CN103627165B - 高粘度玻璃纤维增强聚酰胺树脂及制备方法 - Google Patents

高粘度玻璃纤维增强聚酰胺树脂及制备方法 Download PDF

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CN103627165B
CN103627165B CN201210310421.5A CN201210310421A CN103627165B CN 103627165 B CN103627165 B CN 103627165B CN 201210310421 A CN201210310421 A CN 201210310421A CN 103627165 B CN103627165 B CN 103627165B
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glass fibre
reinforced polyamide
polyamide resin
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李俊伟
刘凡
朱欣睿
朱明毅
杨刚
浦蔚蔚
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Mitac Precision Technology Kunshan Ltd
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Abstract

一种高粘度玻璃纤维增强聚酰胺树脂及制备方法，按重量百分数计算，该树脂包括如下组分：低粘度玻璃纤维增强聚酰胺树脂30～80%；扁平玻璃纤维5～50%；聚酰胺树脂5～50%；阻燃剂1～30%；加工助剂0～5%。该制备方法包括以下步骤：（a）将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；（b）称取阻燃剂及加工助剂加入到高速混合机中高速预混；（c）将上述步骤（a）、步骤（b）中混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒。

Description

高粘度玻璃纤维增强聚酰胺树脂及制备方法
【技术领域】
本发明涉及一种玻璃纤维增强聚酰胺树脂，具体涉及一种高粘度玻璃纤维增强聚酰胺树脂及制备方法。
【背景技术】
由于近年来对产品降低成本，轻量化等需求变高，金属正逐渐被树脂替代，但必须要求树脂具有和金属同等的强度、刚性，尤其对于电气安装部件、笔记本电脑或家电产品。工程塑料中的玻璃纤维增强聚酰胺树脂具有高硬度、高冲击强度、高热变形温度，在汽车、家用电器、娱乐电子及机械工程设备等领域得到广泛应用。
随着工程塑料的应用，其不可降解的问题也受到了广泛的关注，其产品在被使用后难以处理，不仅造成浪费，而且对环境也造成污染，此外，注塑级工程塑料在成型时下脚料或不良品的分量也越来越重，对其进行回收利用有着显著地经济效益和社会效益。工程塑料一次使用过后，塑料分解严重，分子链断裂，生成大量的小分子或挥发性物质，粘度降低，同时力学性能下降，无法达到使用要求。
【发明内容】
鉴于上述问题，本发明目的在于提供一种方法可以提高玻璃纤维增强聚酰胺树脂的粘度及力学性能，从而达到注塑成型的要求。
为了达到上述目的，本发明提供一种高粘度玻璃纤维增强聚酰胺树脂，按重量百分数计算，其包括如下组分：
较佳的，所述低粘度玻璃纤维增强聚酰胺树脂的熔融指数为50～150g/10min,熔点为240～320℃。
较佳的，所述低粘度玻璃纤维增强聚酰胺树脂中的玻璃纤维重量为低粘度玻璃纤维增强聚酰胺树脂重量的30～70%。
较佳的，所述扁平玻璃纤维的扁平率为2～8，更佳的为4～6。
较佳的，所述扁平玻璃纤维的截面的短径为0.5～25μm，截面的长径为1.0～250μm。
较佳的，所述聚酰胺树脂为PA6、PA66、PA6/6T、PA6T、PA6T/61、PA66/6T中的一种、两种或两种以上的混合物。
较佳的，所述阻燃剂包括主阻燃剂和助阻燃剂。
较佳的，所述主阻燃剂为二乙基次磷酸铝、二乙基次磷酸锌、甲基次磷酸铝、甲基次磷酸锌中的一种、两种或两种以上的混合物。
较佳的，所述助阻燃剂为磷酸三聚氰胺或多磷酸三聚氰胺，较佳的为多磷酸三聚氰胺。
较佳的，所述加工助剂为润滑剂、抗氧化剂、静电防止剂、扩链剂、紫外线吸收剂、脱模剂及着色剂中的一种、两种或两种以上的混合物。
另外本发明提供一种高粘度玻璃纤维增强聚酰胺树脂的制备方法，用于制备上述高粘度玻璃纤维增强树脂，该方法包括以下步骤：
（a）将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；
（b）称取阻燃剂及加工助剂加入到高速混合机中高速预混；
（c）将上述步骤（a）、步骤（b）中混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒，双螺杆挤出机的各区间温度分别为：一区间150～180℃，二区间200～250℃，三区间270～310℃，四区间280～320℃，五区间280～320℃，六区间280～320℃，七区间280～320℃，八区间280～320℃，九区间280～320℃，机头温度为310～340℃。
相较于现有技术，本发明高粘度玻璃纤维增强聚酰胺树脂及其制备方法，在低粘度的玻璃纤维增强聚酰胺树脂中加入扁平玻璃纤维、聚酰胺树脂、阻燃剂及加工助剂对其进行回收利用得到高粘度的玻璃纤维增强聚酰胺树脂，该高粘度玻璃纤维增强聚酰胺树脂具有高粘度、耐高温性及力学性能更强，使其更加广泛应用于汽车、家电产品、娱乐电子及机械设备等领域。
【具体实施方式】
为对本发明的目的、功能及技术手段有进一步的了解，现结合具体实施例对本发明详细说明如下。
实施例及对比例中所使用的原材料如下：
低粘度玻璃纤维增强聚酰胺树脂为汉达精密电子公司生产，牌号为2273#；
聚酰胺树脂为solvay公司生产，牌号为TH-00T；
扁形玻璃纤维为Nittobo公司生产，牌号为820s；
圆形玻璃纤维为巨石集团生产，牌号为560H；
阻燃剂为Clariant公司生产，牌号为OP1240。
实施例1：
本发明高粘度玻璃纤维增强聚酰胺树脂，按重量百分数计算，其包括如下组分：
将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；称取阻燃剂及加工助剂加入到高速混合机中高速预混；然后将上述低粘度玻璃纤维增强聚酰胺树脂、高速预混得到的混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒，双螺杆挤出机的各区间温度分别为：一区间150～180℃，二区间200～250℃，三区间270～310℃，四区间280～320℃，五区间280～320℃，六区间280～320℃，七区间280～320℃，八区间280～320℃，九区间280～320℃，机头温度为310～340℃。
对比例1：
对比例1与实施例1的不同之处在于：对比例1将实施例1中扁平玻璃纤维换为等重量百分数的圆形玻璃纤维；其余组分及重量百分数均相同，然后用同样的制备方法制备。
实施例2：
本发明高粘度玻璃纤维增强聚酰胺树脂，按重量百分数计算，其包括如下组分：
将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；称取阻燃剂及加工助剂加入到高速混合机中高速预混；然后将上述低粘度玻璃纤维增强聚酰胺树脂、高速预混得到的混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒，双螺杆挤出机的各区间温度分别为：一区间150～180℃，二区间200～250℃，三区间270～310℃，四区间280～320℃，五区间280～320℃，六区间280～320℃，七区间280～320℃，八区间280～320℃，九区间280～320℃，机头温度为310～340℃。
对比例2：
对比例2与实施例2的不同之处在于：对比例2将实施例2中扁平玻璃纤维换为等重量百分数的圆形玻璃纤维；其余组分及重量百分数均相同，然后用同样的制备方法制备。
实施例3：
本发明高粘度玻璃纤维增强聚酰胺树脂，按重量百分数计算，其包括如下组分：
将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；称取阻燃剂及加工助剂加入到高速混合机中高速预混；然后将上述低粘度玻璃纤维增强聚酰胺树脂、高速预混得到的混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒，双螺杆挤出机的各区间温度分别为：一区间150～180℃，二区间200～250℃，三区间270～310℃，四区间280～320℃，五区间280～320℃，六区间280～320℃，七区间280～320℃，八区间280～320℃，九区间280～320℃，机头温度为310～340℃。
对比例3：
对比例3与实施例3的不同之处在于：对比例3将实施例3中扁平玻璃纤维换为等重量百分数的圆形玻璃纤维；其余组分及重量百分数均相同，然后用同样的制备方法制备。
以上各实施例及对比例熔融挤出造粒后，然后在注塑机上注塑成型测试样条，按国家标准GB/T1634-2004测试热变形温度，按国家标准GB/T1040-2006测试拉伸强度及断裂伸长率，按国家标准GB/T9341-2008测试弯曲强度及弯曲模量，按UL-94标准测试阻燃等级，测试结果如表1所示：
表1：实施例与对比例的测试结果
测试项目 实施例1 实施例2 实施例3 对比例1 对比例2 对比例3
HDT℃（1.80MPa） 242 251 256 221 230 235
HDT℃（8.0MPa） 201 204 212 187 193 209
拉伸強度MPa 181 205 216 161 178 195
断裂伸长率％ 1.81 1.62 1.33 1.96 1.85 1.73
弯曲强度MPa 255 280 295 220 232 251
弯曲模量GPa 15.5 16.9 18 13 14.5 15.6
阻燃等级（0.8㎜） V0 V0 V0 V0 V0 V0
通过表1，实施例中采用扁平玻璃纤维与对比例中采用圆形玻璃纤维相比较可得到：
（1）制备后的树脂可达到240℃以上的热变形温度，具有优异的耐高温性能，同时保持了优良的阻燃性，均可达到UL94-V0的等级。
（2）该树脂的热变形温度、拉伸强度、弯曲强度及弯曲模量均得到一定程度的提高。
（3）如果扁平玻璃纤维截面太细，玻璃纤维的纺线有时会比较困难得到，相反如果其截面太粗，由于与树脂的接触面积减少作为增强材料的增强效果会减小，因此，发明人经过悉心研究理想的扁平率为4～6，扁平率在3以上，弯曲模量、弯曲强度及热变形温度可以维持在特别高的水平。
（4）该树脂添加重量百分数为10～50%的扁平玻璃纤维使制备后的成型品不易发生收缩成型不良现象同时强度及流动性也相应的增高。
综上所述，本发明通过添加扁平玻璃纤维提高了树脂的粘度，更加提高了该树脂的耐高温性及力学性能，使其更加广泛应用于汽车、家电产品、娱乐电子及机械设备等领域。
以上所述，本发明的所述实施方案都只能认为是对本发明的说明而不能限制本发明，权利要求书指出了本发明的范围，而所述的说明并未指出本发明的范围，因此，在与本发明的权利要求书相当的含义和范围内的任何改变，都应认为是包括在权利要求书的范围内。

Claims (7)

1.一种高粘度玻璃纤维增强聚酰胺树脂，其特征在于，按重量百分数计算，包括如下组分：
其中，所述低粘度玻璃纤维增强聚酰胺树脂的熔融指数为50～150g/10min，熔点为240～320℃，所述低粘度玻璃纤维增强聚酰胺树脂中的玻璃纤维重量为低粘度玻璃纤维增强聚酰胺树脂重量的30～70％，所述扁平玻璃纤维的截面的短径为0.5～25μm，截面的长径为1.0～250μm，所述扁平玻璃纤维的扁平率为4～6，所述聚酰胺树脂为PA6、PA66、PA6/6T、PA6T、PA6T/6I、PA66/6T中的一种、两种或两种以上的混合物。
2.根据权利要求1所述的高粘度玻璃纤维增强聚酰胺树脂，其特征在于，所述阻燃剂包括主阻燃剂和助阻燃剂。
3.根据权利要求2所述的高粘度玻璃纤维增强聚酰胺树脂，其特征在于，所述主阻燃剂为二乙基次磷酸铝、二乙基次磷酸锌、甲基次磷酸铝、甲基次磷酸锌中的一种、两种或两种以上的混合物。
4.根据权利要求2所述的高粘度玻璃纤维增强聚酰胺树脂，其特征在于，所述助阻燃剂为磷酸三聚氰胺或多磷酸三聚氰胺。
5.根据权利要求4所述的高粘度玻璃纤维增强聚酰胺树脂，其特征在于，所述助阻燃剂为多磷酸三聚氰胺。
6.根据权利要求1所述所述的高粘度玻璃纤维增强聚酰胺树脂，其特征在于，所述加工助剂为润滑剂、抗氧化剂、静电防止剂、扩链剂、紫外线吸收剂、脱模剂及着色剂中的一种、两种或两种以上的混合物。
7.一种制备权利要求1-6中任一项所述的高粘度玻璃纤维增强聚酰胺树脂的方法，其特征在于，该方法包括以下步骤：
(a)将低粘度玻璃纤维增强聚酰胺树脂及聚酰胺树脂于90～110℃的温度下在带有除湿干燥机烘箱中干燥4～8小时；
(b)称取阻燃剂及加工助剂加入到高速混合机中高速预混；
(c)将上述步骤(a)、步骤(b)中混合物及称取的扁平玻璃纤维依次加入到双螺杆挤出机上熔融挤出造粒，双螺杆挤出机的各区间温度分别为：一区间150～180℃，二区间200～250℃，三区间270～310℃，四区间280～320℃，五区间280～320℃，六区间280～320℃，七区间280～320℃，八区间280～320℃，九区间280～320℃，机头温度为310～340℃。
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