CN103122142A - 一种纳米增强增韧pa6改性合金的制备方法 - Google Patents
一种纳米增强增韧pa6改性合金的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米增强增韧PA6改性合金的制备方法,首先将无机纳米粒子、硅烷偶联剂混合均匀,经超声分散10~30min后加入乙醇和水,在60~80℃的水溶液中搅拌1~2h,再用氨水调节pH值到8.5~9.5,冷却、过滤、洗涤,100~120℃干燥后,得到硅烷偶联剂表面改性的无机纳米粒子;然后,将尼龙、硅烷偶联剂表面改性的无机纳米粒子、接技PP、润滑剂、抗氧剂在1000~2000转/分下高速混合15~30分钟,得到预混料;最后将预混料喂入双螺杆挤出机中,添加玻璃纤维,其中螺杆区的温度为220~270℃,螺杆转速为200~500转/分,挤出造粒即得目标产物。本发明的制备方法可以同时实现增韧增强的目的,提高材料的综合性能,满足多种用途的需要。
Description
技术领域
本发明属于高分子纳米复合材料领域,特别涉及一种纳米微粒、玻璃纤维及接技PP协同改性尼龙的制备方法。
背景技术
尼龙具有力学强度高、熔点高、耐磨耐油等优点,被广泛用于汽车、机电、电子、纺织、家电等领域。随着应用领域的不断拓展,对尼龙的韧性和强度提出了更高的要求。通常的增韧方法是加入增韧剂如PP(聚丙烯)、PE(聚乙烯)等非极性聚合物。这类非极性聚合物能有效降低尼龙的吸水性,从而达到增韧目的。但是,这种增韧方法往往同时大幅度地降低了尼龙的强度,不能满足高强度要求。通过在尼龙中加入玻璃纤维可以大大提高尼龙6的强度,但是,现有的涉及改性尼龙6的技术文献显示虽在材料的强度、韧性上有很大提升,但也不同程度存在着材料表面质量欠佳、力学性能在某些情况下不能满足应用要求的问题。
发明内容
鉴于以上问题,本发明的目的是提供一种纳米微粒、玻璃纤维、接技PP多元协同改性尼龙的方法,可以同时实现增强增韧的目的,满足不同领域的需要。
一种纳米增强增韧PA6改性合金的制备方法,包括如下步骤:
(1)将无机纳米粒子、硅烷偶联剂混合均匀,经超声分散10~30min后加入乙醇和水,在60~80℃的水溶液中搅拌1~2h,再用氨水调节pH值到8.5~9.5,冷却、过滤、洗涤,100~120℃干燥后,得到硅烷偶联剂表面改性的无机纳米粒子;其中,硅烷偶联剂的加入量为无机纳米粒子的2~5%;
(2)将尼龙、步骤(1)中得到的硅烷偶联剂表面改性的无机纳米粒子、接技PP、润滑剂、抗氧剂在1000~2000转/分下高速混合15~30分钟,得到预混料;
(3)将步骤(2)得到的预混料喂入双螺杆挤出机中,在双螺杆挤出机的专用玻璃纤维口处添加玻璃纤维,其中螺杆区的温度为220~270℃,螺杆转速为200~500转/分,挤出造粒,即可得纳米微粒、玻璃纤维、接技PP多元协同改性的所述纳米增强增韧PA6改性合金。
原料按如下重量份进行添加:尼龙50~70份,硅烷偶联剂表面改性的无机纳米粒子2~10份,接技PP 5~20份,润滑剂0.5~1份,抗氧剂0.5~1份,玻璃纤维15~20份。
所述接技PP为马来酸酐接技PP即PP-g-MAH,马来酸二丁脂接技PP即PP-g-DBM,马来酸接枝PP即PP-g-MAC。
所述无机纳米粒子为纳米碳酸钙、纳米二氧化硅、纳米三氧化二铝中的一种和几种的混合物。
所述硅烷偶联剂选自γ-氨丙基三乙氧基硅烷(KH550)、γ-(2,3-環氧丙基)丙基三甲氧基硅烷(KH560)、r-(甲基丙烯酸氧)丙基三甲氧基硅烷(KH570)中的一种或几种的混合物。
所述尼龙6选自任意一种密度在1.09~1.17g/cm2,熔点在210~230℃。
所述玻璃纤维是无碱玻璃纤维,直径5~20μm。
所述润滑剂为硬脂酸钙、聚乙烯蜡或乙撑双硬脂酰胺或由它们组成的混合物。
所述的抗氧剂为四(β-(3,5-二叔丁基-4羟基苯基)丙酸)季戊四醇脂(抗氧剂1010),N, N’一双[3-(3.5-二叔丁基-4-羟基苯基)丙酰]肼(抗氧剂1098)或三(2.4-二叔丁基丙基)亚磷酸酯(抗氧剂168)或由它们组成的混合物。
本发明的优点和积极效果如下:经硅烷偶联剂处理的纳米粒子的加入把聚合物的韧性强,介电性、阻隔性好,外观观感适应性广,易加工等优异性能,与无机物的刚性,尺寸稳定性和热稳定性结合起来。由于聚合物对纳米粒子的包覆,使纳米粒子的尺寸及表面特征得以稳定,因而使复合材料的特性得以长期稳定,保持他们之间的优势互补的协同效应。纳米粒子以它巨大的表面能与聚合物相作用,有活性键,成为即增韧又增强的复合材料,当受到冲击时,每个微粒子虽仍是应力点,但能通过粒子将应力传递分散到更大的基体体积去共同承担外力,并在各个粒子的周边,可诱发产生大量的银紋或微裂纹,在它们本身消耗冲击能转化为分子键变形能及新产生的表面能的同时,在银纹或微裂纹的前锋相会处,在两条纹间的基体会产生剪切变形,变形需要吸收能量,直至基体条被扭断,微裂纹才能继续发展,这一过程就起到吸收冲击性能并拟制微裂纹扩展的作用,有利于提高材料的冲击韧性。由于材料微裂时内部有裂纹,但宏观表现只是发白,材料并不断裂,能吸收大量冲击能而不破坏,材料就具有较好的韧性。接技PP的加入,不仅改善了PA6的吸湿性,提高了制品的尺寸稳定性,同时对PA6有一定的增韧作用,提高了其冲击强度。玻璃纤维对尼龙有较好的增强作用。
所以,本发明的纳米微粒、接技PP、玻璃纤维多元协同改性尼龙,可以同时实现增韧增强的目的,提高材料的综合性能,满足多种用途的需要。
具体实施方式
下面结合实施例对本发明作进一步说明,但不应以此限制本发明的保护范围。
实施例见下表1,表中各组分的含量均为质量分数。制备方法如下:
(1)将无机纳米粒子、硅烷偶联剂混合均匀,经超声分散10~30min后加入乙醇和水,在60~80℃的水溶液中搅拌1~2h,再用氨水调节pH值到8.5~9.5,冷却、过滤、洗涤,100~120℃干燥后,得到硅烷偶联剂表面改性的无机纳米粒子;
(2)将尼龙、步骤(1)中得到的硅烷偶联剂表面改性的无机纳米粒子、接技PP、润滑剂、抗氧剂在1000~2000转/分下高速混合15~30分钟,得到预混料;
(3)将步骤(2)得到的预混料喂入双螺杆挤出机中,在双螺杆挤出机的专用玻璃纤维口处添加玻璃纤维,其中螺杆区的温度为220~270℃,螺杆转速为200~500转/分,挤出造粒,即可得纳米微粒、玻璃纤维、接技PP多元协同改性的所述纳米增强增韧PA6改性合金。
实施例1~7采用的硅烷偶联剂表面改性的无机纳米粒子如下:
实施例1:硅烷偶联剂K550——纳米粒子CaCO3;
实施例2:硅烷偶联剂K570——纳米粒子CaCO3;
实施例3:硅烷偶联剂K550——纳米粒子SiO2;
实施例4:硅烷偶联剂K570——纳米粒子SiO2;
实施例5:硅烷偶联剂K550——纳米粒子CaCO3;
实施例6:硅烷偶联剂K570——纳米粒子SiO2;
实施例7:硅烷偶联剂K570——纳米粒子Al2O3。
实施例1~7采用的改性PP如下:
实施例1:PP-g-MAH;
实施例2:PP-g-DBM;
实施例3:PP-g-MAH;
实施例4:PP-g-MAC;
实施例5:PP-g-DBM;
实施例6:PP-g-MAC;
实施例7:PP-g-DBM。
从表1的实验结果可以看出:
1、与未加纳米粒子的对比组相比,加入纳米粒子后的实施例中产物的材料抗拉强度、弯曲强度、冲击韧性都有明显的提高;
2、实施例3加入的接枝PP为PP-g-MAH,实施例4加入的接枝PP为PP-g-MAC,实施例5加入的接枝PP为PP-g-DBM,实施例6加入的接枝PP为PP-g-MAC,可以看出,加入接枝PP为PP-g-MAC比加入接枝PP为PP-g-MAH和接枝PP为PP-g-DBM更有利于性能的提高;
3、相比仅加入接枝PP的实施例和既加入接枝PP又加入PP的实施例,可以看出,仅加入接枝PP更有利于综合性能的提高。
Claims (9)
1.一种纳米增强增韧PA6改性合金的制备方法,其特征在于,包括如下步骤:
(1)将无机纳米粒子、硅烷偶联剂混合均匀,经超声分散10~30min后加入乙醇和水,在60~80℃的水溶液中搅拌1~2h,再用氨水调节pH值到8.5~9.5,冷却、过滤、洗涤,100~120℃干燥后,得到硅烷偶联剂表面改性的无机纳米粒子;其中,硅烷偶联剂的加入量为无机纳米粒子的2~5%;
(2)将尼龙、步骤(1)中得到的硅烷偶联剂表面改性的无机纳米粒子、接技PP、润滑剂、抗氧剂在1000~2000转/分下高速混合15~30分钟,得到预混料;
(3)将步骤(2)得到的预混料喂入双螺杆挤出机中,在双螺杆挤出机的专用玻璃纤维口处添加玻璃纤维,其中螺杆区的温度为220~270℃,螺杆转速为200~500转/分,挤出造粒,即可得纳米微粒、玻璃纤维、接技PP多元协同改性的所述纳米增强增韧PA6改性合金。
2.根据权利要求1所述的制备方法,其特征在于,原料按如下重量份进行添加:尼龙50~70份,硅烷偶联剂表面改性的无机纳米粒子2~10份,接技PP 5~20份,润滑剂0.5~1份,抗氧剂0.5~1份,玻璃纤维15~20份。
3.根据权利要求1所述的制备方法,其特征在于,所述接技PP为马来酸酐接技PP即PP-g-MAH,马来酸二丁脂接技PP即PP-g-DBM,马来酸接枝PP即PP-g-MAC。
4.根据权利要求1所述的制备方法,其特征在于,所述无机纳米粒子为纳米碳酸钙、纳米二氧化硅、纳米三氧化二铝中的一种和几种的混合物。
5.根据权利要求1所述的制备方法,其特征在于,所述硅烷偶联剂选自γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙基)丙基三甲氧基硅烷、r-(甲基丙烯酸氧)丙基三甲氧基硅烷中的一种或几种的混合物。
6.根据权利要求1所述的制备方法,其特征在于,所述尼龙6选自任意一种密度在1.09~1.17g/cm2,熔点在210~230℃。
7.根据权利要求1所述的制备方法,其特征在于,所述玻璃纤维是无碱玻璃纤维,直径5~20μm。
8.根据权利要求1所述的制备方法,其特征在于,所述润滑剂为硬脂酸钙、聚乙烯蜡或乙撑双硬脂酰胺或由它们组成的混合物。
9.根据权利要求1所述的制备方法,其特征在于,所述的抗氧剂为四(β-(3,5-二叔丁基-4羟基苯基)丙酸)季戊四醇脂、N, N’-双[3-(3.5-二叔丁基-4-羟基苯基)丙酰]肼或三(2.4-二叔丁基丙基)亚磷酸酯或由它们组成的混合物。
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