CN103724786A - 无卤膨胀阻燃eva专用料及其制备方法 - Google Patents
无卤膨胀阻燃eva专用料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种无卤膨胀阻燃EVA专用料及其制备方法。按重量百分比计,包含复合膨胀阻燃剂的无卤膨胀阻燃EVA包括以下组分:乙烯-醋酸乙烯酯55~70%,复合膨胀阻燃剂15~30%,多壁碳纳米管0.1~3%,相容剂5~10%,抗氧剂0.1~1%,润滑剂0.1~2%。将原料按配比称量,将原料放入高速搅拌机中混合均匀,烘干,干燥温度为60~80℃,再用双螺杆挤出机挤出造粒,挤出机长径比为30~45,挤出温度90~150℃。本发明选用复合阻燃剂及采用独特的纳米复合技术,制备的膨胀阻燃EVA专用料,既具有优异的阻燃性能,又具有理想的物理力学性能、抗化学腐蚀,绿色环保。
Description
技术领域
本发明涉及高分子材料改性技术领域,具体是电线电缆护套料、玩具、包装用无卤阻燃EVA专用料及其制备方法。
背景技术
随着高分子材料应用的快速增长以及经济的迅速发展,人们对阻燃EVA材料的要求在不断提高,特别是通讯行业用电线电缆料、儿童玩具用材料对阻燃性能和力学性能有了更高的要求。现有的阻燃材料大多加入了大量的无机阻燃剂,对材料的物理力学性能造成了较大的损失,从而限制了其在电子线、儿童玩具等领域的使用。经过多年的研究,膨胀阻燃剂因其高效的阻燃性能而快速发展。但是目前市场上用的膨胀阻燃剂大多采用具有酸源、炭源、气源功能的物质进行复配,配比及混合工艺会影响这些复配阻燃剂的协同效果,导致配方及操作工艺复杂。因此,选用集酸源、炭源、气源于一体的复合阻燃剂开发既具有优异的力学性能又具有理想的阻燃效果的无卤膨胀阻燃EVA专用料,具有广阔的应用前景。
发明内容
本发明的目的提供一种无卤膨胀阻燃EVA专用料及其制备方法,本发明选用复合阻燃剂及采用独特的纳米复合技术,制备的膨胀阻燃EVA专用料,既具有优异的阻燃性能,又具有理想的物理力学性能、抗化学腐蚀,绿色环保,该阻燃EVA专用料生产工艺简单,质量稳定。
本发明的目的是通过以下技术方案实现的,无卤膨胀阻燃EVA专用料,由以下质量百分比的各组分组成:
乙烯-乙酸乙烯树脂(EVA) 55~70%;
复合膨胀阻燃剂 15~30%;
多壁碳纳米管 0.1~3%;
相容剂 5~10%;
抗氧剂 0.1~1%;
润滑剂 0.1~2%。
进一步地,所述复合膨胀阻燃剂的结构式为:
进一步地,所述EVA树脂中乙酸乙烯(VA)的质量百分比26~33%。
进一步地,所述多壁碳纳米管纯度大于90%,多壁碳纳米管直径为5~50 nm。
进一步地,所述相容剂为PE-g-MAH(马来酸酐接枝聚乙烯)、EVA-g-MAH(马来酸酐接枝乙烯-乙酸乙烯共聚物)、POE-g-MAH(马来酸酐接枝乙烯-辛烯共聚物)中的任意一种或任意两种混合物或三种混合物。
进一步地,所述抗氧剂为抗氧剂1010、抗氧剂1076、抗氧剂CA中的任意一种或任意两种混合物或三种混合物。
进一步地,所述润滑剂为聚乙烯蜡、白油、固体石蜡中的任意一种或任意两种混合物或三种混合物。
上述无卤膨胀阻燃EVA专用料的制备方法,包括以下步骤:
(1)将配方量的复合膨胀阻燃剂、EVA树脂和润滑剂加入高速混合机中,于40-60℃下搅拌15-30min,充分混匀;
(2)高速混合机中继续加入配方量的多壁碳纳米管、相容剂、抗氧剂,继续搅拌至混合均匀后,烘干,烘干温度为60-80℃;
(3)混匀烘干的物料经双螺杆挤出机挤出造粒,双螺杆挤出机转速为80-200 rpm,双螺杆挤出机长径比为30-45,双螺杆挤出机螺杆各区挤出温度设定为(℃)90,120,140,140,150,150,150,150,150,140。物料经熔融、塑化、挤出成型、定型、冷却牵引、造粒,得到无卤膨胀阻燃EVA专用料。
进一步地,所述高速混合机的搅拌速度设定为150-500rpm。
与现有技术相比,本发明具有以下有益效果:
1. 本发明选用的复合膨胀阻燃剂,复合膨胀阻燃剂为磷氮大分子结构,该阻燃剂磷含量为16~22%,氮含量>25%,平均粒径<10 μm,分解温度(℃)>300,是集三源于一体的复合体系,符合ROHS要求,具有添加方便、与树脂相容性好、阻燃效率高的特点。复合膨胀阻燃剂分子结构是磷氮大分子,集酸源、炭源、气源于一体,高效阻燃,填充后对阻燃EVA专用料的力学性能影响小;复合膨胀阻燃剂因磷氮含量高,在燃烧过程中产生膨胀炭层具有较好的隔热、隔氧效果,并且低烟、无毒、无熔滴,是一种绿色环保高性能阻燃剂,符合ROSH指令。
2.本发明利用复合膨胀阻燃剂分子中的活性胺基,可在熔融条件下与多壁碳纳米管发生界面相互作用,从而有效地改善了碳纳米管在EVA基体中的分散以及与基体的界面粘结力。结果显示:少量(低于1 wt%)的填充量便能同时提高EVA专用料的力学性能及阻燃性能的效果。
附图说明
图1是实施例1制得的膨胀阻燃剂阻燃EVA体系的脆断面微观形貌的SEM图;
图2是实施例5制得的膨胀阻燃剂和多壁碳纳米管协效阻燃EVA体系的脆断面微观形貌的SEM图。
具体实施方式
下面结合实施例和实验例对本发明作进一步详细说明,但它们不是对本发明的限定。
实施例1:
膨胀阻燃EVA专用料的组分比例(重量%):
EVA树脂 60
复合膨胀阻燃剂 30
相容剂 8
抗氧剂 0.5
润滑剂 1.5
将原料按顺序放入高速搅拌机中混合均匀,上料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,冷却所得粒料。
实施例2:
本实施例所述膨胀阻燃EVA专用料,一种配方及其含量为:
膨胀阻燃EVA专用料的组分比例(重量%):
EVA树脂 75
复合膨胀阻燃剂 15
多壁碳纳米管 2
相容剂 5
抗氧剂 1
润滑剂 2
将原料按顺序放入高速搅拌机中混合均匀,上料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,各区温度设定为(℃)90,120,140,140,150,150,150,150,150,140。
实施例3:
膨胀阻燃EVA专用料的组分比例(重量%):
EVA树脂 70
复合膨胀阻燃剂 20
多壁碳纳米管 1.5
相容剂 6
抗氧剂 1
润滑剂 1.5
将原料按顺序放入高速搅拌机中混合均匀,上料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,冷却所得粒料。
实施例4:
膨胀阻燃EVA专用料的组分比例(重量%):
EVA树脂 65
复合膨胀阻燃剂 25
多壁碳纳米管 1
相容剂 7
抗氧剂 0.5
润滑剂 1.5
将原料按顺序放入高速搅拌机中混合均匀,上料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,冷却所得粒料。
实施例5:
膨胀阻燃EVA专用料的组分比例(重量%):
EVA树脂 60
复合膨胀阻燃剂 30
多壁碳纳米管 0.5
相容剂 8
抗氧剂 0.5
润滑剂 1
将原料按顺序放入高速搅拌机中混合均匀,上料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,冷却所得粒料。
对比例1:
EVA树脂 100
将原料烘干,干燥温度为70℃,再用双螺杆挤出机挤出造粒,挤出机长径比为45,冷却所得粒料。用压片机压片成型,以备测试用。
通过以上实施例制得的阻燃EVA专用料的性能检测结果如表1:
表1实施例性能测试结果
实施例 | 拉伸强度/MPa | 断裂伸长率/% | 氧指数/% | 室温时体积电阻率/Ω㎝ |
实施例1 | 8.47 | 1187.9 | 31.1 | 5.54×1016 |
实施例2 | 10.68 | 991.6 | 29.6 | 7.01×1012 |
实施例3 | 11.23 | 1068.5 | 30.9 | 9.48×1013 |
实施例4 | 11.80 | 1124.9 | 33.1 | 6.76×1014 |
实施例5 | 12.76 | 1187.9 | 33.9 | 3.03×1015 |
对比例1 | 15.46 | 1753.7 | 18.3 | - |
对比对比例1的数据可以看出,复合阻燃剂对EVA具有明显的阻燃效果。表1的数据还表明少量(0.5-1wt%)多壁碳纳米管的填充与复合阻燃剂能发挥较好的协效阻燃效果。图1、2是材料脆断面微观形貌的SEM图,图1显示出复合阻燃剂颗粒在EVA基体中总体分散均匀,但是与EVA基体之间出现了一些相分离现象,导致实施例1相比对比例1力学性能大幅度降低。加入多壁碳纳米管后,图2显示出良好的界面粘接性,这是因为多壁碳纳米管与复合阻燃剂上官能团发生相互作用,提高了体系中相之间的界面粘结力。同时从图2还可以看出,复合阻燃剂与碳纳米管在EVA基体中没有出现聚集现象,说明碳纳米管的填充有效地提高复合阻燃剂的分散性,从而获得了优异的物理力学性能及阻燃性能。而且,MWNT的添加量在0~3wt%的条件下制备的阻燃EVA专用料仍具有良好的电绝缘性能。
Claims (9)
1.无卤膨胀阻燃EVA专用料,其特征是,所述EVA专用料由以下质量百分比的各组分组成:
乙烯-乙酸乙烯树脂 55~70%;
复合膨胀阻燃剂 15~30%;
多壁碳纳米管 0.1~3%;
相容剂 5~10%;
抗氧剂 0.1~1%;
润滑剂 0.1~2%。
2.根据权利要求1所述的无卤膨胀阻燃EVA专用料,其特征是,所述EVA树脂中乙酸乙烯的质量百分比26~33%。
4.根据权利要求1所述的无卤膨胀阻燃EVA专用料,其特征是,所述多壁碳纳米管纯度大于90%,多壁碳纳米管直径为5~50 nm。
5.根据权利要求1所述的无卤膨胀阻燃EVA专用料,其特征是,所述相容剂为PE-g-MAH、EVA-g-MAH、POE-g-MAH中的任意一种或任意两种混合物或三种混合物。
6.根据权利要求1所述的无卤膨胀阻燃EVA专用料,其特征是,所述抗氧剂为抗氧剂1010、抗氧剂1076、抗氧剂CA中的任意一种或任意两种混合物或三种混合物。
7.根据权利要求1所述的无卤膨胀阻燃EVA专用料,其特征是,所述润滑剂为聚乙烯蜡、白油、固体石蜡中的任意一种或任意两种混合物或三种混合物。
8.一种制备权利要求1所述的无卤膨胀阻燃EVA专用料的方法,其特征是,所述制备方法包括以下步骤:
(1)将所述配方量的复合膨胀阻燃剂、EVA树脂和润滑剂加入高速混合机中,于40-60℃下搅拌15-30min,充分混匀;
(2)高速混合机中继续加入配方量的多壁碳纳米管、相容剂、抗氧剂,继续搅拌至混合均匀后烘干,烘干温度为60-80℃;
(3)混匀烘干的物料经双螺杆挤出机挤出造粒,双螺杆挤出机转速为80-200 rpm,双螺杆挤出机长径比为30-45,双螺杆挤出机螺杆各区温度设定为90℃、120℃、140℃、140℃、150℃、150℃、150℃、150℃、150℃、140℃;物料经熔融、塑化、挤出成型、定型、冷却牵引、造粒,得到无卤膨胀阻燃EVA专用料。
9.根据权利要求8所述的制备无卤膨胀阻燃EVA专用料的方法,其特征是,步骤(1)所述高速混合机的搅拌速度为150-500rpm。
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