CN103992624A - 高灼热丝起燃温度无卤阻燃增强pbt组合物及制备方法 - Google Patents

高灼热丝起燃温度无卤阻燃增强pbt组合物及制备方法 Download PDF

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CN103992624A
CN103992624A CN201410228944.4A CN201410228944A CN103992624A CN 103992624 A CN103992624 A CN 103992624A CN 201410228944 A CN201410228944 A CN 201410228944A CN 103992624 A CN103992624 A CN 103992624A
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free flame
halogen
glowing filament
retardant reinforced
reinforced pbt
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薛东升
姚君
李清平
黄华
胥保礼
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Nantong Xingchen Synthetic Materials Co Ltd
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Abstract

本发明公开了一种高灼热丝起燃温度无卤阻燃增强PBT组合物及制备方法，产品由聚对苯二甲酸丁二醇酯（PBT）,无卤阻燃剂，无碱玻璃纤维，增韧剂，抗氧剂，润滑剂等组成。本发明具有灼热丝起燃温度高（GWIT达到825℃），CTI高（CTI600V），无卤阻燃（达到UL94V-0(1.6mm)）等优点，可用于电子电器等行业。

Description

高灼热丝起燃温度无卤阻燃增强PBT组合物及制备方法
技术领域
本发明涉及一种高分子材料领域，是一种树脂组合物。 
背景技术
阻燃增强PBT大量用于生产白色家电：电冰箱、洗衣机、空调、微波炉等的部件零件。这些电子产品都要求材料高的灼热丝起燃温度、高的CTI值；随着技术的进步和人类对环保的新要求，塑料零件无卤阻燃已成为发展趋势。也对阻燃增强PBT等工程塑料提出了更高的要求，因此有必要开发GWIT高、CTI高的无卤阻燃增强PBT，以适应市场的需求。
发明内容
本发明的目的在于提供一种GWIT高、CTI高的高灼热丝起燃温度无卤阻燃增强PBT组合物及制备方法。
为实现上述目的，本发明采取的技术方案是： 
一种高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：由下列重量百分比的成分组成：
聚对苯二甲酸丁二醇酯          40－55%
无卤阻燃剂A　　　　　　　　  0－20%
无卤阻燃剂B                  0－20%
增韧剂                        0－５%
抗氧剂     　　　　           0－1%
玻璃纤维     　　　　　　     10－3５%
润滑剂                        0－4%；
上述各组分用量之和为100%；                 
所述的无卤阻燃剂A为烷基次磷酸盐，所述的无卤阻燃剂B为次磷酸盐，所述的润滑剂是磷酸三苯酯。
所述的PBT为聚对苯二甲酸丁二醇酯，其特性粘度为1.0 dL/g。
所述的无卤型阻燃剂B为次磷酸铝。
所述的玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维。 
所述的增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物。 
所述的抗氧剂是抗氧剂1010与抗氧剂168的复合物。 
所述的润滑剂是磷酸三苯酯。 
一种高灼热丝起燃温度的无卤阻燃增强PBT组合物的制备方法，其特征是：包括下列步骤：
（1）称取各原料； 
（2）将称好的各种原料放入高混机中，混合出料，然后用双螺杆挤出机挤出造粒； 所述的双螺杆挤出机的加工温度为230～245℃，螺杆转数为30～40Hz。
本发明本发明优点在于： 
1、采用新型阻燃剂复配体系，和专利CN200510021394.X （无卤阻燃，GWIT775 ℃），CN200810155087.4（ 无卤阻燃（2.0mmV0），GWIT800 ℃）的阻燃体系相比，新型复配体系能使材料的GWIT值提高25℃到50℃，能够通过825℃灼热丝； 
2、采用磷酸三苯酯作为润滑剂，①提高材料加工流动性，防止阻燃剂分解；②改善材料的表面，防止材料表面浮纤；③提高材料的阻燃性能。 
3、本发明在上述加工条件下，原料分散性较好，材料的质量稳定；制备得到的复合材料的GWIT值及CTI值高，阻燃效果较好，复合材料无卤环保，综合性能均衡，可以广泛用于无人看管电器、白色家电等电子电器领域的产品。 
下面结合实施例对本发明作进一步说明。
具体实施方式
实施例1：PBT复合材料的制备（一）  
PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐、阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010与抗氧剂168的复合物，（抗氧剂1010与抗氧剂的重量比为1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 45%，阻燃剂A 10%，阻燃剂B 10%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加入玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
实施例2：PBT复合材料的制备（二）
 PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐、阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010与抗氧剂168的复合物，（抗氧剂1010与抗氧剂的重量比为1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 45%，阻燃剂A 8%，阻燃剂B 12%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加入玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
实施例3：PBT复合材料的制备（三） 
PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐、阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010与抗氧剂168的复合物，（抗氧剂1010与抗氧剂的重量比为1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 45%，阻燃剂A 12%，阻燃剂B 8%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加入玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz
实施例4：PBT复合材料的制备（四） 
PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐、阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010与抗氧剂168的复合物，（抗氧剂1010与抗氧剂的重量比为1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 44%，阻燃剂A 10%，阻燃剂B 11%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加玻璃纤维30%，入挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
对比例1
PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010/168（1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 45%，阻燃剂A 20%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
对比例2
PBT的特性粘度为1.0 dL/g，阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010/168（1：2），润滑剂是磷酸三苯酯。 
按以下重量百分比含量称取各原料组分：PBT 45%，阻燃剂A 20%，增韧剂2.7%，抗氧剂0.3%，润滑剂2%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
对比例3
PBT的特性粘度为1.0 dL/g，阻燃剂A为烷基次磷酸盐、阻燃剂B为次磷酸铝，玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维，增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物，抗氧剂为抗氧剂1010/168（1：2）。 
按以下重量百分比含量称取各原料组分：PBT 46%，阻燃剂A 10%，阻燃剂B11%，增韧剂2.7%，抗氧剂0.3%。将称好的各原料放入高混机中，混合2分钟，出料，然后用双螺杆挤出机加玻璃纤维30%，挤出造粒；所述的双螺杆挤出机的加工温度为230～250℃，挤出机包括九个温区，其中一段245℃，二段240℃，三段240℃，四段235℃，五段235℃，六段235℃，七段235℃，螺杆转数为30Hz。
表1实施例1-4与对比例1-3的原料配比：
原料 实施例1 实施例2 实施例3 实施例4 对比例1 对比例2 对比例3
PBT 45 45 45 44 45 45 46
阻燃剂A 10 8 12 10 20 -- 10
阻燃剂B 10 12 8 11 -- 20 11
增韧剂 2.7 2.7 2.7 2.7 2.7 2.7 2.7
抗氧剂 0.3 0.3 0.3 0.3 0.3 0.3 0.3
玻璃纤维 30 30 30 30 30 30 30
润滑剂 2 2 2 2 2 2  --
表2实施例1-4与对比例1-3的性能测试：
测试项目 实施例1 实施例2 实施例3 实施例4 对比例1 对比例2 对比例3
拉伸强度(Mpa) 110 107 112 108 114 105 99
弯曲强度(Mpa) 161 158 170 160 172 155 152
缺口冲击强度(KJ/m2) 12.2 11.6 12.3 11.8 12.4 11.1 10.1
无缺口冲击强度(KJ/m2) 51 48 51 50 55 46 42
阻燃（1.6mm） V0 V0 V0 V0 V0 V0 V0
GWIT/℃ 800 815 800 825 800 800 775
CTI/V 600 600 600 600 600 600 600
备注 注塑件外观较好 注塑件外观较好 注塑件外观较好 注塑件外观较好 注塑件外观较好 注塑件外观较好 注塑件表面浮纤
由此可以看出本发明的优异效果。

Claims (8)

1.一种高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：由下列重量百分比的成分组成：
聚对苯二甲酸丁二醇酯          40－55%
无卤阻燃剂A　　　　　　　　  0－20%
无卤阻燃剂B                  0－20%
增韧剂                        0－５%
抗氧剂     　　　　           0－1%
玻璃纤维     　　　　　　     10－3５%
润滑剂                        0－4%；
上述各组分用量之和为100%；                 
所述的无卤阻燃剂A为烷基次磷酸盐，所述的无卤阻燃剂B为次磷酸盐，所述的润滑剂是磷酸三苯酯。
2.根据权利要求1所述的高灼热丝起燃温度的无卤阻燃增强PBT组合物，其特征是：所述的PBT为聚对苯二甲酸丁二醇酯，其特性粘度为1.0 dL/g。
3. 根据权利要求1所述的高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：所述的无卤型阻燃剂B为次磷酸铝。
4. 根据权利要求1或2所述的高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：所述的玻璃纤维为表面经硅烷偶联剂处理的无碱玻璃纤维。 
5. 根据权利要求1或2所述的高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：所述的增韧剂为乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物。 
6. 根据权利要求1或2所述的高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：所述的抗氧剂是抗氧剂1010与抗氧剂168的复合物。 
7. 根据权利要求1或2所述的高灼热丝起燃温度无卤阻燃增强PBT组合物，其特征是：所述的润滑剂是磷酸三苯酯。 
8. 一种权利要求1所述的高灼热丝起燃温度的无卤阻燃增强PBT组合物的制备方法，其特征是：包括下列步骤：
（1）称取各原料； 
（2）将称好的各种原料放入高混机中，混合出料，然后用双螺杆挤出机挤出造粒； 所述的双螺杆挤出机的加工温度为230～245℃，螺杆转数为30～40Hz。
CN201410228944.4A 2014-05-28 2014-05-28 高灼热丝起燃温度无卤阻燃增强pbt组合物及制备方法 Pending CN103992624A (zh)

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