CN103740102B - 一种导电尼龙复合材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种导电尼龙复合材料及其制备方法。导电尼龙复合材料按重量百分比由以下组分组成:PA121282-90%;石墨烯1-5%;抗氧剂0.1-1%;偶联剂0.5-1%;增韧剂8-13%;硅油0.5-1%。本发明的偶联剂可以很好地提高石墨烯与树脂相容性.增韧剂的加入提高了材料的韧性,少量的石墨烯就能够做到导电。本发明的导电尼龙复合材料导电率高、韧性好、制备过程简单,生产工艺容易控制。
Description
[技术领域]
本发明涉及高分子材料领域,尤其涉及一种导电尼龙复合材料及其制备方法。
[背景技术]
长碳链尼龙具备的性能比传统的PA6和PA66有更好的尺寸稳定性,以及优越的耐化学腐蚀性,传统的导电尼龙材料,通常会添加一些导电石墨或者是析出型的导电剂,但是PA6和PA66要做到导电,不仅石墨或者是析出型的导电剂添加量大,而且对PA6和PA66材料的性能影响也大,特别是冲击强度方面会削弱很多,材料会非常脆。
[发明内容]
本发明要解决的技术问题是提供一种具有导电率高、韧性好的导电尼龙复合材料及其制备方法。
为了解决上述技术问题,本发明采用的技术方案是,一种导电尼龙复合材料,其特征在于,按重量百分比由以下组分组成:
根据权利要求1所述的导电尼龙复合材料,其特征在于,所述的石墨烯为南京先锋的羧基化石墨烯粉末。
根据权利要求1所述的导电尼龙复合材料,其特征在于,偶联剂为南京向前化工的KH-550,纯度≥97%。
根据权利要求1所述的导电尼龙复合材料,其特征在于,所述的增韧剂为POE接枝马来酸酐,接枝率为0.8%。
根据权利要求1所述的导电尼龙复合材料,其特征在于,所述的抗氧剂为N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺,熔点110-125摄氏度。
一种权利要求1所述导电尼龙复合材料的制备方法,其特征在于,包括以下步骤:
1)按上述的重量百分比称取原料;
2)将PA1212与硅油在混合器中混合3-7分钟;
3)将步骤2)中混合好的PA1212与硅油混合物与偶联剂、增韧剂、抗氧剂、石墨烯在混合器中混合3-7分钟;
4)将步骤3)中混合好的原料投置于双螺杆挤出机中,经过熔融挤出,造粒。生产工艺条件为:双螺杆挤出机一区温度为180-220℃,二区温度为180-220℃,三区温度为180-220℃,四区温度为180-220℃,混合料在螺杆中输送时间为1-2分钟。
本发明的偶联剂可以很好地提高石墨烯与树脂相容性.增韧剂的加入提高了材料的韧性,少量的石墨烯就能够做到导电,本发明的导电尼龙复合材料导电率高、韧性好、制备过程简单,生产工艺容易控制。
[具体实施方式]
下面通过实施例对本发明进行进一步阐述:
本发明提供的一种导电尼龙复合材料,其组成按重量百分比为:
PA1212 82-90%;石墨烯 1-5%;偶联剂KH-550 0.1-1%;增韧剂POE-MAH 8-13%;抗氧剂 10100.1-1%;硅油0.5-1%;
其中,PA1212为山东东辰AIVS01。其冲击强度(ASTM D256)为25KJ/M3。
抗氧剂为北京极易化工的N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺1010,熔点110-125摄氏度。
偶联剂为南京向前化工的KH-550,其纯度为≥97%。
增韧剂为自制的POE接枝马来酸酐,接枝率为0.8%。POE接枝马来酸酐的制备方法为:将如下重量百分比的各组分混合,用双螺杆挤出机在温度为140-200℃的条件下挤出:
石墨烯为南京先锋的羧基化石墨烯粉末XF004
硅油为普通硅油。
本发明中PA1212和石墨烯的硅氧烷偶联剂,能够很好提高无机与有机物的相容性,而且能够起到添加量小,却能达到高效的导电系数
其制造过程如下:
1)按上述的重量百分比称取原料;
2)将PA1212与硅油在混合器中混合3-7分钟;
3)将步骤2)中混合好的PA1212与硅油混合物与偶联剂、增韧剂、抗氧剂、石墨烯在混合器中混合3-7分钟;
4)将步骤3)中混合好的原料投置于双螺杆挤出机中,经过熔融挤出,造粒。生产工艺条件为:双螺杆挤出机一区温度为180-220℃,二区温度为180-220℃,三区温度为180-220℃,四区温度为180-220℃,混合料在螺杆中输送时间为1-2分钟。
下面结合具体实施例对本发明作详细的描述:
实施例1
PA121286.9%;石墨烯1%;偶联剂KH-5500.5%;增韧剂POE-MAH10%;抗氧剂10100.1%;硅油0.5%;
先添加硅油与PA1212充分混合均与,使硅油很好地附于PA1212表面,然后再添加石墨烯粉和其它原料混合,使得石墨烯能够均匀的分散在树脂中。
经过熔融温度为200-260℃双螺杆挤出机挤出,造粒。
其中各区段温度为:一区180℃,二区200℃,三区220℃,四区220℃,五区220℃,停留时间为90秒钟。
实施例2
PA121284.9%;石墨烯2%;偶联剂KH-5500.5%;增韧剂POE-MAH10%;抗氧剂10100.1%;硅油0.5%;
先添加硅油与PA1212充分混合均与,使硅油很好地附于PA1212表面,然后再添加石墨烯粉和其它原料混合,使得石墨烯能够均匀的分散在树脂中。
经过熔融温度为200-260℃双螺杆挤出机挤出,造粒。
其中各区段温度为:一区180℃,二区200℃,三区220℃,四区220℃,五区220℃,停留时间为90秒钟。
实施例3
PA121282.9%;石墨烯3%;偶联剂KH-5500.5%;增韧剂POE-MAH10%;抗氧剂10100.1%;硅油0.5%;
先添加硅油与PA1212充分混合均与,使硅油很好地附于PA1212表面,然后再添加石墨烯粉和其它原料混合,使得石墨烯能够均匀的分散在树脂中。
经过熔融温度为200-260℃双螺杆挤出机挤出,造粒。
其中各区段温度为:一区180℃,二区200℃,三区220℃,四区220℃,五区220℃,停留时间为90秒钟。
实施例4
PA121280.9%;石墨烯4%;偶联剂KH-5500.5%;增韧剂POE-MAH10%;抗氧剂10100.1%;硅油0.5%;
先添加硅油与PA1212充分混合均与,使硅油很好地附于PA1212表面,然后再添加石墨烯粉和其它原料混合,使得石墨烯能够均匀的分散在树脂中。
经过熔融温度为200-260℃双螺杆挤出机挤出,造粒。
其中各区段温度为:一区180℃,二区200℃,三区220℃,四区220℃,五区220℃,停留时间为90秒钟。
实施例5
PA121283.9%;石墨烯1%;偶联剂KH-5501%;增韧剂POE-MAH13%;抗氧剂10100.1%;硅油1%;
先添加硅油与PA1212充分混合均与,使硅油很好地附于PA1212表面,然后再添加石墨烯粉和其它原料混合,使得石墨烯能够均匀的分散在树脂中。
经过熔融温度为200-260℃双螺杆挤出机挤出,造粒。
其中各区段温度为:一区180℃,二区200℃,三区220℃,四区220℃,五区220℃,停留时间为90秒钟。
性能测试:
将上述5个实施例完成造粒的粒子在80-100℃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/T1040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/min;
弯曲强度和弯曲模量按GB9341/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/min;
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;
塑胶抗静电(导电系数)测试按GB/T15662-1995标准进行测试。表1:实施例1-5的配方表
组分(重量百分比) | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
PA1212 | 87.9 | 86.9 | 85.9 | 84.9 | 83.9 |
石墨烯 | 1 | 2 | 3 | 4 | 1 |
增韧剂 | 10 | 10 | 10 | 10 | 13 |
偶联剂 | 0.5 | 0.5 | 0.5 | 0.5 | 1 |
抗氧剂 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
硅油 | 0.5 | 0.5 | 0.5 | 0.5 | 1 |
表2:实施例1-5的能见表
性能 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
缺口冲击强度(J/M) | 600 | 625 | 665 | 668 | 690 |
拉伸强度(MPa) | 36 | 35 | 40 | 43 | 42 |
弯曲强度(MPa) | 45 | 43 | 48 | 47 | 46 |
导电系数(Ω·m) | 106 | 104 | 103 | 102 | 102 |
弯曲模量(MPa) | 1320 | 1600 | 1585 | 880 | 1450 |
石墨烯目前是世上最薄却也是最坚硬的纳米材料,它几乎是完全透明的,只吸收2.3%的光;导热系数高达5300W/m·K,高于碳纳米管和金刚石,常温下其电子迁移率*超过15000cm²/V·s,又比纳米碳管或硅晶体*高,而电阻率只约10-6Ω·cm,比铜或银更低,为目前世上电阻率最小的材料
通过对上述表格中的数据分析后得知,石墨烯的添加对复合材料的整体性能有一定的提升效果,特别是冲击强度,原因主要还是石墨烯本色的纳米结构,从而对整体的复合材料性能有一定的提升作用,从导电系数来看,石墨烯一般添加1%就已经达到了一个抗静电效果,相对于导电石墨来说,已经大大减少了添加比例,随着石墨烯添加比例的增加,导电系数也提升,当添加比例大于等于2%的时候,整体材料就已经可以达到导电效果,因此,石墨烯填充PA1212对材料的性能不仅有提升作用,而且也赋予了很好的导电效果。
本发明以上实施例中的硅氧烷的偶联剂可以很好地提高石墨烯与树脂相容性.石墨烯添加之前,先添加一定量的硅油与树脂充分混合均与,做到硅油能够很好的附于树脂表面,然后再添加石墨烯粉,使得石墨烯能够均匀的分散在树脂中。自制增韧剂的加入直接提高了材料的韧性。PA1212本来材料的冲击就非常的优越,而且吸水率低,对一些尺寸要求高的产品也适合,只要添加少量的石墨烯就能够做到导电,由于石墨烯属于纳米级别的,因此添加后不仅对材料的性能没有降低,反而在冲击强度方面可以得到提高。
以上对本发明所提供的一种石墨烯填充PA1212的复合导电材料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,本说明书内容不应理解为对本发明的限制。
Claims (5)
1.一种导电尼龙复合材料,其特征在于,按重量百分比由以下组分组成:
各组分之和为100%;增韧剂为POE接枝马来酸酐,接枝率为0.8%;POE接枝马来酸酐的制备方法为:将如下重量百分比的各组分混合,用双螺杆挤出机在温度为140-200℃的条件下挤出:
2.根据权利要求1所述的导电尼龙复合材料,其特征在于,所述的石墨烯为南京先锋的羧基化石墨烯粉末。
3.根据权利要求1所述的导电尼龙复合材料,其特征在于,偶联剂为南京向前化工的KH-550,纯度≥97%。
4.根据权利要求1所述的导电尼龙复合材料,其特征在于,所述的抗氧剂为N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺,熔点110-125摄氏度。
5.一种权利要求1所述导电尼龙复合材料的制备方法,其特征在于,包括以下步骤:
1)按权利要求1所述的重量百分比称取原料;
2)将PA1212与硅油在混合器中混合3-7分钟;
3)将步骤2)中混合好的PA1212与硅油混合物与偶联剂、增韧剂、抗氧剂、石墨烯在混合器中混合3-7分钟;
4)将步骤3)中混合好的原料投置于双螺杆挤出机中,经过熔融挤出,造粒;生产工艺条件为:双螺杆挤出机一区温度为180-220℃,二区温度为180-220℃,三区温度为180-220℃,四区温度为180-220℃,混合料在螺杆中输送时间为1-2分钟。
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