二苯乙烷的相对分子量大于900，溴含量大于80％。
所述磷氮阻燃剂为磷酸盐与氮系阻燃剂按重量百分比1-2∶1复配、次膦酸盐类或三聚氰胺磷酸盐类，且磷氮阻燃剂的热分解温度大于260℃。
所述无机阻燃剂为三氧化二锑、锑酸钠或五氧化二锑。
所述的PET树脂为聚对苯二甲酸乙二醇酯，其相对密度为1.35-1.38，熔点为255-260℃，粘度为0.6-0.8Pa·S。
所述的复合成核剂为长链羧酸盐与滑石粉按1∶2-4的重量百分比复配。
所述增韧剂为乙烯-甲基丙烯酸丁酯-丙烯酸缩水甘油酯共聚物、乙烯-丙烯酸甲酯共聚物、聚乙烯辛烯-丙烯酸缩水甘油酯共聚物中的一种。
所述润滑剂为乙撑双硬脂酰胺及其改性物、聚硅氧烷的一种或多种；所述抗氧化剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯与亚磷酸三(2，4-二叔丁基苯酯)的复配混合物或三甘醇双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙烯腈、三(2，4-二叔丁基酚)亚磷酸酯中的一种。
所述玻璃纤维为无碱玻璃纤维，直径5-10微米。
一种上述阻燃增强PET材料的制备方法的技术方案是，包括以下步骤：
1)按上述的重量百分比称取物料；
2)将物料倒入搅拌桶中搅拌5-10分钟，搅拌转速为300-800转/分钟；
3)将混合好的原料投入到双螺杆挤出机熔融挤出造粒，在生产过程中从挤出机中段加入长玻璃纤维或用侧喂料加入短玻璃纤维，加工工艺如下：双螺杆挤出机一区230-240℃、二区240-260℃、三区240-260℃、四区240-260℃、五区230-250℃、六区230-250℃、七区230-250℃、八区240-260℃；螺杆转速350-500转/分钟。
本发明的有益效果是：
1)阻燃增强PET材料的GWIT在850℃以上；
2)阻燃增强PET材料的物理机械性能优异。
[具体实施方式]
在本发明以下的实施例和对比例中，PET树脂为聚对苯二甲酸乙二醇酯，其相对密度为1.357，熔点为255-260℃，动力粘度为0.6-0.8Pa·S；十溴二苯乙烷为雅宝8010，相对分子量大于900，溴含量(质量分数)大于80％；磷氮阻燃剂为次膦酸盐类(科莱恩OP 1240)、三聚氰胺磷酸盐(市售BPP)或磷酸盐磷酸三甲苯脂TPP与氮系阻燃剂MCA按重量比1.5∶1复配，以上磷氮阻燃剂同时含有磷元素和氮元素，且热分解温度大于260℃；无机阻燃剂为三氧化二锑，锑酸钠或五氧化二锑中的一种；复合成核剂为长链羧酸盐与滑石粉按1∶3的重量百分比复配而成；玻璃纤维为无碱玻璃纤维(巨石长纤988A或巨石短纤534)；增韧剂为乙烯-甲基丙烯酸丁酯-丙烯酸缩水甘油酯共聚物(杜邦PTW)、乙烯-丙烯酸甲酯共聚物(阿科玛AX-8900)和聚乙烯辛烯-丙烯酸缩水甘油酯共聚物(能之光E516)中的一种；润滑剂为乙撑双硬脂酰胺及其改性物、聚硅氧烷中的一种或几种组合物(市售型号：虎丘TAF，科宁P728，英宝P-2015等)；抗氧化剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯与亚磷酸三(2，4-二叔丁基苯酯)的复配混合物或三甘醇双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙烯腈、三(2，4-二叔丁基酚)亚磷酸酯中的一种或几种混合物(市售型号1010，168，PW-225等)。
实施例1
将重量比PET 55.0％、8010 6.0％、OP 1240 2.0％、三氧化二锑2.0％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
实施例2
将重量比PET 53.0％、8010 4.0％、BPP 6.0％、三氧化二锑1.50％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
实施例3
将重量比PET 53.0％、8010 5.0％、TPP与MCA混合物4.0％、三氧化二锑1.5％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-2250.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
实施例4
将重量比PET 50.0％、8010 5.0％、OP 1240 2.0％、锑酸钠2.0％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤35.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
对比例1
将重量比PET 52.0％、8010 9.0％、三氧化二锑3.0％、PTW 2.5％、复合成核剂1.5％、P7280.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
对比例2
将重量比PET 48.0％、OP 1240 14％、三氧化二锑3.0％、PTW2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
对比例3
将将重量比PET 48.0％、BPP 14％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
对比例4
将将重量比PET 48.0％、TPP与MCA混合物14％、PTW 2.5％、复合成核剂1.5％、P728 0.5％、PW-225 0.4％在搅拌桶中搅拌5分钟，搅拌桶转速为300-800转/分钟；再经双螺杆挤出机熔融挤出造粒，同时从挤出机中段添加长纤30.0％。其加工工艺如下：双螺杆挤出机一区230℃、二区250℃、三区260℃、四区250℃、五区220℃、六区220℃、七区2230℃，八区240℃；螺杆转数控制在450转/分钟。
性能评价标准及性能指标
将上述方法完成造粒的粒子物料先在鼓风烘箱中120-130℃的条件下干燥4-6小时，然后用将干燥好的粒子物料用注射成型机制成样条测试。
实施例与对比例的性能分别如表1和表2：
表1
Figure BSA00000193152200071
表2
Figure BSA00000193152200072
结合表1和表2可以看出，单独使用十溴二苯乙烷、次膦酸盐、三聚氰胺磷酸盐、磷酸盐和氮系阻燃剂混合物都无法使材料的灼热丝点燃温度达850℃以上，而且，单独使用磷氮类阻燃剂会使材料的物理机械性能明显下降，但通过调整十溴二苯乙烷与次膦酸盐、三聚氰胺磷酸盐、磷酸盐和氮系阻燃剂混合物的配比可得到灼热丝点燃温度大于850℃、物理机械性能优异的阻燃增强PET材料。

Claims (9)

1.一种阻燃增强PET材料，其特征在于，按重量百分比由以下组分组成：
所述磷氮阻燃剂为磷酸盐磷酸三甲苯酯与氮系阻燃剂MCA按重量比1.5∶1复配、次膦酸盐类科莱恩OP1240或三聚氰胺磷酸盐，以上磷氮阻燃剂同时含有磷元素和氮元素，且热分解温度大于260℃。
2.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述的十溴二苯乙烷的相对分子量大于900，溴含量大于80％。
3.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述无机阻燃剂为三氧化二锑、锑酸钠或五氧化二锑。
4.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述的PET树脂为聚对苯二甲酸乙二醇酯，其相对密度为1.35-1.38，熔点为255-260℃，粘度为0.6-0.8Pa·S。
5.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述的复 合成核剂为长链羧酸盐与滑石粉按1∶2-4的重量百分比复配。
6.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述增韧剂为乙烯-甲基丙烯酸丁酯-丙烯酸缩水甘油酯共聚物、乙烯-丙烯酸甲酯共聚物、聚乙烯辛烯-丙烯酸缩水甘油酯共聚物中的一种。
7.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述润滑剂为乙撑双硬脂酰胺及其改性物、聚硅氧烷的一种或多种；所述抗氧化剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯与亚磷酸三(2，4-二叔丁基苯酯)的复配混合物或三甘醇双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙烯腈、三(2，4-二叔丁基酚)亚磷酸酯中的一种。
8.根据权利要求1所述的阻燃增强PET材料，其特征在于，所述玻璃纤维为无碱玻璃纤维，直径5-10微米。
9.一种权利要求1所述阻燃增强PET材料的制备方法，其特征在于，包括以下步骤：
1)按权利要求1所述的重量百分比称取物料；
2)将物料倒入搅拌桶中搅拌5-10分钟，搅拌转速为300-800转/分钟；
3)将混合好的原料投入到双螺杆挤出机熔融挤出造粒，在生产过程中从挤出机中段加入长玻璃纤维或用侧喂料加入短玻璃纤维，加工工艺如下：双螺杆挤出机一区230-240℃、二区240-260℃、三区240-260℃、四区240-260℃、五区230-250℃、六区230-250℃、七区230-250℃、八区240-260℃；螺杆转速350-500转/分钟。 
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