CN110883975A - 低粗糙度、高cti值阻燃聚酰胺复合材料的制备方法 - Google Patents
低粗糙度、高cti值阻燃聚酰胺复合材料的制备方法 Download PDFInfo
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Abstract
本申请公开了一种低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,依次包括如下步骤:S1按质量份数准备如下原料:半芳香族聚酰胺30~70份、复合型阻燃剂5~30份、阻燃协效剂2~15份、钛酸钾晶须5~30份、氮化硼晶须5~30份、抗氧剂0.1~5份、润滑剂0.1~5份;S2将上述半芳香族聚酰胺、抗氧剂、润滑剂经高速混合机混合后,经主送料器从双螺杆挤出机主下料口投入,然后将上述复合型阻燃剂、阻燃协效剂混合后经主送料器从所述双螺杆挤出机主下料口投入,将上述钛酸钾晶须、氮化硼晶须分别经振动式送料器从所述双螺杆挤出机第一侧喂料口、第二侧喂料口投入,进行熔融混合挤出造粒。本发明的优点在于制得的复合材相较传统的玻纤增强红磷阻燃PA66材表面粗糙度更低,CTI值更高。
Description
技术领域
本发明涉及工程塑料复合材领域,特别涉及一种低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法。
背景技术
随着科技的发展人类生活的安全性越来越广受社会的关注,为提高电子产品的安全可靠性,特别对于潮湿环境下使用的绝缘材料安全可靠性,高CTI(相对漏电起痕指数)指标愈发重要,尤其是目前电器部件常用的聚酰胺材料领域,当材料表面比较潮湿且有杂物,在较高的电场作用下,材料表面由于碳化形成导电路,最终引起设备短路甚至引发火灾,因此制备具有高CTI值的聚酰胺工程塑料有着十分积极的意义。目前常见的高CTI值聚酰胺材料制备方法为聚酰胺中添加无卤磷氮系阻燃剂,如红磷母粒、三聚氰胺尿酸盐,或无机阻燃剂如氢氧化铝、氢氧化镁或有卤阻燃剂,如溴化聚苯乙烯及相应阻燃协效剂的方式,利用阻燃剂的气相或固相阻燃机理提高材料耐热性,吸收泄漏电流产生的热量,减少游离碳的生成堆积进而减少材料表面闪络放电机会,提高材料CTI值。
现有高CTI值聚酰胺材料存在各种问题,尤其是玻纤增强型阻燃聚酰胺材料,常见如红磷母粒阻燃配方挤出加工时的磷化氢毒性气体及配色局限性问题(黑红色局限),产品表面粗糙度高,CTI值不稳定的问题。
发明内容
本发明采用半芳香族聚酰胺为基体树脂,添加复合型阻燃剂(无卤有机次膦酸盐及磷腈阻燃剂复配型),白色钛酸钾晶须及氮化硼晶须为填充补强材,制得的复合材相较传统的玻纤增强红磷阻燃PA66材表面粗糙度更低,CTI值更高。
为实现上述目的,本发明提供如下技术方案。
本申请实施例公开了一种低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,依次包括如下步骤:
依次包括如下步骤:
S1按质量份数准备如下原料:半芳香族聚酰胺30~70份、复合型阻燃剂5~30份、阻燃协效剂2~15份、钛酸钾晶须5~30份、氮化硼晶须5~30份、抗氧剂0.1~5份、润滑剂0.1~5份;
S2将上述半芳香族聚酰胺、抗氧剂、润滑剂经高速混合机混合后,经主送料器从双螺杆挤出机主下料口投入,然后将上述复合型阻燃剂、阻燃协效剂混合后经主送料器从所述双螺杆挤出机主下料口投入,将上述钛酸钾晶须、氮化硼晶须分别经振动式送料器从所述双螺杆挤出机第一侧喂料口、第二侧喂料口投入,进行熔融混合挤出造粒。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述半芳香族聚酰胺为PA6T、PA9T、PA10T、PA11T、PA12T及其共聚改性物中的一种或多种。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述复合型阻燃剂为二乙基次膦酸铝以及六苯氧基环三磷腈按质量比1∶1~2∶1复配。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述阻燃协效剂为硼酸锌、锡酸锌、三氧化二锑、氧化锌、氧化钙、硫化锌、硫化镁中的一种或多种。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述氮化硼晶须为偶联剂表面处理过的氮化硼纤维,纤维长度为20~50μm,直径为0.1~5μm。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述抗氧剂为IRGANOX 168、1098。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述润滑剂为季戊四醇硬脂酸酯、脂肪族金属盐、有机硅酮粉中的一种或多种。
优选地,在上述低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法中,所述回转式混合机转速为60~120rpm,混合时间为5~10min,所述双螺杆挤出机吐出量为50~200Kg/h,转速为100~300rpm,机筒温度为300±20℃,机头温度为310±10℃,真空段抽出压力为-0.08±0.02MPa。
本发明的优点在于采用半芳香族聚酰胺为基体树脂,添加复合型阻燃剂(无卤有机次膦酸盐及磷腈阻燃剂复配型),白色钛酸钾晶须及氮化硼晶须为填充补强材,制得的复合材相较传统的玻纤增强红磷阻燃PA66材表面粗糙度更低,CTI值更高。
具体实施方式
下面将对本发明实施例中的技术方案进行详细的描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面将采用2组实施例进行示例性说明,并将实施例与典型对比例(PA66/30%GF/红磷)做性能对比。
实施例1与2的制备方法相同,但组分含量不同,制备方法如下:将半芳香族聚酰胺、抗氧剂、润滑剂经高速混合机混合后,经主送料器从双螺杆挤出机主下料口投入,然后将复合型阻燃剂、阻燃协效剂混合后经主送料器从双螺杆挤出机主下料口投入,将钛酸钾晶须、氮化硼晶须分别经振动式送料器从双螺杆挤出机第一侧喂料口、第二侧喂料口投入,进行熔融混合挤出造粒。回转式混合机转速为60~120rpm,混合时间为5~10min,双螺杆挤出机吐出量为50~200Kg/h,转速为100~300rpm,机筒温度为300±20℃,机头温度为310±10℃,真空段抽出压力为-0.08±0.02MPa。
上述制备方法中,半芳香族聚酰胺为PA6T、PA9T、PA10T、PA11T、PA12T及其共聚改性物中的一种或多种。复合型阻燃剂为克莱恩产二乙基次膦酸铝以及大塚化学产六苯氧基环三磷腈按质量比1∶1~2∶1复配。阻燃协效剂为硼酸锌、锡酸锌、三氧化二锑、氧化锌、氧化钙、硫化锌、硫化镁中的一种或多种。钛酸钾晶须为日本大塚化学产TISMO D系列。氮化硼晶须为偶联剂表面处理过的氮化硼纤维,纤维长度为20~50μm,直径为0.1~5μm。抗氧剂为巴斯夫产IRGANOX 168、1098。润滑剂为季戊四醇硬脂酸酯、脂肪族金属盐、有机硅酮粉中的一种或多种。
实施例1与2具体成分组成如下表所示:
将实施例1-2以及典型对比例(PA66/30%GF/红磷)性能做对比,结果如下:
项目 | 实施例1 | 实施例2 | 对比例 |
拉伸强度(MPa) | 125 | 135 | 140 |
弯曲强度(MPa) | 175 | 180 | 190 |
表面粗糙度Ra(μm) | 0.512 | 0.517 | 1.561 |
阻燃等级UL94 1.6mm | V-0 | V-0 | V-0 |
相对漏电起痕指数(V) | 500 | 550 | 450 |
按照本发明制备的复合材性能达到如下,表面粗糙度、CTI值都超过了典型对比例(PA66/30%GF/红磷)。
本实施方式只是对本专利的示例性说明而并不限定它的保护范围,本领域人员还可以对其进行局部改变,只要没有超出本专利的精神实质,都视为对本专利的等同替换,都在本专利的保护范围之内。
Claims (8)
1.一种低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,依次包括如下步骤:
S1按质量份数准备如下原料:半芳香族聚酰胺30~70份、复合型阻燃剂5~30份、阻燃协效剂2~15份、钛酸钾晶须5~30份、氮化硼晶须5~30份、抗氧剂0.1~5份、润滑剂0.1~5份;
S2将上述半芳香族聚酰胺、抗氧剂、润滑剂经高速混合机混合后,经主送料器从双螺杆挤出机主下料口投入,然后将上述复合型阻燃剂、阻燃协效剂混合后经主送料器从所述双螺杆挤出机主下料口投入,将上述钛酸钾晶须、氮化硼晶须分别经振动式送料器从所述双螺杆挤出机第一侧喂料口、第二侧喂料口投入,进行熔融混合挤出造粒。
2.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述半芳香族聚酰胺为PA6T、PA9T、PA10T、PA11T、PA12T及其共聚改性物中的一种或多种。
3.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述复合型阻燃剂为二乙基次膦酸铝以及六苯氧基环三磷腈按质量比1∶1~2∶1复配。
4.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述阻燃协效剂为硼酸锌、锡酸锌、三氧化二锑、氧化锌、氧化钙、硫化锌、硫化镁中的一种或多种。
5.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述氮化硼晶须为偶联剂表面处理过的氮化硼纤维,纤维长度为20~50μm,直径为0.1~5μm。
6.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述抗氧剂为IRGANOX 168、1098。
7.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述润滑剂为季戊四醇硬脂酸酯、脂肪族金属盐、有机硅酮粉中的一种或多种。
8.根据权利要求1所述的低粗糙度、高CTI值阻燃聚酰胺复合材料的制备方法,其特征在于,所述回转式混合机转速为60~120rpm,混合时间为5~10min,所述双螺杆挤出机吐出量为50~200Kg/h,转速为100~300rpm,机筒温度为300±20℃,机头温度为310±10℃,真空段抽出压力为-0.08±0.02MPa。
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