CN112625432B - 一种微发泡尼龙复合材料及其应用 - Google Patents
一种微发泡尼龙复合材料及其应用 Download PDFInfo
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Abstract
本发明提供一种微发泡尼龙复合材料及其应用。本发明的材料包括以下重量份数的组分:尼龙30‑98.5份;超支化聚合物0.5‑5份;发泡剂0.5‑10份;加工助剂0.5‑5份;增强材料0‑35份;填充剂0‑30份;阻燃剂0‑35份;所述的尼龙为高熔点及低熔点尼龙树脂按比例复配得到的共混物。本发明的微发泡尼龙复合材料,通过高熔点及低熔点尼龙树脂复配共混与超支化聚合物的合理设计,规避了不易控制的交联固化手段,实现了减重效果显著、原始性能影响小、尺寸精度高等优点,不受限于特定领域使用,利于推广。本发明的微发泡尼龙复合材料应用于汽车、电子电气、机械仪表等领域。
Description
技术领域
本发明属于微发泡尼龙技术领域,特别涉及一种微发泡尼龙复合材料及其应用。
背景技术
尼龙材料集优异的力学性能、阻隔性能、高低温性能、电性能、耐化学药品性、耐磨性、耐候性及尺寸稳定性等于一身,成型工艺简单且能耗小,已成为发展最快的工程塑料,经常被用于制造各种汽车、电子电器、电动工具等关键结构零部件。微孔发泡材料是一种外部具有坚韧致密表层,内部呈均匀微孔(直径20~200μm)泡沫结构的轻质化新材料,可降低零部件重量,还具有较高刚性、缓冲性、隔热、隔音性能等优点。尼龙属于半结晶型聚合物,当温度超过其熔点,其黏度急剧降低,气体难以被熔体所束缚,容易在基体中塌陷、串泡、并泡,导致泡孔难以控制,限制了尼龙微发泡材料的应用范围。因此如何控制尼龙的发泡行为受到了研究者们的关注。
如专利CN107903620A公开了一种汽车发动机罩盖用微发泡尼龙材料,采用二异氰酸酯、环氧树脂、酯化二内酰胺、噁唑啉等增粘剂提高熔体强度。专利CN108727809A公开了一种中空吹塑尼龙微发泡材料,采用环氧树脂、噁嗪类、咪唑啉类、酯化二内酰胺类等支化剂和聚酯的协同作用,增加了尼龙分子量,改善了材料的抗熔垂性能。专利CN111875871A公开了一种低温改性尼龙弹性体橡塑复合发泡材料,采用了过氧化二异丙苯架桥剂。然而,上述采用增粘剂、支化剂、架桥剂等本质上是交联的手段在极性的尼龙基体中起到了过犹不及的结果,交联固化是提高熔体强度但也抑制了分子链网络的胀大,不利于泡孔长大,实际上难以通过后续温度、压力、剪切等工艺调整,减重效果不明显,因此交联固化手段在尼龙材料中的效果远不及在聚丙烯材料中的发泡效果。
此外,研究者们注意到了聚合物共混角度。如专利CN107201026B公开了一种聚酰胺/丁腈橡胶共混弹性体微孔发泡材料,采用40-80份丁腈橡胶与20-60份聚酰胺,通过辐射交联共混获得微发泡制品。专利CN111138851A公开了一种阻燃增强微发泡尼龙材料,采用了40-65份尼龙与10-20份聚苯硫醚共混,产品阻燃达到UL94 1.6mm以上V0级别。专利CN108264759A公开了一种微发泡注塑尼龙/聚苯醚复合材料,采用了30-80份尼龙与20-65份PPO共混,增加了泡孔密度,提升了刚性、韧性和耐热性。专利CN111087684A公开了一种聚丙烯-尼龙6合金微发泡吸波材料,采用40-80份聚丙烯与5-30份尼龙6共混做成发泡状态。专利CN107163346A公开了一种LDPE/PA6共混二级发泡材料,将20重量份尼龙发泡剂填充在80重量份LDPE中,制备尼龙发泡母料。专利CN108178920A公开了一种轻质、高韧、低吸水率的超高分子量聚乙烯尼龙6微发泡复合材料,采用53-82份PA6与10-30份UHMWPE共混,提高了PA6的熔体强度。专利CN107177090B公开了一种尼龙发泡鞋材及其制作方法,采用30-50%尼龙共聚物与25-45%EVA共混发泡,相比传统的EVA发泡体系,比重降低至50%,拉伸强度提升15%左右。然而,上述方案有的是采用了聚苯硫醚、聚苯醚等树脂,无疑增加了成本;有的是将尼龙作为辅助物引入聚乙烯、聚丙烯、EVA等树脂中,牺牲了尼龙作为主体树脂的特性,且材料热变形温度、力学性能都无法与尼龙材料相比。
再者,研究者们在其它特殊角度也进行了相关研究。周海等人报道了将聚四氟乙烯纤维加入聚丙烯中,在二次开模条件下注塑成型制备出聚丙烯/聚四氟乙烯纤维微发泡复合材料,提高了拉伸强度、弯曲强度、缺口冲击强度和耐热性。专利CN104877236B公开了一种辐射交联聚丙烯泡沫塑料及其连续生产方法,采用辐射可控交联提高了PP熔体强度,消除了化学交联引发剂易残留对产品性能的影响,实现了工业化批量生产。专利CN108250728B公开了一种聚合物/石墨烯气凝胶复合泡沫材料,以石墨烯气凝胶为骨架,热塑性聚合物附着在石墨烯气凝胶的三维网络结构上,热塑性聚合物上具有闭孔结构的泡孔,该复合泡沫材料具有相互连通的三维网络结构。专利CN107868344B公开了一种轻量化聚丙烯微发泡复合材料,采用阴离子表面活性剂处理后的海泡石纤维,获得了小而细腻的泡孔。专利CN111087684A公开了一种聚丙烯-尼龙6合金微发泡吸波材料,采用铁纤维、镍纤维、钻纤维等多晶金属纤维在聚丙烯-尼龙6基体中形成三维网状结构,显著提高聚丙烯机械性能及熔体强度,达到优异的吸波屏蔽效果。然而,上述方案仅限于特定领域使用,有的仅在聚丙烯树脂中适合,在尼龙树脂中效果未知;有的组分比重极大,不利于轻量化;有的成本高昂,不利于推广。
发明内容
为解决以上问题,本发明提供一种微发泡尼龙复合材料及其制备方法,通过高熔点及低熔点尼龙树脂复配共混与超支化聚合物的合理设计,规避了不易控制的交联固化手段,实现了减重效果显著、原始性能影响小、尺寸精度高等优点,不受限于特定领域使用,利于推广。
为实现上述目的,本发明采用如下技术方案:
一种微发泡尼龙复合材料,包括以下重量份数的组分:
尼龙30-98.5份;
超支化聚合物0.5-5份;
发泡剂0.5-10份;
加工助剂0.5-5份;
增强材料0-40份;
填充剂0-30份;
阻燃剂0-35份。
所述尼龙为高熔点及低熔点尼龙树脂按比例复配得到的共混物。
其中,尼龙树脂复配得到的共混物经熔融混合均匀后可被DSC检测到一个以上熔融峰;优选的,不同熔融峰温度相差大于10℃。
其中,尼龙为PA66、PA56、PA6、PA66与PA6共聚物、PA6与PA66共聚物、PA612、PA11、PA12、PA1212中的两种或以上的组合。
所述超支化聚合物包括超支化聚酰胺、超支化聚酯、超支化聚醚或超支化聚苯中的一种或多种。
所述发泡剂为碳酸盐、偶氮化合物、对甲苯磺酰类化合物、酰肼类化合物、亚硝基化合物中的一种或几种,包括实质为以上成分的粉末、压缩颗粒、微胶囊、微球、母粒等形态。
所述加工助剂,包括润滑剂、稳定剂、增韧剂、颜色添加剂中的一种或几种混合物。
所述增强纤维,包括玻璃纤维(GF)、芳纶纤维(AF)、碳纤维(CF)、玄武岩纤维(BF)中的一种或多种。
所述填充剂,包括硅灰石、玻璃微珠、硫酸镁晶须、滑石粉、碳酸钙、木粉的一种或多种。
所述阻燃剂,包括卤系阻燃剂、氮系阻燃剂、磷酸盐系阻燃剂的一种。
上述的微发泡尼龙复合材料应用于汽车、电子电气、机械仪表等领域。
与现有技术相比,本发明具有的有益效果:
1)采用两种以上熔点的尼龙基体树脂复配:
首先,拓宽了熔融加工窗口,赋予材料在不同温度和剪切梯度下都具备合适的熔体强度,规避了以往常规采用增粘剂、交联剂、扩链剂等提高熔体强度时会导致泡孔难以长大的弊端,保障泡孔在合适的工艺配合下可控长大;
其次,利用加工温度下高低熔点组分尼龙的粘度不匹配性,加速剪切流动中分散体的旋流以产生更进一步的缠结作用,可通过注塑工艺调整剪切作用强弱来调整熔体强度可控;
再者,一方面利用高熔点组分实现熔体强度可控,从而调控泡孔尺寸和形态;另一方面利用低熔点组分的低结晶温度特点,提升材料成型后冷却过程中的应***化,保证泡孔薄壁在内压作用下不形变坍塌;
2)采用超支化聚合物作为发泡助剂,不仅有利于发泡剂在物料中充分混合分散,创造更多的微孔成核点,而且有助于改善制品外观;
3)本发明制备的微发泡尼龙复合材料具备减重效果显著、原始性能影响小(力学性能保持率高、热学性能衰减小、阻燃性能不受影响等)、尺寸精度高等优点,不受限于特定领域使用,适合各种不同的尼龙用复合材料使用场景的应用。如采用本发明制备的增强微发泡尼龙材料在产品整体减重16%的情况下,强度保留超过91%,适合在汽车发动机罩盖、减震支架、降噪隔板等场所应用;而且,本发明制备的阻燃微发泡尼龙材料具备了阻燃等级V0、减重9%、隔热、降噪减震等功能,实现了在新能源汽车电池模组、工控断路器面板等重要零件的应用。
4)本发明提供的该材料的制备方法,工艺调整窗口大、泡孔可控,生产成本低,效率高、易于实现工业化。
附图说明
图1是本发明中的发泡尼龙材料产品截面显微图片;
图2是现有技术中尼龙发泡产品截面显微图片;
具体实施方式
为使本发明的技术方案更加清晰明确,下面对本发明进行进一步描述,任何对本发明技术方案的技术特征进行等价替换和常规推理得出的方案均落入本发明保护范围。
本发明的实施例采用下列物料:
PA66:EP1106,华峰集团
PA6:MF800,江苏瑞美福
PA6/66:HYG-2500E,江苏海阳化纤
PA1012:山东东辰工程塑料
玻璃纤维:568H,巨石集团
碳纤维:TR06NL,日本三菱
超支化聚酯:C100,武汉超支化树脂科技
超支化聚酰胺:HPN202,武汉超支化树脂科技
发泡剂:RA发泡剂,市售
发泡剂:EB207母粒,日本永和化成
发泡剂:980MB 120微球母粒,阿克苏诺贝尔
润滑剂:Licowax OP蜡,瑞士科莱恩
稳定剂:H10,布吕格曼
溴化聚苯乙烯:山东兄弟科技
三氧化二锑:闪星锑业
表1采用上述方式制备得到的微发泡尼龙复合材料各组分配比(重量份)如下:
产品性能测试方法:
零件克重:公司内部小型发动机罩盖验证模具,厚度约2.3~3.5mm;
拉伸性能:零件上取样,按ISO527-2方法,样条尺寸:170*10mm;
弯曲性能:零件上取样,按ISO178-1方法,样条尺寸:80*10mm;
缺口冲击性能:零件上取样,按ISO 180方法,样条尺寸:80*10mm;
阻燃等级:零件上取样,按UL94方法,样条尺寸:127*12.7mm;
发泡效果评价:TipScope显微相机,零件脆断截面拍照;
表面外观评价:零件表面目视;
表2采用上述方式制备得到的微发泡尼龙复合材料性能测试结果如下:
从实施例4与对比例1来看,本发明制备的增强微发泡尼龙材料在产品整体减重16%的情况下,强度保留超过91%,适合在汽车发动机罩盖、减震支架、降噪隔板等场所应用。而不含超支化聚合物的对比例1虽然也有完整的泡孔结构,但是泡孔密度小,减重率低,并且在与化学发泡剂的配合中外观较差。
从实施例7与对比例2来看,常规溴系阻燃产品阻燃效果好,但是阻燃剂比重大,本发明制备的阻燃微发泡尼龙材料具备了阻燃等级V0、减重9%、强度保留超过95%,且具备隔热、降噪减震等功能,非常适合在新能源汽车电池模组、工控断路器面板等重要零件的阻燃和轻量化应用。
对比例3在成型窗口(±10℃的温度波动是大部分工厂都认可的机台管控范围)下波动大,量产困难(温度高10℃材料流涎,温度低10℃材料堵浇口无法成型),由于泡孔破裂并孔严重,并孔大孔多,虽然具有较大的减重率,但是性能下降程度大,已不能满足工况使用。
以上所述仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,不论闭模发泡、开模发泡、化学发泡、物理发泡等工艺,还是注塑、挤出、吹塑成型等制备方法,任何熟悉本领域的技术人员根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种微发泡尼龙复合材料,其特征在于:包括以下重量份数的组分:
尼龙30-98.5份;
超支化聚合物0.5-5份;
发泡剂0.5-10份 ;
加工助剂0.5-5份 ;
增强材料0-40份 ;
填充剂0-30份;
阻燃剂0-35份;
所述尼龙为高熔点及低熔点尼龙树脂按比例复配得到的共混物;尼龙树脂复配得到的共混物经熔融混合均匀后可被DSC检测到一个以上熔融峰;且不同熔融峰温度相差大于10℃;所述超支化聚合物包括超支化聚酰胺、超支化聚酯中的一种或两种;所述发泡剂为碳酸盐、偶氮化合物、对甲苯磺酰类化合物、酰肼类化合物、亚硝基化合物中的一种或几种。
2.根据权利要求1所述的一种微发泡尼龙复合材料,其特征在于:尼龙为PA66、PA56、PA6、PA66与PA6共聚物、PA6与PA66共聚物、PA612、PA11、PA12、PA1212中的两种或以上的组合。
3.根据权利要求1所述的一种微发泡尼龙复合材料,其特征在于:所述发泡剂包括实质为以上成分的粉末、压缩颗粒、微胶囊、微球、母粒形态。
4.根据权利要求1所述的一种微发泡尼龙复合材料,其特征在于:所述加工助剂,包括润滑剂、稳定剂、增韧剂、颜色添加剂中的一种或几种混合物。
5.根据权利要求1所述的一种微发泡尼龙复合材料,其特征在于:所述增强纤维选自玻璃纤维(GF)、芳纶纤维(AF)、碳纤维(CF)、玄武岩纤维(BF)中的一种或多种。
6.根据权利要求1所述的一种微发泡尼龙复合材料,其特征在于:所述填充剂选自硅灰石、玻璃微珠、硫酸镁晶须、滑石粉、碳酸钙、木粉的一种或多种;
所述阻燃剂选自卤系阻燃剂、氮系阻燃剂、磷酸盐系阻燃剂的一种。
7.根据权利要求1-6任意之一所述的一种微发泡尼龙复合材料,其特征在于:所述的微发泡尼龙复合材料应用于汽车、电子电气、机械仪表领域。
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