CN112646366A - 长玻纤增强尼龙复合材料无卤环保阻燃母粒及其制备方法 - Google Patents

长玻纤增强尼龙复合材料无卤环保阻燃母粒及其制备方法 Download PDF

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CN112646366A
CN112646366A CN202011525880.6A CN202011525880A CN112646366A CN 112646366 A CN112646366 A CN 112646366A CN 202011525880 A CN202011525880 A CN 202011525880A CN 112646366 A CN112646366 A CN 112646366A
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glass fiber
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吴建国
刘渊
陈荣
闻辉
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Jiangsu Jitri Advanced Polymer Materials Research Institute Co Ltd
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Abstract

本发明提供了一种长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，包括：向三口烧瓶内分别依次加入400ml甲酸溶液和40g低分子量尼龙并充分搅拌；向溶液中加入120g二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末，经干燥及粉碎后得到微胶囊化的改性二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末；以55％质量百分比的低粘尼龙6为载体，加入阻燃剂粉末、纳米材料阻燃增效剂、抗氧剂、润滑剂，经双螺杆挤出机熔融挤出造粒得到玻纤增强聚丙烯用环保阻燃母粒。本发明在无卤阻燃剂复配基础上，引入纳米材料，大大提高阻燃效率，阻燃剂用量可降低，并且低落现象明显减少，力学性能更优。

Description

长玻纤增强尼龙复合材料无卤环保阻燃母粒及其制备方法
技术领域
本发明涉及无卤环保阻燃母粒领域，特别涉及一种长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法。
背景技术
长玻纤增强尼龙复合材料制备过程中不方便直接添加阻燃剂，长玻纤增强尼龙复合材料加工温度高、受热时间长，阻燃剂易受热分解失效，通常将长玻纤增强尼龙复合材料颗粒料与阻燃母粒混合均匀后注塑或模压成型。
但是，目前用于玻纤增强尼龙的无卤阻燃剂品种少，可用于尼龙的阻燃剂主要有红磷、二乙基次磷酸铝、三聚氰胺聚磷酸盐等，且无卤环保阻燃剂为亲水性极性材料，尼龙为疏水性非极性材料，二者相溶性差，无卤环保阻燃剂加入尼龙中会对力学性能带来负面影响。
发明内容
本发明提供了一种长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，以解决至少一个上述技术问题。
为解决上述问题，作为本发明的一个方面，提供了一种长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，包括：
步骤1，将1000ml三口烧瓶置于水浴锅中固定，并将水浴锅的温度调至60℃，并在此温度下向三口烧瓶内分别依次加入400ml甲酸溶液和40g低分子量尼龙并充分搅拌；待低分子量尼龙完全溶解于甲酸溶液后，向溶液中加入120g二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末，持续搅拌30min，然后取出三口烧瓶内的混合物，经干燥及粉碎后得到微胶囊化的改性二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末；
步骤2，以55％质量百分比的低粘尼龙6为载体，加入35-43.8％质量百分比的所述阻燃剂粉末、1-8％质量百分比的纳米材料阻燃增效剂、0.1-1.0％质量百分比的一种抗氧剂或两种复配抗氧剂、及0.1-1.0％质量百分比的润滑剂，经双螺杆挤出机熔融挤出造粒得到玻纤增强聚丙烯用环保阻燃母粒。
优选地，低分子量尼龙的分子量为5000-30000。
优选地，二乙基次磷酸铝与三聚氰胺聚磷酸盐配比为0.1-0.9质量百分比。
优选地，所述步骤1中的干燥及粉碎包括：放入80℃的真空烘箱中干燥去除甲酸溶剂，经气流式超微粉机粉碎。
优选地，所述纳米材料选自有机化蒙脱土、碳纳米管、石墨烯。
优选地，抗氧剂或两种复配抗氧剂选自抗氧剂1010、抗氧剂168。
优选地，润滑剂为硅酮。
本发明还提供了一种长玻纤增强尼龙复合材料用无卤环保阻燃母粒，其特征在于，采用上述的方法制得。
可见，本发明通过对无卤环保阻燃剂的表面改性处理(偶联剂改性或能与阻燃剂形成氢键的介质包覆形成微胶囊)，改善其与尼龙的相容性，在改善尼龙的阻燃性能的同时，尽量降低其对长玻纤增强尼龙复合材料力学性能的负面影响，并提高其阻燃效率；此外，低分子量尼龙上的酰胺基团可与二乙基次磷酸铝与三聚氰胺聚磷酸盐上-C＝O和-N-H结合形成氢键，用低分子量尼龙囊包覆二乙基次磷酸铝与三聚氰胺聚磷酸盐后，与尼龙相容性改善。
综上所述，本发明在无卤阻燃剂复配(二乙基次磷酸铝与三聚氰胺聚磷酸盐复配)基础上，引入第三组分-纳米材料(阻燃增效剂)，大大提高阻燃效率，阻燃剂用量可降低，并且低落现象明显减少，力学性能更优。
具体实施方式
以下对本发明的实施例进行详细说明，但是本发明可以由权利要求限定和覆盖的多种不同方式实施。
本发明中的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法采用以下步骤进行：
步骤1，将1000ml三口烧瓶置于水浴锅中固定，并将水浴锅的温度调至60℃；在此温度下，向三口烧瓶内依次加入400ml甲酸溶液和40g低分子量尼龙(分子量5000-30000)并充分搅拌；待低分子量尼龙完全溶解于甲酸溶液后，向溶液中加入120g二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末(二乙基次磷酸铝与三聚氰胺聚磷酸盐配比为0.1-0.9)(质量百分比)，持续搅拌30min，然后取出三口烧瓶内的混合物，并放入80℃的真空烘箱中干燥去除甲酸溶剂，经气流式超微粉机粉碎后得到微胶囊化的改性二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末。
步骤2，以低粘尼龙6为载体55％(都是质量百分比)，分别加入微胶囊化的改性二乙基次磷酸铝与三聚氰胺聚磷酸盐复配粉末阻燃剂35-43.8％，有机化蒙脱土、碳纳米管、石墨烯等纳米材料中任意一种阻燃增效剂1-8％，抗氧剂1010(牌号)、抗氧剂168(牌号)等中一种或任意两种复配抗氧剂0.1-1.0％，硅酮等润滑剂0.1-1.0％，经双螺杆挤出机熔融挤出造粒值得玻纤增强聚丙烯用环保阻燃母粒。
通过上述方法制备的长玻纤增强尼龙复合材料用无卤环保阻燃母粒的性能对比情况，如下表所示：
Figure BDA0002850786500000031
Figure BDA0002850786500000041
下面，结合现有技术中进行进一步的比较。
(1)CN106147221A：为短玻纤增强，与本发明中的长玻纤增强工艺技术完全不同；所用阻燃剂虽为两种复配，但二者均为含磷阻燃剂，并且未进行表面改性处理，其阻燃效率低、对材料力学性能负面影响大；本发明为含磷和氮的两种阻燃剂复配，比单一含磷或氮阻燃剂复配阻燃效果好。
(2)CN 107778527A：所用两种阻燃剂也均为含磷阻燃剂，并且未进行表面改性处理，其阻燃效率低、对材料力学性能负面影响大；本发明为含磷和氮的两种阻燃剂复配，比单一含磷或氮阻燃剂复配阻燃效果好。
(3)CN 108102361A：虽为多种含磷和氮阻燃剂复配，氮关键是阻燃剂表面未进行改性处理，其与高分子材料相容性差，不仅阻燃效率低，而且对材料力学性能负面影响大；本发明的核心技术是磷氮两种阻燃剂复配的同时进行了表面改性微胶囊化，粒径小、分散均匀，与高分子材料相容性好，阻燃效率高，对材料力学性能负面影响降到最低。
可见，本发明通过对无卤环保阻燃剂的表面改性处理(偶联剂改性或能与阻燃剂形成氢键的介质包覆形成微胶囊)，改善其与尼龙的相容性，在改善尼龙的阻燃性能的同时，尽量降低其对长玻纤增强尼龙复合材料力学性能的负面影响，并提高其阻燃效率；此外，低分子量尼龙上的酰胺基团可与二乙基次磷酸铝与三聚氰胺聚磷酸盐上-C＝O和-N-H结合形成氢键，用低分子量尼龙囊包覆二乙基次磷酸铝与三聚氰胺聚磷酸盐后，与尼龙相容性改善。
综上所述，本发明在无卤阻燃剂复配(二乙基次磷酸铝与三聚氰胺聚磷酸盐复配)基础上，引入第三组分-纳米材料(阻燃增效剂)，大大提高阻燃效率，阻燃剂用量可降低，并且低落现象明显减少，力学性能更优。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (8)

1.一种长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，包括：
步骤1，将1000ml三口烧瓶置于水浴锅中固定，并将水浴锅的温度调至60℃，并在此温度下向三口烧瓶内分别依次加入400ml甲酸溶液和40g低分子量尼龙并充分搅拌；待低分子量尼龙完全溶解于甲酸溶液后，向溶液中加入120g二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末，持续搅拌30min，然后取出三口烧瓶内的混合物，经干燥及粉碎后得到微胶囊化的改性二乙基次磷酸铝与三聚氰胺聚磷酸盐复配阻燃剂粉末；
步骤2，以55％质量百分比的低粘尼龙6为载体，加入35-43.8％质量百分比的所述阻燃剂粉末、1-8％质量百分比的纳米材料阻燃增效剂、0.1-1.0％质量百分比的一种抗氧剂或两种复配抗氧剂、及0.1-1.0％质量百分比的润滑剂，经双螺杆挤出机熔融挤出造粒得到玻纤增强聚丙烯用环保阻燃母粒。
2.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，低分子量尼龙的分子量为5000-30000。
3.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，二乙基次磷酸铝与三聚氰胺聚磷酸盐配比为0.1-0.9质量百分比。
4.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，所述步骤1中的干燥及粉碎包括：放入80℃的真空烘箱中干燥去除甲酸溶剂，经气流式超微粉机粉碎。
5.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，所述纳米材料选自有机化蒙脱土、碳纳米管、石墨烯。
6.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，抗氧剂或两种复配抗氧剂选自抗氧剂1010、抗氧剂168。
7.根据权利要求1所述的长玻纤增强尼龙复合材料无卤环保阻燃母粒制备方法，其特征在于，润滑剂为硅酮。
8.一种长玻纤增强尼龙复合材料用无卤环保阻燃母粒，其特征在于，采用权利要求1-7中任一项所述的方法制得。
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