CN103709742A - 一种改性芳纶纤维增强pa66材料及其制备方法 - Google Patents

一种改性芳纶纤维增强pa66材料及其制备方法 Download PDF

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CN103709742A
CN103709742A CN201210369747.5A CN201210369747A CN103709742A CN 103709742 A CN103709742 A CN 103709742A CN 201210369747 A CN201210369747 A CN 201210369747A CN 103709742 A CN103709742 A CN 103709742A
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CN103709742B (zh
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穆兴文
宋阳
宫克难
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Heilongjiang Xinda Enterprise Group Co Ltd
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Abstract

本发明涉及一种改性芳纶纤维增强PA66材料及其制备方法。芳纶纤维先经微波辐射改性，辐射频率为0.5～5GHZ，辐射剂量为0.1～2mW/cm2，辐射时间为1～240S；然后用低温等离子体处理，处理功率为10～400W，处理气氛为5～15%氢气、5～15%氟气和70～90%氦气，处理腔体内的气体压强为10～106Pa，处理温度为0～150℃，处理时间为1～20min。微波辐射改性后的芳纶纤维表皮层与芯层发生交联，提高了纤维的横向抗拉强度；低温等离子改性后，芳纶纤维表面变得粗糙而且表面富含活性自由基和官能团。此方法改性后的芳纶纤维与PA66树脂通过双螺杆挤出机共混挤出制备的复合材料，其力学、耐磨性能比国外同类产品高15～20%，可以满足高速铁路、航空航天等领域对高性能耐磨部件的要求。

Description

一种改性芳纶纤维增强PA66材料及其制备方法
技术领域
本发明涉及高分子材料领域，具体涉及一种改性芳纶纤维增强PA66材料及其制备方法。
背景技术
芳纶纤维全称为芳香族聚酰胺纤维，它具有比强度高、比模量高、密度小、耐高温、韧性高和高耐磨等优点。由于其优异的性能，使其在航空航天、军事装备、建筑、交通、通讯电缆等领域得到了广泛的应用。
PA66全称聚己二酸己二胺，是工程塑料中应用最广泛的材料之一。PA66与芳纶纤维都属于聚酰胺类，从两者的分子结构上分析，芳纶纤维与PA66应具有较好的相容性。但是，芳纶纤维表面光滑、缺少活性基团，致使其与PA66的复合材料的界面粘结较弱，严重影响芳纶纤维增强PA66复合材料的各项性能。芳纶纤维单丝由表皮和芯两部分组成：表皮厚度约占整个纤维直径的1～10%，由结晶程度较高的刚性分子链沿纤维轴向排列而成；芯部由许多靠氢键连接的棒状分子构成。由于芳纶纤维这一独特的结构，导致一旦纤维表皮被破坏，整个纤维的力学性能急剧下降，影响芳纶纤维增强复合材料的整体力学性能，给芳纶纤维的表面改性带来了困难。
芳纶纤维表面改性方法包括化学改性和物理改性：化学改性反应速度快，很难控制反应仅在纤维表皮发生。物理改性包括射线辐射技术和等离子体技术，射线辐射技术设备昂贵，而且往往需要引入一定的溶剂和单体，不利于大规模工业化生产。等离子体技术只增加了纤维表面的粗糙度和活性基团的数量，单纯的等离子处理不能增加纤维的本体强度。
微波辐射技术是近年来一种新型的改性技术，该技术具有处理剂量可控、处理时间短、处理效率高等优点。微波辐射在适当的条件下，可以引发自由基反应，使芳纶纤维的表皮和芯层之间发生交联，在不降低纤维的纵向抗拉强度的前提下，提高纤维的横向抗拉强度。
用于芳纶纤维改性的等离子体多为低温等离子体，其能量低，而且作用强度高，穿透力小，可以在芳纶纤维表皮极薄一层引起物理和化学变化，增加纤维表面的粗糙度和活性基团的数量，因而可以在不影响纤维的本体性能的同时改善芳纶纤维与其增强树脂之间界面的亲和力。
发明内容
本发明所要解决的技术问题是提供了一种改性芳纶纤维增强PA66材料及其制备方法。
本发明的技术方案由以下三个步骤组成：
步骤一，芳纶纤维经微波辐射改性，辐射频率为0.5～5GHZ，辐射剂量为0.1～2mW/cm2，辐射时间为1～240S。
步骤二，经微波辐射后的芳纶纤维再经低温等离子体处理，处理功率为10～400W，处理气氛为5～15%氢气、5～15%氟气和70～90%氦气，处理腔体内的气体压强为10～106Pa，处理温度为0～150℃，处理时间为1～20min，得到改性芳纶纤维。
步骤三、按以下质量百分比称取各组分：
PA66                           55～90%
改性芳纶纤维                    5～40%
马来酸酐接枝聚乙烯               3～5%
聚四氟乙烯                      1～10%
抗氧剂                         0.3～1%
将PA66、马来酸酐接枝聚乙烯、聚四氟乙烯和抗氧剂干燥后按配比加入高速混合机中混合均匀，混合后的物料加入双螺杆挤出机中进行熔融挤出。改性芳纶纤维按配方比例通过侧喂料加入。挤出工艺为一区260～270℃、二区260～270℃、三区260～270℃、四区260～270℃、五区245～255℃、六区245～255℃、七区245～255℃、八区245～255℃、九区245～255℃、十区245～255℃；主机转速为400～600rpm；侧喂料转数为5～10rpm；主喂料喂料转数为20～30rpm。经水冷、风冷、造粒后得到改性芳纶纤维增强PA66复合材料。
本发明的有益效果是：在微波辐射的作用下，芳纶纤维的表皮层和芯层发生交联，增加了纤维的横向抗拉强度；再经低温等离子处理，增加了纤维的表面粗糙度、表面极性和活性基团数量。与现有的表面改性技术相比，这种芳纶纤维的表面改性方法不仅仅增加了纤维的表面粗糙度、表面活性，而且通过交联作用提高了纤维的本体强度。用该方法制备的改性芳纶纤维增强PA66材料具有良好的力学性能和耐磨性能，该方法属于物理改性法，工艺简单，适合大规模工业化生产。
具体实施例：
实施例一
首先，将芳纶纤维置于微波辐射装置中心，辐射频率0.5GHz，辐射剂量0.1mW/cm2，辐射时间1S；然后，将经微波辐射改性后的芳纶纤维放置于低温等离子体装置的中心区域，开启真空泵将腔体内的空气抽出，通入5%氢气、5%氟气和90%氦气的混合气体，气体压强10Pa，处理功率为400W，处理温度0℃，处理时间20min，得到改性芳纶纤维。
将PA66、马来酸酐接枝聚乙烯、聚四氟乙烯和抗氧剂在80℃下真空干燥6h。各原料质量百分比为PA66 70%，聚四氟乙烯 5%，马来酸酐接枝聚乙烯5%，抗氧剂 0.3%，加入高速混合机中混合10min。将混合后的物料加入到双螺杆挤出机中进行熔融挤出，按质量百分比称取改性芳纶纤维 20%通过侧喂料加入。挤出工艺为：一区265℃、二区265℃、三区265℃、四区265℃、五区250℃、六区250℃、七区250℃、八区250℃、九区250℃、十区250℃；主机转数为500rpm；侧喂料转数为8rpm；主喂料转数为25rpm。经水冷、风冷、造粒后得到芳纶纤维增强PA66复合材料。材料真空干燥后，按相关检测标准要求注塑成标准样件。
 
实施例二
首先，将芳纶纤维置于微波辐射装置中心，辐射频率2.5GHz，辐射剂量0.5mW/cm2，辐射时间60S；然后，将经微波辐射改性后的芳纶纤维放置于低温等离子体装置的中心区域，开启真空泵将腔体内的空气抽出，通入10%氢气、10%氟气和80%氦气的混合气体，气体压强103Pa，处理功率为300W，处理温度23℃，处理时间15min，得到改性芳纶纤维。
将PA66、马来酸酐接枝聚乙烯、聚四氟乙烯和抗氧剂在80℃下真空干燥6h。各原料质量百分比为PA66 70%，聚四氟乙烯 5%，马来酸酐接枝聚乙烯 5%，抗氧剂 0.5%，加入高速混合机中混合10min。将混合后的物料加入到双螺杆挤出机中进行熔融挤出，按质量百分比称取改性芳纶纤维 20%通过侧喂料加入。挤出工艺为：一区265℃、二区265℃、三区265℃、四区265℃、五区250℃、六区250℃、七区250℃、八区250℃、九区250℃、十区250℃；主机转数为500rpm；侧喂料转数为8rpm；主喂料转数为25rpm。经水冷、风冷、造粒后得到芳纶纤维增强PA66复合材料。材料真空干燥后，按相关检测标准要求注塑成标准样件。
实施例三
首先，将芳纶纤维置于微波辐射装置中心，辐射频率3.5GHz，辐射剂量1.5mW/cm2，辐射时间120S；然后，将经微波辐射改性后的芳纶纤维放置于低温等离子体装置的中心区域，开启真空泵将腔体内的空气抽出，通入12%氢气、12%氟气和76%氦气的混合气体，气体压强105Pa，处理功率为100W，处理温度120℃，处理时间5min，得到改性芳纶纤维。
将PA66、马来酸酐接枝聚乙烯、聚四氟乙烯和抗氧剂在80℃下真空干燥6h。各原料质量百分比为PA66 70%，聚四氟乙烯 5%，马来酸酐接枝聚乙烯 5%，抗氧剂 0.5%，加入高速混合机中混合10min。将混合后的物料加入到双螺杆挤出机中进行熔融挤出，按质量百分比称取改性芳纶纤维 20%通过侧喂料加入。挤出工艺为：一区265℃、二区265℃、三区265℃、四区265℃、五区250℃、六区250℃、七区250℃、八区250℃、九区250℃、十区250℃；主机转数为500rpm；侧喂料转数为8rpm；主喂料转数为25rpm。经水冷、风冷、造粒后得到芳纶纤维增强PA66复合材料。材料真空干燥后，按相关检测标准要求注塑成标准样件。
实施例四
首先，将芳纶纤维置于微波辐射装置中心，辐射频率5GHz，辐射剂量2mW/cm2，辐射时间240S；然后，将经微波辐射改性后的芳纶纤维放置于低温等离子体装置的中心区域，开启真空泵将腔体内的空气抽出，通入15%氢气、15%氟气和70%氦气的混合气体，气体压强106Pa，处理功率为10W，处理温度150℃，处理时间1min，得到改性芳纶纤维。
将PA66、马来酸酐接枝聚乙烯、聚四氟乙烯和抗氧剂在80℃下真空干燥6h。各原料质量百分比为PA66 70%，聚四氟乙烯 5%，马来酸酐接枝聚乙烯 5%，抗氧剂 0.5%，加入高速混合机中混合10min。将混合后的物料加入到双螺杆挤出机中进行熔融挤出，按质量百分比称取改性芳纶纤维 20%通过侧喂料加入。挤出工艺为：一区265℃、二区265℃、三区265℃、四区265℃、五区250℃、六区250℃、七区250℃、八区250℃、九区250℃、十区250℃；主机转数为500rpm；侧喂料转数为8rpm；主喂料转数为25rpm。经水冷、风冷、造粒后得到芳纶纤维增强PA66复合材料。材料真空干燥后，按相关检测标准要求注塑成标准样件。
 
实施例一至实施例四检测结果列于表1，参比例为国外同类产品的性能：
表1
检测项目 单位 检测标准 实施例一 实施例二 实施例三 实施例四 参比例
简支梁无缺口冲击强度 KJ/m2 ISO 179 42.3 40.6 41.7 44.2 35
简支梁缺口冲击强度 KJ/m2 ISO 179 4.5 3.9 4.2 4.6 2.5
拉伸强度 MPa ISO 527 85.4 86.2 83.9 80.2 80
断裂伸长率 % ISO 527 4.2 3.9 4.1 4.5 3
弯曲强度 MPa ISO 178 145.6 152.3 140.7 142.9 130
弯曲模量 MPa ISO 178 4280 4359 4005 4156 4000
摩擦系数   GB 3960 0.15 0.18 0.16 0.17 0.20
体积磨损率 10-14m3·(Nm)-1 GB 3960 1.35 1.34 1.32 1.36 1.40

Claims (3)

1.一种改性芳纶纤维增强PA66材料，其特征在于，改性芳纶纤维是由对位芳香族聚酰胺纤维或间位芳香族聚酰胺纤维先经微波辐射改性，再用低温等离子处理后得到的；其纤维长度为0.15～15mm，单丝直径9～14μm。
2.根据权利要求1所述改性芳纶纤维增强PA66材料，其特征在于：芳纶纤维经微波辐射改性，辐射频率为0.5～5GHZ，辐射剂量为0.1～2mW/cm2，辐射时间为1～240S。
3.根据权利要求1、2所述改性芳纶纤维增强PA66材料，其特征在于：经微波辐射后的芳纶纤维再经低温等离子体处理，处理功率为10～400W，处理气氛为5～15%氢气、5～15%氟气和70～90%氦气，处理腔体内的气体压强为10～106Pa，处理温度为0～150℃，处理时间为1～20min；此方法改性后的芳纶纤维与PA66树脂通过双螺杆挤出机共混挤出制备的复合材料，其力学性能和耐磨性能比国外同类产品高15～20%。
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