CN114456585A - 一种长期耐热聚酰胺组合物及其制备方法 - Google Patents
一种长期耐热聚酰胺组合物及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种长期耐热聚酰胺组合物及其制备方法,包括聚酰胺、抗氧剂、黑种和其它助剂。本发明通过添加复配的抗氧体系,可以改善材料长期耐热后的拉伸强度和断裂伸长率保持率;同时,材料长期耐热后的颜色稳定性也得到了改善。
Description
技术领域
本发明属于工程塑料领域,特别涉及一种长期耐热聚酰胺组合物及其制备方法。
背景技术
聚酰胺是一种常见的工程塑料,用途广泛。在一些传统的注塑、挤出等产品中都有比较成熟的产品。随着各行业的发展,对于终端产品的功能性、泛用性等的要求逐渐提到,因此对于原材料的综合性能也提出了更高的要求。在聚酰胺的所有应用中,挤出产品占据了超过50%,然而由于高分子材料本身的特性,长时间受热状态下,大分子容易产生分解,导致分子量下降,进而影响材料的强度、断裂伸长率等。
在实际应用中,常采用抗氧剂,尤其是铜盐,作为改善聚酰胺长期耐热性能。然而铜盐本身仍然会导致一些问题,比如铜离子导致的电荷屏蔽能力下降、铜离子氧化变色等。
镍元素和铜同属于d区的过渡金属,其化合物也在聚酰胺改性中有应用。专利CN106280431A中使用镍粉作为填充剂,增强了材料电镀的结合力,解决了尼龙不易电镀和电镀后结合力较差的问题。
发明内容
本发明所要解决的技术问题是提供一种长期耐热聚酰胺组合物及其制备方法,该组合物通过添加复配的抗氧体系,可以改善材料长期耐热后的拉伸强度和断裂伸长率保持率;同时,材料长期耐热后的颜色稳定性也得到了改善。
本发明提供了一种长期耐热聚酰胺组合物,按质量份数,包括如下组分:
其中,所述抗氧剂为铜盐抗氧剂和次磷酸镍的复配物。
所述聚酰胺为一种或多种氨基酸聚合,或者内酰胺开环聚合获得的均聚产物,包括但不限于PA6、PA11、PA12等;或者是通过缩聚一种或多种二元羧酸和二元胺的聚合物,包括但不限于PA46、PA56、PA66、PA610、PA612、PA6T、PA9T、PA10T、PA1010、PA1012等;亦或是上述聚酰胺的两种或两种以上的混合物或共聚物。
优选的,所述聚酰胺按照ISO 307-2007标准,使用96%浓度硫酸,测试的特性粘数在100-200mL/g范围内。
所述铜盐抗氧剂和次磷酸镍的质量比为(1-9):(1-9)。优选的,所述质量比为(3-7):(3-7)。
优选的,所述铜盐抗氧剂包括质量比为1:(3-20)、优选质量比为1:(5-10)范围内的铜化合物和碱金属卤化物。该铜化合物不限于以下:氧化亚铜(I)、氧化铜(II)、亚铜(I)盐,例如乙酸亚铜、硬脂酸亚铜、乙酰丙酮酸铜、卤化亚铜等。其中优选卤化亚铜,例如碘化亚铜、溴化亚酮、氯化亚铜等。进一步优选为碘化亚铜。所述碱金属卤化物为Li、Na、和K的碘化物和/或溴化物中的一种或一种以上的组合。
所述黑种为炭黑或者炭黑质量分数在10-60%范围内的炭黑母粒,其中炭黑母粒添加量按照实际炭黑含量计算。
优选的,所述黑种的添加量为1-2份。
所述其它助剂包含热稳定剂、润滑剂中的一种或几种。
所述热稳定剂为酚类热稳定剂、胺类热稳定剂中的一种或几种;所述润滑剂为高级脂肪酸酯、高级脂肪酸及其金属盐、高级脂肪酸酰胺、硅酮中的一种或几种。
本发明还提供了一种长期耐热聚酰胺组合物的制备方法,包括:
按质量份数,将组分混合加入到双螺杆挤出机中混炼、熔融、均化后挤出造粒,挤出温度220-260℃,得到长期耐热聚酰胺组合物。
本发明还提供了一种长期耐热聚酰胺组合物在汽车产品中的应用。
有益效果
本发明通过添加复配的抗氧体系,铜盐抗氧剂和次磷酸镍复配具有协效作用:加工过程中和较低老化温度下,次磷酸镍对聚酰胺树脂的还原性更强,其在老化前期发挥保护作用;较高老化温度和老化时间较长的情况下,铜盐抗氧剂对基体聚酰胺树脂发挥保护作用更明显、更有效。两种抗氧剂产生良好的协同效果,共同提升了材料整体的长期耐热能力。
针对聚酰胺材料在加工、使用过程中,容易受到热、光、射线及强剪切作用而发生分解老化的问题,本发明通过铜盐抗氧剂和次磷酸镍复配作为聚酰胺材料的混合抗氧剂,再通过添加一定配比的黑种和助剂,并且通过优化其配比和用量,可以改善材料长期耐热后的拉伸强度和断裂伸长率保持率;同时,材料长期耐热后的颜色稳定性也得到了改善。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例和对比例所用原料来源如下:
聚酰胺树脂1:牌号为PA6 HY-2800A,特性粘数在180mL/g左右,江苏海阳化纤;
聚酰胺树脂2:牌号为PA6 HY2500A,特性粘数在150mL/g左右,江苏海阳化纤;
抗氧剂A:次磷酸镍,湖北弘景;
铜盐抗氧剂B1:H320,其中碘化亚铜和碘化钾的质量比约为1:8,布吕格曼;
铜盐抗氧剂B2:H328F,其中碘化亚铜和溴化钾的质量比约为1:7,布吕格曼;
助剂C1:钛酸镍,市售;
助剂C2:氯化钙,市售;
黑种1:M717,100%炭黑,卡博特;
黑种2:炭黑黑种PE2772,其中炭黑比例约50%,卡博特;
润滑剂:硬脂酸盐类润滑剂,市售。
实施例和对比例均使用相同的上述市售产品。
实施例和对比例制备方法包括:
按照重量份数,将组分混合加入到双螺杆挤出机中混炼、熔融、均化后挤出造粒,挤出温度220-260℃,得到长期耐热聚酰胺组合物。
材料性能与测试方法:
(1)拉伸强度,断裂伸长率:按照ISO 527-2-2012标准,将样料注塑成1A型拉伸样条进行测试。分别记录老化前、180℃老化1000h和180℃老化1600h后的拉伸强度与断裂伸长率,测试条件:10mm/min,23℃。
(2)色差测量方法:将所有样料分别注塑成尺寸不小于30mm×30mm的表面光亮的方板,使用台式分光光度仪,按照GB/T 7921-2008标准计算方板高温老化前后的ΔE,计算公式为:△E=[(△L)2+(△a)2+(△b)2]1/2。
表1
表2
通过表1和表2可以发现,通过添加一定比例的次磷酸镍和铜盐抗氧剂,材料高温老化后的拉伸强度和断裂伸长率保持率都有明显提升。并且相对于单独使用,次磷酸镍和铜盐抗氧剂复配使用可以进一步提升材料的长期耐热性能,表现出协同效果。并且进一步的研究发现,次磷酸镍和黑种复配使用,可以有效改善材料180℃长期加热后的颜色稳定性。
Claims (10)
2.根据权利要求1所述的组合物,其特征在于:所述聚酰胺为PA6、PA11、PA12、PA46、PA56、PA66、PA610、PA612、PA6T、PA9T、PA10T、PA1010、PA1012中的一种或几种。
3.根据权利要求1所述的组合物,其特征在于:所述铜盐抗氧剂和次磷酸镍的质量比为(1-9):(1-9)。
4.根据权利要求1或3所述的组合物,其特征在于:所述铜盐抗氧剂包括质量比为1:(3-20)的铜化合物和碱金属卤化物。
5.根据权利要求1所述的组合物,其特征在于:所述黑种为炭黑或者炭黑质量分数在10-60%范围内的炭黑母粒。
6.根据权利要求1所述的组合物,其特征在于:所述黑种的添加量为1-2份。
7.根据权利要求1所述的组合物,其特征在于:所述其它助剂包含热稳定剂、润滑剂中的一种或几种。
8.根据权利要求7所述的组合物,其特征在于:所述热稳定剂为酚类热稳定剂、胺类热稳定剂中的一种或几种;所述润滑剂为高级脂肪酸酯、高级脂肪酸及其金属盐、高级脂肪酸酰胺、硅酮中的一种或几种。
9.一种如权利要求1-8任一所述的长期耐热聚酰胺组合物的制备方法,其特征在于:
按质量份数,将组分混合加入到双螺杆挤出机中混炼、熔融、均化后挤出造粒,挤出温度220-260℃,得到长期耐热聚酰胺组合物。
10.一种如权利要求1所述的长期耐热聚酰胺组合物在汽车、电子电气、建筑材料等产品中的应用。
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