CN103980707B - 韧化聚醚酰亚胺复合材料及其制备方法 - Google Patents
韧化聚醚酰亚胺复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种韧化聚醚酰亚胺复合材料及其制备方法,该韧化聚醚酰亚胺复合材料由以下重量份的原材料配置而成:聚醚酰亚胺树脂88~97份,聚烯烃树脂2~10份和抗氧剂0.5~2份。通过高速配料机将上述原料搅拌混合后置于双螺杆机中熔融后挤出造粒,然后将所得物料浸入冷水中冷却,再用切粒机切粒即成韧化聚醚酰亚胺复合材料。本发明仅需使用较低含量的聚烯烃,就可获得韧化聚醚酰亚胺复合材料,其缺口冲击强度可达到纯聚醚酰亚胺树脂的3倍以上,而且本发明韧化聚醚酰亚胺复合材料的熔体流动性更佳,易注塑成型,并能够较好地保持聚醚酰亚胺的耐热特性,其长期使用温度可以达到170~180℃。
Description
技术领域
本发明的实施方式涉及高分子材料领域,更具体地,本发明的实施方式涉及一种韧化聚醚酰亚胺复合材料及其制备方法。
背景技术
聚醚酰亚胺(PEI)是琥珀色透明固体,密度约在1.28~1.42g/cm3之间,氧指数为47%,燃烧等级为UL94-V-0级,玻璃化转变温度高达215℃左右,在不添加任何添加剂的情况下,就有固有的阻燃性、低烟度和低收缩率。同时,聚醚酰亚胺具有优良的抗拉弯性能、电绝缘性能、耐高低温、耐辐照性能及耐磨性能,可透过微波,可在-160~180℃的工作温度范围内长期使用。由于聚醚酰亚胺具有优良的综合性能,使其卓有成效地应用于电子、电机、医疗器械、武器装备和航空等部门,并可用作传统产品和文化生活用品的金属代用材料。由于聚醚酰亚胺分子中含有大量的苯环结构导致其刚性极强,使得其韧性较差(其表现为缺口冲击强度仅为5~6KJ/m2)。因此,韧化聚醚酰亚胺复合材料的研制有助于改善聚醚酰亚胺的韧性,以可拓宽其应用领域。而目前国内外关于韧化聚醚酰亚胺复合材料的制备方法的文献主要采用合金化技术和弹性体增韧技术。例如,将聚醚酰亚胺在与聚醚醚酮(PEEK),聚酯(PBT)以及聚苯乙烯(PS)等制备成符合材料。例如,Vallejo通过添加10%的PBT树脂,使得PEI/PBT合金材料的屈服应力提高了10%。而GE公司利用弹性体改性聚醚酰亚胺冲击韧性,获得了冲击韧性为纯聚醚酰亚胺树脂2倍以上的聚醚酰亚胺合金材料。而关于改善聚醚酰亚胺复合材料力学性能的专利主要集中在提高其强度。例如,中国专利(申请号:201010606988.8)将聚醚酰亚胺、玻璃纤维、玻璃纤维改性剂和润滑剂进行共混,获得了一种玻璃纤维加入量小、工艺过程易于实现,机械性能显著提高的玻璃纤维增强聚醚酰亚胺复合材料;中国专利(申请号:201010218363.4)利用热致液晶聚合物的剪切变稀的流变特性,有效降低了复合材料加工过程中的熔体黏度,提高了熔体流动速率,进而改善了材料加工性能。同时,热致液晶聚合物在聚醚酰亚胺基体中能够形成微纤结构,提高了聚醚酰亚胺复合材料强度。然而,关于韧化聚醚酰亚胺复合材料的专利报道相对较少。例如中国专利(申请号:201210292129.5)将聚苯醚和聚醚酰亚胺进行共混,通过使用聚苯醚接枝马来酸酐作为相容剂,改善了聚苯醚和聚醚酰亚胺之间的界面相容性,使得聚苯醚和聚醚酰亚胺之间良好相容,获得了一种冲击强度有一定改善、成本较低的聚醚酰亚胺复合材料。
纵观上述文献和专利情况,聚醚酰亚胺的增韧改性的原理主要为弹性粒子增韧和纤维刚性增韧,其使用的增韧剂较多或者增韧效果不太理想,使增韧后的聚醚酰亚胺材料在加工和应用上收到一定的限制,因此需要一种全新的增韧技术来提高聚醚酰亚胺复合材料的的韧性。
发明内容
本发明克服了现有技术的不足,提供一种韧化聚醚酰亚胺复合材料及其制备方法的实施方式,采用一种全新的增韧技术,仅需在较低的增韧剂含量,就可获得了一种韧化度高的聚醚酰亚胺复合材料。
为解决上述的技术问题,本发明的一种实施方式采用以下技术方案:
一种韧化聚醚酰亚胺复合材料,由以下重量份的原材料配置而成:聚醚酰亚胺树脂88~97份,聚烯烃树脂2~10份和抗氧剂0.5~2份。
进一步的技术方案是:所述聚醚酰亚胺树脂的相对密度为1.4,熔点为330~340℃,介电常数为3.8~4.0。
更进一步的技术方案是:所述聚烯烃树脂的相对密度为0.9,熔点为190~220℃,热分解温度为330~350℃。
更进一步的技术方案是:所述抗氧剂为β-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、N,N’-1,6-亚己基-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰胺、三(2,4-二叔丁基苯基)亚磷酸酯中的一种或几种的混合物。
一种韧化聚醚酰亚胺复合材料的制备方法,包括以下步骤:
(1)将聚醚酰亚胺树脂烘干后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合均匀制得预混料;
(2)将所述预混料置于双螺杆机中经熔融后挤出造粒;
(3)将挤出造粒所得的物料浸入水槽中冷却后送入切粒机中切粒即成韧化聚醚酰亚胺复合材料。
进一步的技术方案是:所述聚醚酰亚胺、聚烯烃树脂、抗氧剂的重量之比为(88~97):(2~10):(0.5~2)。
更进一步的技术方案是:所述烘干的温度为130~150℃,烘干时间为4~8小时。
更进一步的技术方案是:所述双螺杆机温度区为:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率20~24Hz、喂料频率22-25Hz;切粒机转速200-400r/min。
与现有技术相比,本发明的有益效果之一是:本发明利用聚酰亚胺树脂加工温度与聚烯烃分解温度的匹配关系(都约为340~350℃),通过聚烯烃的分解产生气压获得了一种微气囊化聚醚酰亚胺/聚烯烃复合材料。在聚醚酰亚胺和聚烯烃二者界面所产生的微气囊极小且均匀分布在聚醚酰亚胺基体中,这些微气囊通过钝化裂纹尖端,增加传播裂纹所需要的能量来阻止裂纹的扩展,以获得了一种韧化聚醚酰亚胺复合材料。本发明仅需使用较低含量的聚烯烃,就可获得韧化聚醚酰亚胺复合材料,其缺口冲击强度可达到纯聚醚酰亚胺树脂的3倍以上。而且本发明韧化聚醚酰亚胺复合材料的熔体流动性更佳,易注塑成型,并能够较好地保持聚醚酰亚胺的耐热特性,其长期使用温度可以达到170~180℃。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
按以下重量配比的原材料配制原料:
本实施例的韧化聚醚酰亚胺复合材料的制备方法如下:
1)配料步骤
将聚醚酰亚胺树脂经130℃,8小时的烘干预处理后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合2分钟,使其混合均匀。
2)挤出步骤
将混合后的预混料置于双螺杆中经熔融挤出造粒,其挤出工艺为:双螺杆机温度区:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率20Hz、喂料频率22Hz;切粒机转速200r/min。双螺杆机温度区的各段温度在该段温度范围值内变动。
将挤出的物料浸入水槽中冷却,送入切粒机中切粒,最后将切好的粒子打包,即制成韧化聚醚酰亚胺复合材料。
实施例2
按以下重量配比的原材料配制原料:
本实施例的韧化聚醚酰亚胺复合材料的制备方法如下:
1)配料步骤
将聚醚酰亚胺树脂经150℃,4小时的烘干预处理后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合2分钟,使其混合均匀。
2)挤出步骤
将混合后的预混料置于双螺杆中经熔融挤出造粒,其挤出工艺为:双螺杆机温度区:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率24Hz、喂料频率25Hz;切粒机转速400r/min。将挤出的物料浸入水槽中冷却,送入切粒机中切粒,最后将切好的粒子打包,即制成韧化聚醚酰亚胺复合材料。
实施例3
按以下重量配比的原材料配制原料:
本实施例的韧化聚醚酰亚胺复合材料的制备方法如下:
1)配料步骤
将聚醚酰亚胺树脂经140℃,6小时的烘干预处理后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合1分钟,使其混合均匀。
2)挤出步骤
将混合后的预混料置于双螺杆中经熔融挤出造粒,其挤出工艺为:双螺杆机温度区:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率22Hz、喂料频率25Hz;切粒机转速350r/min。将挤出的物料浸入水槽中冷却,送入切粒机中切粒,最后将切好的粒子打包,即制成韧化聚醚酰亚胺复合材料。
实施例4
按以下重量配比的原材料配制原料:
本实施例涉及的韧化聚醚酰亚胺复合材料的制备方法如下:
1)配料步骤
将聚醚酰亚胺树脂经135℃,7小时的烘干预处理后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合1分钟,使其混合均匀。
2)挤出步骤
将混合后的预混料置于双螺杆中经熔融挤出造粒,其挤出工艺为:双螺杆机温度区:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率24Hz、喂料频率24Hz;切粒机转速300r/min。将挤出的物料浸入水槽中冷却,送入切粒机中切粒,最后将切好的粒子打包,即制成韧化聚醚酰亚胺复合材料。
实施例5
按以下重量配比的原材料配制原料:
本实施例的韧化聚醚酰亚胺复合材料的制备方法如下:
1)配料步骤
将聚醚酰亚胺树脂经150℃,5小时的烘干预处理后加入高速配料搅拌机中,再加入聚烯烃树脂和抗氧剂混合2分钟,使其混合均匀。
2)挤出步骤
将混合后的预混料置于双螺杆中经熔融挤出造粒,其挤出工艺为:双螺杆机温度区:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率20Hz、喂料频率22Hz;切粒机转速200r/min。将挤出的物料浸入水槽中冷却,送入切粒机中切粒,最后将切好的粒子打包,即制成韧化聚醚酰亚胺复合材料。
以上各实施例所述的韧化聚醚酰亚胺复合材料制备过程中使用的聚醚酰亚胺树脂的相对密度为1.4,熔点为330~340℃,介电常数为3.8~4.0;所述的聚烯烃树脂的相对密度为0.9,熔点为190~220℃,热分解温度为330~350℃。
下表是本发明韧化聚醚酰亚胺复合材料实施例1~5的性能对照表。
尽管这里参照本发明的多个解释性实施例对本发明进行了描述,但是,应该理解,本领域技术人员可以设计出很多其他的修改和实施方式,这些修改和实施方式将落在本申请公开的原则范围和精神之内。更具体地说,在本申请公开和权利要求的范围内,可以对主题组合布局的组成部件和/或布局进行多种变型和改进。除了对组成部件和/或布局进行的变型和改进外,对于本领域技术人员来说,其他的用途也将是明显的。
Claims (3)
1.一种韧化聚醚酰亚胺复合材料的制备方法,其特征在于:包括以下步骤:
(1)按重量份计,将88~97份聚醚酰亚胺树脂烘干后加入高速配料搅拌机中,再加入2~10份聚烯烃树脂和0.5~2份抗氧剂混合均匀制得预混料;
(2)将所述预混料置于双螺杆机中经熔融后挤出造粒;所述双螺杆机温度区为:一段温度330~340℃、二段温度335~345℃、三段温度335~350℃、四段温度340~350℃、五段温度340~345℃、机头温度335~345℃;主机频率20~24Hz、喂料频率22~25Hz;切粒机转速200~400r/min;
(3)将挤出造粒所得的物料浸入水槽中冷却后送入切粒机中切粒即成韧化聚醚酰亚胺复合材料。
2.根据权利要求1所述的韧化聚醚酰亚胺复合材料的制备方法,其特征在于:所述烘干的温度为130~150℃,烘干时间为4~8小时。
3.根据权利要求1所述的韧化聚醚酰亚胺复合材料的制备方法,其特征在于:所述抗氧剂为β-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、N,N’-1,6-亚己基-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰胺、三(2,4-二叔丁基苯基)亚磷酸酯中的一种或几种的混合物。
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