CN102311639A - 一种高灼热丝易配色阻燃玻纤增强聚酰胺材料及其制备方法 - Google Patents

一种高灼热丝易配色阻燃玻纤增强聚酰胺材料及其制备方法 Download PDF

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CN102311639A
CN102311639A CN201010612297A CN201010612297A CN102311639A CN 102311639 A CN102311639 A CN 102311639A CN 201010612297 A CN201010612297 A CN 201010612297A CN 201010612297 A CN201010612297 A CN 201010612297A CN 102311639 A CN102311639 A CN 102311639A
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徐东
徐永
邢家思
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Polymer Science Shenzhen New Materials Co Ltd
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Abstract

本发明公开了一种高灼热丝易配色玻纤增强聚酰胺材料及其制备方法。本发明高灼热丝易配色玻纤增强聚酰胺材料按重量百分比由下列组分组成：聚酰胺41～49％；阻燃剂10～15％；协效阻燃剂3～5％；MC4～8；增韧剂2～4％；抗氧剂0.2～0.6％；加工助剂0.1～0.3％；玻璃纤维20～38％。本发明利用MC高温时脱水成炭，燃烧时释放氮气、二氧化碳和水的特性。当制品接触灼热丝瞬间，MC脱水，释放气体阻隔制品与空气中氧气接触，使玻纤增强尼龙材料达到灼热丝850℃不起燃的阻燃要求标准，MC的加入还大大提高了粒子的白度，起到了易配色的效果。

Description

一种高灼热丝易配色阻燃玻纤增强聚酰胺材料及其制备方法
[技术领域]
本发明涉及高分子材料技术领域，尤其涉及一种高灼热丝易配色玻纤增强聚酰胺材料及其制备方法。
[背景技术]
PA6(聚酰胺6或尼龙6)是半透明或不透明乳白色半结晶形聚合物，它的特点为热力学性能优异，轻质、韧性好、耐化学品和耐久性好，还具有良好的耐磨性、自润滑性。目前尼龙阻燃材料只能做到灼热丝750℃接触30S不起燃。
目前市场上使用的尼龙阻燃剂为十溴二苯乙烷和聚溴化苯乙烯等。使用这两款阻燃剂生产的阻燃尼龙灼热丝只可做到750℃不起燃。十溴二苯乙烷其溴含量高，热稳定性好，抗紫外线性能佳，较其他溴系阻燃剂的渗出性低且售价较低，所以成为目前市场上尼龙通用阻燃剂。然而使用十溴二苯乙烷生产出的阻燃加纤尼龙颜色较黄，当用于配白色等浅色或较鲜艳的颜色时不易配色。
阻燃剂MC为氰尿酸三聚氰胺，属于高效膨胀型阻燃剂，外观：白色结晶粉末，无毒、无味，分解温度约为440～450℃。产品纯度高，高温时脱水成炭，燃烧时释放氮气、二氧化碳和水。本品着色性优越、不含卤素、无腐蚀作用。但使用此款阻燃剂阻燃效果较差，无法制得阻燃V0的阻燃加纤尼龙。
新的澳洲标准即将于2010年10月30日正式实施，新标准要求非金属材料过850℃灼热丝测试，测试条件为测试时间30s，然后移开发热丝，在整个测试期间，试样不可被点燃，滴落无不可引燃绢纸。待澳洲标准实施后，欧美等国家也会相继出台近似标准，提高之前的阻燃要求标准。而目前市场上的阻燃尼龙全部都无法达到此灼热丝要求。
[发明内容]
本发明要解决的技术问题是提供一种阻燃性能好，白度高的高灼热丝易配色玻纤增强聚酰胺材料及其制备方法。
为了解决上述技术问题，本发明采用的技术方案是，一种高灼热丝易配色玻纤增强聚酰胺材料，按重量百分比由下列组分组成：
聚酰胺          41～49％；
阻燃剂          10～15％；
协效阻燃剂      3～5％；
MC              4～8；
增韧剂          2～4％；
抗氧剂          0.2～0.6％；
加工助剂        0.1～0.3％；
玻璃纤维        20～38％。
所述聚酰胺的重均分子量为17000-30000，特性粘度为2.7-2.8的PA6。
所述的阻燃剂为十溴二苯乙烷，所述协效阻燃剂为三氧化二锑。
所述的MC为氰尿酸三聚氰胺。
所述增韧剂为POE接枝马来酸酐。所述的抗氧剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯主抗氧剂和亚磷酸三(2，4-二叔丁基苯酯)辅抗氧剂的复配。
所述的其他助剂包括脱模剂、润滑剂。
以上所述的高灼热丝易配色玻纤增强聚酰胺材料，按重量百分比可以由下列组分组成：
聚酰胺          46～48％；
阻燃剂          10～12％；
协效阻燃剂      3～4％；
MC              4～6；
增韧剂          2～3％；
抗氧剂          0.4～0.6％；
加工助剂        0.1～0.3％；
玻璃纤维        28～32％。
一种上述高灼热丝易配色玻纤增强聚酰胺的其制备方法的技术方案，包括以下步骤：
(1)先将聚酰胺及增韧剂在真空干燥箱中75～85℃干燥4～8小时；
(2)按上述的重量百分比称取全部原料并混合均匀；
(3)将(2)中混合好的原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
本发明利用MC高温时脱水成炭，燃烧时释放氮气、二氧化碳和水。在灼热丝测试时，当制品接触灼热丝瞬间，MC脱水，释放气体阻隔制品与空气中氧气接触，同时十溴二苯乙烷其与Sb203的协同发挥阻燃效应。两种阻燃剂同时使用，使此款阻燃玻纤增强尼龙达到灼热丝850℃不起燃的阻燃要求标准，而MC的加入大大提高了粒子的白度，起到了易配色的效果。
[具体实施方式]
以下结合实施例对本发明作详细的说明：
在下列实施例的复合材料配方中，抗氧剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯，亚磷酸三(2，4-二叔丁基苯酯)，选用Ciba公司生产，商品牌号分别为Irganox1010，和Irganox168。增韧剂为POE接枝马来酸酐，如柏晨PC-28、海尔科化KHEP680C3等，PA6是重均分子量为17000-30000的聚酰胺如新会美达M2800、霍尼韦尔H8202NLB等，粘度为2.8左右的中等粘度PA6；阻燃剂为十溴二苯乙烷如雅宝、寿光、卫东等，协效阻燃剂为三氧化二锑。MC为氰尿酸三聚氰胺如意特、山东卫东等，其他助剂包括脱模剂、润滑剂
实施例1
PA641.7％(重量百分比，下同)、阻燃剂15％、协效阻燃剂5％、MC 4％、增韧剂4％、抗氧剂1010/168 0.1/0.1％、加工助剂0.1％、玻纤30％。
制备方法：先将PA6及增韧剂在真空干燥箱中80℃干燥4～8小时，按配比称取干燥好的PA6和增韧剂及各种助剂，混合好后将全部原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
实施例2，
PA643.1％(重量百分比，下同)、阻燃剂13％、协效阻燃剂4.3％、MC 6％、增韧剂3％、抗氧剂1010/1680.2/0.2％、加工助剂0.2％、玻纤30％。
制备方法：先将PA6及增韧剂在真空干燥箱中80℃干燥4～8小时，按配比称取干燥好的PA6和增韧剂及各种助剂，混合好后将全部原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
实施例3，
PA646.4％(重量百分比，下同)、阻燃剂12％、协效阻燃剂4％、MC 4％、增韧剂3％、抗氧剂1010/168 0.2/0.2％、加工助剂0.2％、玻纤30％。
制备方法：先将PA6及增韧剂在真空干燥箱中80℃干燥4～8小时，按配比称取干燥好的PA6和增韧剂及各种助剂，混合好后将全部原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
实施例4，
PA648.1％(重量百分比，下同)、阻燃剂10％、协效阻燃剂3％、MC 6％、增韧剂2％、抗氧剂1010/168 0.3/0.3％、加工助剂0.3％、玻纤30％。
制备方法：先将PA6及增韧剂在真空干燥箱中80℃干燥4～8小时，按配比称取干燥好的PA6和增韧剂及各种助剂，混合好后将全部原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
实施例5，
PA645.1％(重量百分比，下同)、阻燃剂10％、协效阻燃剂3％、MC 8％、增韧剂3％、抗氧剂1010/168 0.3/0.3％、加工助剂0.3％、玻纤30％。
制备方法：先将PA6及增韧剂在真空干燥箱中80℃干燥4～8小时，按配比称取干燥好的PA6和增韧剂及各种助剂，混合好后将全部原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
性能评价方式及试验标准：
将上述实施例1～5中完成造粒的粒子在130--150℃的鼓风烘箱中干燥4～6小时，再将干燥的粒子在80T注塑机上注塑制样，制样过程中保持模温在70～100℃之间。
拉伸强度按GB/T 1040标准进行检验。试样类型为I型，样条尺寸(mm)：170(长)×(20±0.2)(端部宽度)×(4±0.2)(厚度)，拉伸速度为50mm/分钟；弯曲强度和弯曲模量按GB 9341/T标准进行检验。试样类型为试样尺寸(mm)：(80±2)×(10±0.2)×(4±0.2)，弯曲速度为20mm/分钟；缺口冲击强度按GB/T1043标准进行检验。试样类型为I型，试样尺寸(mm)：(80±2)×(10±0.2)×(4±0.2)；缺口类型为A类，缺口剩余厚度为3.2mm；热变形温度按GB/T 1634.2标准进行检验，负载为1.80MPa.跨距为100mm。灼热丝测试GWIT标准IEC60695标准进行检测，试样尺寸(mm)：(80±2)×(10±0.2)×(4±0.2)，测试时间30s，然后移开发热丝，在整个测试期间，若试样不可被点燃，滴落无不可引燃绢纸即为通过。
实施例1-5的原料重量百分比及制成的复合材料性能表
Figure BDA0000041435580000071
从实施例1-5的原料重量百分比及制成的复合材料性能表可以看出：添加等量玻纤情况下，阻燃剂十溴二苯乙烷添加量10～15％，MC添加量为4～8％时，材料均可达到阻燃V0，均可通过850℃灼热丝GWIT标准。其中当阻燃剂十溴二苯乙烷添加量在10～13％、MC添加量在4～6％时材料性能最好，当阻燃剂十溴二苯乙烷添加量在10～12时材料颜色较白，易配色。
以上对本发明所提供的一种高灼热丝易配色阻燃玻纤增强尼龙及其制备方法进行了详细介绍，本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。

Claims (8)

1.一种高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，按重量百分比由下
列组分组成：
聚酰胺        41～49％；
阻燃剂        10～15％；
协效阻燃剂    3～5％；
MC            4～8；
增韧剂        2～4％；
抗氧剂        0.2～0.6％；
加工助剂      0.1～0.3％；
玻璃纤维      20～38％。
2.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，所述聚酰胺的重均分子量为17000-30000，特性粘度为2.7-2.8的PA6。
3.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，所述的阻燃剂为十溴二苯乙烷，所述协效阻燃剂为三氧化二锑。
4.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，所述的MC为氰尿酸三聚氰胺。
5.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，所述增韧剂为POE接枝马来酸酐；所述的抗氧剂为四[3-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯主抗氧剂和亚磷酸三(2，4-二叔丁基苯酯)辅抗氧剂的复配。
6.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，所述的其他助剂包括脱模剂、润滑剂。
7.根据权利要求1所述的高灼热丝易配色玻纤增强聚酰胺材料，其特征在于，按重量百分比由下列组分组成：
聚酰胺        46～48％；
阻燃剂        10～12％；
协效阻燃剂    3～4％；
MC            4～6；
增韧剂        2～3％；
抗氧剂        0.4～0.6％；
加工助剂      0.1～0.3％；
玻璃纤维      28～32％。
8.一种权利要求1所述高灼热丝易配色玻纤增强聚酰胺的其制备方法，其特征在于，包括以下步骤：
(1)先将聚酰胺及增韧剂在真空干燥箱中75～85℃干燥4～8小时；
(2)按权利要求1所述的重量百分比称取全部原料并混合均匀；
(3)将(2)中混合好的原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度140-180℃，二区温度190-220℃，三区温度220-230℃，四区温度230-250℃，机头180-220℃，停留时间2～3分钟，压力为12-18MPa，螺杆转速130-150转/分钟。
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